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Sample records for hlc-723 g8 hplc

  1. Analytical verification and quality assessment of the Tosoh HLC-723GX HbA1c analyzer

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    Marko Ris

    2017-04-01

    Full Text Available Objectives: Ion-exchange high-performance liquid chromatography (IE-HPLC has long been used as a reproducible and versatile analytical tool for HbA1c measurement.In this study, we performed analytical verification and quality assessment of the recently introduced small IE-HPLC Tosoh HLC-723GX HbA1c analyzer, and a comparison of results to immunoassay (IA and capillary electrophoresis (CE. Design and methods: The total imprecision of Tosoh HLC-723GX was verified according to CLSI EP15-A2 protocol using commercial control materials (C-QC and pooled human whole blood samples (HWB. The Sigma metric was used for the evaluation of quality targets. HbA1c results were compared to automated CE (MiniCap Flex Piercing, Sebia, France and IA (Tina-quant HbA1c Gen 2, Cobas Integra 400+, Roche Diagnostics, USA procedures. Results: The total imprecision of Tosoh HLC-723GX-HbA1c for IFCC(mmol/mol and NGSP(% units was: 1.91/1.25% (HbA1c=31 mmol/mol/5.0% and 0.51/0.63% (HbA1c=84 mmol/mol/9.8% for C-QC, and 0.39/0.2% (HbA1c=47 mmol/mol/6.5% and 0.77/0.46% (HbA1c=94 mmol/mol/10.8% in HWB samples, respectively. Bland-Altman analysis did not reveal any deviation of the results between Tosoh HLC-723GX and CE: mean difference 0.0% (95%CI: −0.02927 to 0.02653%, while the mean HbA1c difference against IA was −0.07% (95%CI: −0.1039 to −0.02765. At the selected HbA1c clinical decision level (48 mmol/mol/6,5%, six sigma analysis gave σ value of 3.91, within a desirable classification of performance. Conclusion: The analytical performance of the Tosoh HLC-723GX complies with the rigorous quality criteria for clinical use of HbA1c, with the results comparable to the CE procedure. Tosoh HLC-723GX provides a plausible analytical choice for reliable HbA1c measurement in low-volume laboratories. Keywords: HbA1c, Quality targets, Six sigma, Tosoh HLC-723GX analyzer

  2. Evaluation of the hemoglobin A1c-analyzer TOSOH HLC-723 G7.

    Science.gov (United States)

    Gremmels, Heinz-Detlef; Richter, Anja; Watzke, Ivonne

    2003-01-01

    The TOSOH HLC-723 G7 is a compact analyzer designed for the measurement of HbA1c under routine laboratory conditions. The analyzer has an automatic blood tube supply and positive sample identification. Samples are transported automatically via racks in a continuous-load mode, cap piercing is optional. Tests devoted to the assessment of reproducibility and accuracy of analytical results indicated that over a test period of 17 days, the intra-assay variation (CV) was 1.79%, and the inter-assay variation 2.60%, respectively. A comparison with the predecessor model G5 showed a very good correlation (r = 0.997, y = 1.0041x - 0.00172; n = 149). The presence of high triglyceride, bilirubin or urea concentrations in patient samples did not influence the analytical precision. The labile HbA1c fraction (L-A1c) is clearly separated during chromatography and thus does not compromise HbA1c analysis. With a protocol of 1.2 minutes, the TOSOH G7 is a very fast analyzer, designed for laboratories with a high throughput of samples.

  3. Heterozygote Hemoglobin G-Coushatta as the Cause of a Falsely Decreased Hemoglobin A1C in an Ion-Exchange HPLC Method

    Directory of Open Access Journals (Sweden)

    Kurtoğlu Ayşegül Uğur

    2017-09-01

    Full Text Available Glycated hemoglobin (HbA1c is used for the assessment of glycemic control in patients with diabetes. The presence of genetic variants of hemoglobin can profoundly affect the accuracy of HbA1c measurement. Here, we report two cases of Hemoglobin G-Coushatta (HBB:c.68A>C variant that interferes in the measurement of HbA1c by a cation-exchange HPLC (CE-HPLC method. HbA1c was measured by a CE-HPLC method in a Tosoh HLC-723 G7 instrument. The HbA1c levels were 2.9% and 4%. These results alerted us to a possible presence of hemoglobinopathy. In the hemoglobin variant analysis, HbA2 levels were detected as 78.3% and 40.7% by HPLC using the short program for the Biorad Variant II. HbA1c levels were measured by an immunoturbidimetric assay in a Siemens Dimension instrument. HbA1c levels were reported as 5.5% and 5.3%. DNA mutation analysis was performed to detect the abnormal hemoglobin variant. Presence of Hemoglobin G-Coushatta variant was detected in the patients. The Hb G-Coushatta variants have an impact on the determination of glycated hemoglobin levels using CEHPLC resulting in a false low value. Therefore, it is necessary to use another measurement method.

  4. HLC/pullulan and pullulan hydrogels: their microstructure, engineering process and biocompatibility

    Energy Technology Data Exchange (ETDEWEB)

    Li, Xian [College of chemistry & materials science, Northwest University, Taibai North Road 229, Xi’an, Shaanxi 710069 (China); Shaanxi Key Laboratory of Degradable Biomedical Materials, Department of Chemical Engineering, Northwest University, Taibai North Road 229, Xi’an, Shaanxi 710069 (China); Xue, Wenjiao [Shannxi provincial institute of microbiology, Xi’ an 710043 (China); Liu, Yannan; Li, Weina [Shaanxi Key Laboratory of Degradable Biomedical Materials, Department of Chemical Engineering, Northwest University, Taibai North Road 229, Xi’an, Shaanxi 710069 (China); Fan, Daidi, E-mail: fandaidi@nwu.edu.cn [Shaanxi Key Laboratory of Degradable Biomedical Materials, Department of Chemical Engineering, Northwest University, Taibai North Road 229, Xi’an, Shaanxi 710069 (China); Zhu, Chenhui [Shaanxi Key Laboratory of Degradable Biomedical Materials, Department of Chemical Engineering, Northwest University, Taibai North Road 229, Xi’an, Shaanxi 710069 (China); Wang, Yaoyu, E-mail: wyaoyu@nwu.edu.cn [College of chemistry & materials science, Northwest University, Taibai North Road 229, Xi’an, Shaanxi 710069 (China)

    2016-01-01

    New locally injectable biomaterials that are suitable for use as soft tissue fillers are needed to address a significant unmet medical need. In this study, we used pullulan and human-like collagen (HLC) based hydrogels with various molecular weights (MWs) in combination therapy against tissue defects. Briefly, pullulan was crosslinked with NaIO{sub 4} to form a pullulan hydrogel and then may coupled with HLC using the reaction between the –NH{sub 2} end-group of HLC and the –CHO group present on the aldehyde pullulan to form the HLC/pullulan hydrogel, wherein the NaIO{sub 4} acted as the crosslinking and oxidizing agent. The good miscibility of pullulan and HLC in the hydrogels was confirmed via Fourier transform infrared spectroscopy, scanning electron microscopy, compression testing, enzyme degradation testing, cell adhesions, live/dead staining and subcutaneous filling assays. Here, pullulan hydrogels with various MWs were fabricated and physicochemically characterized. Limitations of the pullulan hydrogels included inflammation, poor mechanical strength, and degradation. By contrast, the properties of the HLC/pullulan hydrogels strongly enhanced. The efficacy of these hydrogels was evaluated both in vitro and in vivo. Our results indicate that HLC/pullulan hydrogels may have therapeutic value as efficient soft tissue fillers, with reduced inflammation, improved cell adhesion and delayed hydrogel degradation. - Graphical abstract: The HLC/pullulan hydrogels were prepared by dialysis, wet granulation and UV radiation after various MWs of pullulan and HLC were crosslinked with NaIO{sub 4}, and injected subcutaneously into Kunming mouse. The formation of HLC/pullulan hydrogels is due to the amide bond linkage with the amino group of HLC and the aldehyde groups in pullulan aqueous media after crosslinking by NaIO{sub 4}. HLC/pullulan hydrogels may have therapeutic value as efficient soft tissue fillers, with reduced inflammation, improved cell adhesion and

  5. Effects of common hemoglobin variants on HbA1c measurements in China: results for α- and β-globin variants measured by six methods.

    Science.gov (United States)

    Xu, Anping; Chen, Weidong; Xia, Yong; Zhou, Yu; Ji, Ling

    2018-04-07

    HbA1c is a widely used biomarker for diabetes mellitus management. Here, we evaluated the accuracy of six methods for determining HbA1c values in Chinese patients with common α- and β-globin chains variants in China. Blood samples from normal subjects and individuals exhibiting hemoglobin variants were analyzed for HbA1c, using Sebia Capillarys 2 Flex Piercing (C2FP), Bio-Rad Variant II Turbo 2.0, Tosoh HLC-723 G8 (ver. 5.24), Arkray ADAMS A1c HA-8180V fast mode, Cobas c501 and Trinity Ultra2 systems. DNA sequencing revealed five common β-globin chain variants and three common α-globin chain variants. The most common variant was Hb E, followed by Hb New York, Hb J-Bangkok, Hb G-Coushatta, Hb Q-Thailand, Hb G-Honolulu, Hb Ube-2 and Hb G-Taipei. Variant II Turbo 2.0, Ultra2 and Cobas c501 showed good agreement with C2FP for most samples with variants. HLC-723 G8 yielded no HbA1c values for Hb J-Bangkok, Hb Q-Thailand and Hb G-Honolulu. Samples with Hb E, Hb G-Coushatta, Hb G-Taipei and Hb Ube-2 produced significant negative biases for HLC-723 G8. HA-8180V showed statistically significant differences for Hb E, Hb G-Coushatta, Hb G-Taipei, Hb Q-Thailand and Hb G-Honolulu. HA-8180V yielded no HbA1c values for Hb J-Bangkok. All methods showed good agreement for samples with Hb New York. Some common hemoglobin variants can interfere with HbA1c determination by the most popular methods in China.

  6. Characterization and biodistribution of recombinant and recombinant/chimeric constructs of monoclonal antibody B72.3

    International Nuclear Information System (INIS)

    Colcher, D.; Milenic, D.; Roselli, M.

    1989-01-01

    Radiolabeled B72.3 has been administered both i.v. and i.p. in patients with colorectal and ovarian cancer as well as other carcinomas and has been shown to selectively bind to approximately 70-80% of metastatic lesions. Greater than 50% of the patients that have been treated with B72.3 have developed an immunological response to murine IgG after a single injection. In an attempt to minimize the immune response of these patients to the administered murine monoclonal antibody, we developed a recombinant form of the murine B72.3 as well as a recombinant/chimeric antibody, using the variable regions of the murine B72.3 and human heavy chain (gamma 4) and light chain (kappa) constant regions. We report here that both the recombinant B72.3 [rB72.3] and the recombinant/chimeric B72.3 [cB72.3(gamma 4)] IgGs maintain the tissue binding and idiotypic specificity of the native murine IgG. The native B72.3, rB72.3, and cB72.3(gamma 4) IgGs were radiolabeled and the biodistribution of these IgGs was studied in athymic mice bearing human colon carcinoma xenografts (LS-174T). Differences were observed between the cB72.3(gamma 4) and the native B72.3 in the percentage of injected dose/g that localized in the tumor. The somewhat lower absolute amounts of the cB72.3(gamma 4) in the tumor are mostly likely due to the observed more rapid clearance from the blood and body of the mouse as compared to the native B72.3 and rB72.3. All three forms [native B72.3, rB72.3, and cB72.3(gamma 4)] of the IgG, however, were able to localize the colon tumor with similar radiolocalization indices [percentage of injected dose/g in tumor divided by the percentage of injected dose/g in normal tissue

  7. 5 CFR 723.140 - Employment.

    Science.gov (United States)

    2010-01-01

    ... 5 Administrative Personnel 2 2010-01-01 2010-01-01 false Employment. 723.140 Section 723.140... PERSONNEL MANAGEMENT § 723.140 Employment. No qualified individual with handicaps shall, on the basis of handicap, be subject to discrimination in employment under any program or activity conducted by the agency...

  8. Simultaneous Analytical Techniques for Determination of 8 Synthetic Food Colors in Foods by HPLC

    Energy Technology Data Exchange (ETDEWEB)

    Park, S.K.; Lee, C.H.; Park, J.S.; Yoon, H.J.; Kim, S.H.; Hong, Y.; Lee, J.O.; Lee, C.W. [Korea Food and Drug Administration, Seoul (Korea)

    2000-06-01

    This Study has been carried out to develop a method of analysis of 8 permitted synthetic food colors [including Brilliant Blue FCF (B1), Indigocarmine (B2), Fast green FCF (G3), Amaranth (R2), Erythrosine (R3), Allura red (R40), Tartrazine (Y4), Sunset Yellow FCF (Y5)] in Korean foods by HPLC. After adjusting to 0.5% HCl, each of the food colors extracted was eluted by Sep-pak C{sub 18} cartridge. Eluates were then determined by high performance liquid chromatograph with a UV-VIS detector. Recoveries of the 8 synthetic food colors were found to be 81.2-98.0% for soft drinks, 80.6-96.1% for candy, 79.8-96.3% for chewing gum, 76.5-91.7% for cereals, 79.0-93.8% for ice cream and 78.6-94.7% for jelly, respectively. The detection limits were 0.05-0.1 {mu}g/g. (author). 24 refs., 2 tabs., 4 figs.

  9. 46 CFR 169.723 - Safety belts.

    Science.gov (United States)

    2010-10-01

    ... 46 Shipping 7 2010-10-01 2010-10-01 false Safety belts. 169.723 Section 169.723 Shipping COAST... Control, Miscellaneous Systems, and Equipment § 169.723 Safety belts. Each vessel must carry a harness type safety belt conforming to Offshore Racing Council (ORC) standards for each person on watch or...

  10. 21 CFR 172.723 - Epoxidized soybean oil.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Epoxidized soybean oil. 172.723 Section 172.723... CONSUMPTION Other Specific Usage Additives § 172.723 Epoxidized soybean oil. Epoxidized soybean oil may be... reacting soybean oil in toluene with hydrogen peroxide and formic acid. (b) It meets the following...

  11. 40 CFR 35.723 - Competitive process.

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 1 2010-07-01 2010-07-01 false Competitive process. 35.723 Section 35... Grants (pub.l. 105-276) § 35.723 Competitive process. EPA will award Tribal hazardous waste program... guidance. After the competitive process is complete, the recipient can, at its discretion, accept the award...

  12. Use of monoclonal antibody B72.3 in the management of gynecologic malignancies

    International Nuclear Information System (INIS)

    Simpson, J.; Schlom, J.

    1988-01-01

    Monoclonal antibodies are currently used in the diagnosis of gynecologic malignancies by way of immunohistochemical assays, serum assays, and in situ radiolocalization of carcinoma lesions. Among them is MAb B72.3, generated against a human tumor-associated antigen (TAG-72). Using immunohistochemical techniques, MAb B72.3 has shown reactivity with 100 percent of common epithelial ovarian carcinomas and endometrial carcinomas and non-reactivity with normal adult tissues, with the exception of normal secretory endometrium. B72.3 appears to be a valuable immunocytologic adjunct, with greater than 90 percent of effusions and fine-needle aspiration biopsies from gynecologic carcinomas showing reactivity. Using a serum assay developed to detect the presence of the TAG-72 antigen, 48 percent of patients with ovarian carcinoma demonstrated TAG-72-positive sera versus 1 percent of control sera. 131 I-labeled MAb B72.3 IgG and gamma scanning have been used for the in situ detection of metastatic carcinoma. Twelve of 15 patients with ovarian carcinoma showed positive gamma scans, and approximately 80 percent of the lesions demonstrated specific localization of the antibody. These studies indicate the potential utility of MAb B72.3 in the diagnosis of gynecologic carcinoma. 57 references

  13. 27 CFR 7.23 - Brand names.

    Science.gov (United States)

    2010-04-01

    ... 27 Alcohol, Tobacco Products and Firearms 1 2010-04-01 2010-04-01 false Brand names. 7.23 Section... Beverages § 7.23 Brand names. (a) General. The product shall bear a brand name, except that if not sold under a brand name, then the name of the person required to appear on the brand label shall be deemed a...

  14. BSN723T Prevents Atherosclerosis and Weight Gain in ApoE Knockout Mice Fed a Western Diet.

    Science.gov (United States)

    Williams, Jarrod; Ensor, Charles; Gardner, Scott; Smith, Rebecca; Lodder, Robert

    This study tests the hypothesis that BSN723T can prevent the development of hyperlipidemia and atherosclerosis in ApoE -/- knockout mice fed a Western (high fat, high cholesterol, and high sucrose) diet. BSN723T is a combination drug therapy consisting of D-tagatose and dihydromyricetin (BSN723). D-tagatose has an antihyperglycemic effect in animal and human studies and shows promise as a treatment for type 2 diabetes and obesity. Many claims regarding BSN723's pharmacological activities have been made including anti-cancer, anti-diabetic, anti-hypertensive, anti-inflammatory, and anti-atherosclerotic effects. To our knowledge this is the first study that combines D-tagatose and BSN723 for the treatment of hyperlipidemia and the prevention of atherosclerosis. ApoE-deficient mice were randomized into five groups with equivalent mean body weights. The mice were given the following diets for 8 weeks: Group 1 - Standard diet; Group 2 - Western diet; Group 3 - Western diet formulated with D-tagatose; Group 4 - Western diet formulated with BSN723; Group 5 - Western diet formulated with BSN723T. Mice were measured for weight gain, tissue and organ weights, total serum cholesterol and triglycerides and formation of atherosclerosis. The addition of D-tagatose, either alone or in combination with BSN723, prevented the increase in adipose tissue and weight gain brought on by the Western diet. Both D-tagatose and BSN723 alone reduced total cholesterol and the formation of atherosclerosis in the aorta compared to mice on the Western diet. Addition of BSN723 to D-tagatose (BSN723T) did not increase efficacy in prevention of increases in cholesterol or atherosclerosis compared to D-tagatose alone. Addition of either D-tagatose or BSN723 alone to a Western diet prevented weight gain, increases in total serum cholesterol and triglycerides, and the formation of atherosclerosis. However, there was no additive or synergistic effect on the measured parameters with the combination BSN

  15. [The value of serum heavy/light chain immunoassay to assess therapeutic response in patients with multiple myeloma].

    Science.gov (United States)

    Yu, X C; Su, W; Zhuang, J L

    2018-04-14

    Objective: To assess the value of immunoglobulin heavy/light chain (HLC) immunoassay on therapeutic response in patients with multiple myeloma(MM). Methods: A total of 45 newly diagnosed MM patients were retrospectively enrolled in Peking Union Medical College Hospital from 2013 to 2016, whose 115 serum samples were consecutively collected. HLC was tested to evaluate response and compare with other methods for M protein detection. Results: ①There were 30 males and 15 females in total of whom the monoclonal immunoglobulin was IgG in 27 (IgGκ∶IgGλ 12∶15) and IgA (IgAκ∶IgAλ 9∶9) in 18. The arerage age of the studied population was 59 (range 43-80) . ② In 34 patients with serum sample at diagnosis, 32 (94.1%) had abnormal HLC ratio (rHLC) while 2 patients with IgG had normal rHLC. The percentages of abnormal rHLC was 81.8% (18/22) at partial response、50.0%(9/18) at very good complete response and 16.0%(4/25) at complete response. ③In 25 patients reaching CR, there were 13 with IgG and 12 with IgA. 4 patients equally split of IgG and IgA had abnormal rHLC at complete response. ④By monitoring the rHLC of some patients consecutively, we found that the remission of rHLC was to some extent behind the remission of SPE and IEF, or even rFLC. Conclusion: Immunoglobulin HLC detection is one feasible method for minimal residual disease detection.

  16. 31 CFR 501.723 - Prehearing disclosures; methods to discover additional matter.

    Science.gov (United States)

    2010-07-01

    ... (9)) and the Privacy Act (5 U.S.C. 552a). Parties may obtain discovery regarding any matter, not... Information Act (5 U.S.C. 552(b)(1) through (9)). (g) Updating discovery. A party who has made an initial..., PROCEDURES AND PENALTIES REGULATIONS Trading With the Enemy Act (TWEA) Penalties § 501.723 Prehearing...

  17. Preparation and biological evaluation of 111In-, 177Lu- and 90Y-labeled DOTA analogues conjugated to B72.3

    International Nuclear Information System (INIS)

    Mohsin, Huma; Fitzsimmons, Jonathan; Shelton, Tiffani; Hoffman, Timothy J.; Cutler, Cathy S.; Lewis, Michael R.; Athey, Phillip S.; Gulyas, Gyongyi; Kiefer, Garry E.; Frank, R. Keith; Simon, Jaime; Lever, Susan Z.; Jurisson, Silvia S.

    2007-01-01

    Three 1,4,7,10-tetraazacyclododecane-N,N',N '' ,N '' '-tetraacetic acid (DOTA) analogues were evaluated for relative in vivo stability when radiolabeled with 111 In, 90 Y and 177 Lu and conjugated to the monoclonal antibody B72.3. The DOTA analogues evaluated were 'NHS-DOTA' [N-hydroxysuccinimdyl (NHS) group activating one carboxylate], 'Arm-DOTA' (also known as MeO-DOTA; with a p-NCS, o-MeO-benzyl moiety on the methylene group of one acetic acid arm) and 'Back-DOTA' (with a p-NCS-benzyl moiety on a backbone methylene group of the macrocycle). The B72.3 was conjugated to the DOTA analogues to increase the retention time of the radioloabeled conjugates in vivo in mice. The serum stability of the various radiometalated DOTA conjugates showed them to have good stability out to 168 h (all >95% except 111 In-NHS-DOTA-B72.3, which was 91% stable). Hydroxyapatite stability for the 111 In and 177 Lu DOTA-conjugates was >95% at 168 h, while the 90 Y DOTA-conjugates were somewhat less stable (between 90% and 95% at 168 h). The biodistribution studies of the radiometalated DOTA-conjugates showed that no significant differences were observed for the 111 In and 177 Lu analogues; however, the 90 Y analogues showed lower stabilities, as evidenced by their increased bone uptake relative to the other two [2-20% injected dose per gram (% ID/g) for 90 Y and 2-8% ID/g for 111 In and 177 Lu]. The lower stability of the 90 Y analogues could be due to the higher beta energy of 90 Y and/or to the larger ionic radius of Y 3+ . Based on the bone uptake observed, the 177 Lu-NHS-DOTA-B72.3 had slightly lower stability than the 177 Lu-Arm-DOTA-B72.3 and 177 Lu-Back-DOTA-B72.3, but not significantly at all time points. For 90 Y, the analogue showing the lowest stability based on bone uptake was 90 Y-Arm-DOTA-B72.3, perhaps because of the metal's larger ionic radius and potential steric interactions minimizing effective complexation. The 111 In analogues all showed similar biological

  18. Determination of anthocyanins from camu-camu (Myrciaria dubia) by HPLC-PDA, HPLC-MS, and NMR.

    Science.gov (United States)

    Zanatta, Cinthia Fernanda; Cuevas, Elyana; Bobbio, Florinda O; Winterhalter, Peter; Mercadante, Adriana Z

    2005-11-30

    Camu-camu [Myrciaria dubia (HBK) McVaugh] is a small fruit native to the Amazonian rain forest. Its anthocyanin profile has now been investigated for the first time. Fruits from two different regions of the São Paulo state, Brazil, were analyzed. The major anthocyanins were isolated by high-speed countercurrent chromatography. HPLC-PDA, HPLC-MS/MS, and 1H NMR were used to confirm the identity of the main anthocyanins of camu-camu. Cyanidin-3-glucoside was identified as the major pigment in the fruits from both regions, representing 89.5% in the fruits produced in Iguape and 88.0% in those from Mirandópolis, followed by the delphinidin-3-glucoside, ranging between 4.2 and 5.1%, respectively. Higher total anthocyanin contents were detected in the fruits from Iguape (54.0 +/- 25.9 mg/100 g) compared to those from Mirandópolis (30.3 +/- 6.8 mg/100 g), most likely because of the lower temperatures in the Iguape region.

  19. 12 CFR 723.2 - What are the prohibited activities?

    Science.gov (United States)

    2010-01-01

    ... MEMBER BUSINESS LOANS § 723.2 What are the prohibited activities? (a) Who is ineligible to receive a... senior management employees is tied to the profit or sale of the business or commercial endeavor for... 12 Banks and Banking 6 2010-01-01 2010-01-01 false What are the prohibited activities? 723.2...

  20. 8-Hydroxy-2'-deoxyguanosine (8-OH-dG): A biomarker of oxidative damage in yellow bullheads chronically exposed to low-level radiation

    International Nuclear Information System (INIS)

    McCreedy, C.D.; Glickman, L.T.

    1995-01-01

    8-hydroxy-2'-deoxyguanosine (8-OH-dG), an oxidation product of the nucleotide deoxyguanosine (dG) was used as a biomarker to assess oxidative damage in brain and gill tissues of yellow bullhead catfish (Ameiurus natalis; n = 18) inhabiting an abandoned reactor reservoir contaminated with low levels of d137 Cs (Pond B, Savannah River Site, SC). DNA was isolated by chloroform-isoamyl extraction, enzymatically digested with Nuclease P1/Calf Intestinal Phosphatase, and analyzed by HPLC with electrochemical detection.Length, weight, age, condition and muscle 137 Cs activity of each fish were also determined. Concentrations of 8-OH-dG were greater in brain than in gill tissues. 8-OH-dG in gill tissues decreased as condition of fish increased, but as age increased, the effect of condition declined. Brain 8-OH-dG concentration was not related to age or condition of fish, but was greater in females and the interaction between gender and 137 Cs was significant. Brain 8-OH-dG was positively associated with muscle 137 Cs concentration among females, but was unrelated to 137 Cs concentration in males. At lower 137 Cs concentrations, females tended to have fewer oxidative DNA adducts in brian than did males. Deposition of somatic lipids into eggs may provide females some anti-oxidant benefit by diminishing the contribution of lipid peroxidation to DNA damage. 8-OH-dG is a sensitive biomarker of low-level radiation exposure, however, its application in fish requires consideration of factors such as gender, age, body-condition, and the tissue type sampled

  1. Determination of patulin in fruit juices using HPLC-DAD and GC-MSD techniques.

    Science.gov (United States)

    Moukas, Athanasios; Panagiotopoulou, Vasiliki; Markaki, Panagiota

    2008-08-15

    A high performance liquid chromatography with a diode-array detector (HPLC-DAD) and a gas chromatography with a mass spectrometer (GC-MSD) are described for the determination of patulin (PAT) in apple juice. The limits of detection (DL) and quantification (QL) for the HPLC-DAD and GC-MSD method were found to be (DL=0.23μgkg(-1) QL=1.2μgkg(-1)) and (DL=5.8μgkg(-1) and QL=13.8μgkg(-1)), respectively. The recovery factors for HPLC-DAD and GC-MSD were found to be 99.5% (RSD%=0.73) and 41% (RSD%=10.03), respectively. The HPLC-DAD method was used to determine the occurrence of PAT in 90 samples of fruit juices. Results revealed the presence of PAT in 100% of the samples examined. The mean values of PAT in concentrated fruit juices and in the commercial fruit juices collected from the Greek market were found to be 10.54μg PAT kg(-1) and 5.57μg PAT kg(-1) juice, respectively. The most contaminated samples were four concentrated juices ranging from 18.10μg PAT kg(-1) to 36.8μg PAT kg(-1) juice. The daily exposure to patulin for the consumers of all ages in Greece, is ranging from 0.008μg PAT kg(-1) bw to 0.1μg PAT kg(-1) bw if the daily intake of fruit juices is from 0.1 to 0.5kg. With the exception to the most contaminated sample, the daily exposure due to the samples examined, is below the provisional maximum tolerable daily intake for PAT (0.4μg PAT kg(-1) bw). Copyright © 2008 Elsevier Ltd. All rights reserved.

  2. 糖尿病视网膜病变患者血小板参数与糖化血红蛋白变化及临床意义%Study on clinical significance of changes in MPV and HbAlc in patients with diabetic retinopathy.

    Institute of Scientific and Technical Information of China (English)

    徐威; 蔡应木; 王彩霞

    2012-01-01

    目的 探讨血小板平均体积(MPV)及糖化血红蛋白(HbA1c)在糖尿病视网膜病变时的变化及临床意义.方法采用BEACKMAN COULTER LH750 全自动血细胞分析仪和TOSOH HLC-723G8全自动糖化血红蛋白分析仪检测85例糖尿病患者[单纯糖尿病者45例,糖尿病视网膜病变(DR)者40例]的血小板计数(PLT)、MPV、血小板分布宽度(PDW)、HbA1c并与40例健康成人(对照组)进行对照比较.结果 DR组HbA1c、MPV、PDW明显高于单纯糖尿病组及对照组(P<0.05,P<0.01),而PLT低于单纯糖尿病组及对照组(P<0.05).结论 HbA1c与MPV的联合检测对糖尿病患者视网膜病变的发生及预后判断方面具有重要意义,有助于早期发现DR的存在.%Objective To explore the clinical significance of changes in MPV and glycosylated hemoglobin ( HbAlc ) in patients with diabetic retinopathy. Methods Blood platelet count, mean platelet volume ( MPV ) and platelet distribution width ( PDW ) of 45 diabetics without retinopathy, 40 diabetics with retinopathy and 40 healthy persons were measured by automatic blood cell analyzer BEACKMAN COULTER LH750. Level of HbAlc was measured by automatic glycosylated hemoglobin analyzer TOSOH HLC -723G8. Results Compared with healthy and diabetes groups, levels of HbAlc, MPV and PDW in diabetic retinopathy group were remarkably increased ( P<0.05, P<0. 01 ), while platelet count was decreased ( P<0.05 ). Conclusion Joint detection of level of HbAlc and MPV is helpful for early diagnosis and prognosis judgement of diabetic retinopathy in patients with diabetes.

  3. 25 CFR 700.723 - Control of livestock disease and parasites.

    Science.gov (United States)

    2010-04-01

    ... 25 Indians 2 2010-04-01 2010-04-01 false Control of livestock disease and parasites. 700.723... RELOCATION PROCEDURES New Lands Grazing § 700.723 Control of livestock disease and parasites. Whenever livestock within the New Lands become infected with contagious or infectious disease or parasites or have...

  4. Chloramine-T induced binding of monoclonal antibody B72. 3 to concanavalin-A

    Energy Technology Data Exchange (ETDEWEB)

    Cole, W.C.; Jhingran, S.G. (Methodist Hospital, Houston, TX (United States) Baylor Coll. of Medicine, Houston, TX (United States))

    1993-07-01

    The effects of chloramine-T (CT) on monoclonal antibody B72.3 were studied with particular reference to Con-A lectin binding. After exposure to chloramine-T concentrations from 0.8 to 4.0 mg/mL (115-574 mol CT/mol B72.3), B72.3 showed progressive binding to agarose-linked Con-A. This behavior was paralleled by decreasing immunoreactivity and increasing fragmentation and aggregation of B72.3 demonstrated by SDS-PAGE and size exclusion HPLC. (Author).

  5. Radioimmunoguided surgery using the monoclonal antibody B72.3 in colorectal tumors

    International Nuclear Information System (INIS)

    Sickle-Santanello, B.J.; O'Dwyer, P.J.; Mojzisik, C.

    1987-01-01

    The authors have developed a hand-held gamma-detecting probe (GDP) for intraoperative use that improves the sensitivity of external radioimmunodetection. Radiolabeled monoclonal antibody (MAb) B72.3 was injected in six patients with primary colorectal cancer and 31 patients with recurrent colorectal cancer an average of 16 days preoperatively. The GDP localized the MAb B72.3 in 83 percent of sites. The technique, known as a radioimmunoguided surgery (RIGS) system did not alter the surgical procedure in patients with primary colorectal cancer but did alter the approach in 26 percent (8/31) of patients with recurrent colorectal cancer. Two patients avoided unnecessary liver resections and two underwent extraabdominal approaches to document their disease. The RIGS system may influence the short-term morbidity and mortality of surgery for colorectal cancer. Larger series and longer follow-up are needed to determine whether the RIGS system confers a survival advantage to the patient with colorectal cancer

  6. Formation and characterization of iron-binding phosphorylated human-like collagen as a potential iron supplement

    International Nuclear Information System (INIS)

    Deng, Jianjun; Chen, Fei; Fan, Daidi; Zhu, Chenhui; Ma, Xiaoxuan; Xue, Wenjiao

    2013-01-01

    Iron incorporated into food can induce precipitation and unwanted interaction with other components in food. Iron-binding proteins represent a possibility to avoid these problems and other side effects, as the iron is protected. However, there are several technical problems associated with protein–iron complex formation. In this paper, the iron-binding phosphorylated human-like collagen (Fe-G6P-HLC) was prepared under physiological conditions through phosphorylated modification. One molecule of Fe-G6P-HLC possesses about 24 atoms of Fe. Spectroscopy analysis, differential scanning calorimetry (DSC) and equilibrium dialysis techniques were employed to investigate the characteristics of the Fe-G6P-HLC. The binding sites (n b ) and apparent association constant (K app ) between iron and phosphorylated HLC were measured at n b = 23.7 and log K app = 4.57, respectively. The amount of iron (Fe 2+ sulfate) binding to phosphorylated HLC was found to be a function of pH and phosphate content. In addition, the solubility and thermal stability of HLC were not significantly affected. The results should facilitate the utilization of HLC as a bioactive iron supplement in the food and medical industry and provide an important theoretical evidence for the application of HLC chelates. - Highlights: • The iron-binding phosphorylated human-like collagen (Fe-G6P-HLC) was prepared. • One molecule of Fe-G6P-HLC possesses about 24 atoms of Fe. • The binding properties could be modulated through alterations in pH and phosphate content presented in HLC. • A novel strategy for preparing iron-binding proteins was provided

  7. Comparative HPLC/ESI-MS and HPLC/DAD study of different populations of cultivated, wild and commercial Gentiana lutea L.

    Science.gov (United States)

    Mustafa, Ahmed M; Caprioli, Giovanni; Ricciutelli, Massimo; Maggi, Filippo; Marín, Rosa; Vittori, Sauro; Sagratini, Gianni

    2015-05-01

    The root of Gentiana lutea L., famous for its bitter properties, is often used in alcoholic bitter beverages, food products and traditional medicine to stimulate the appetite and improve digestion. This study presents a new, fast, and accurate HPLC method using HPLC/ESI-MS and HPLC/DAD for simultaneous analysis of iridoids (loganic acid), secoiridoids (gentiopicroside, sweroside, swertiamarin, amarogentin) and xanthones (isogentisin) in different populations of G.lutea L., cultivated in the Monti Sibillini National Park, obtained wild there, or purchased commercially. Comparison of HPLC/ESI-MS and HPLC/DAD indicated that HPLC/ESI-MS is more sensitive, reliable and selective. Analysis of twenty samples showed that gentiopicroside is the most dominant compound (1.85-3.97%), followed by loganic acid (0.11-1.30%), isogentisin (0.03-0.48%), sweroside (0.05-0.35%), swertiamarin (0.08-0.30%), and amarogentin (0.01-0.07%). The results confirmed the high quality of the G.lutea cultivated in the Monti Sibillini National Park. Copyright © 2014 Elsevier Ltd. All rights reserved.

  8. Determination of boron in uranium and aluminium by high pressure liquid chromatography (HPLC)

    International Nuclear Information System (INIS)

    Rao, Radhika M.; Aggarwal, S.K.

    2003-01-01

    Experiments were conducted for the determination of boron in U 3 O 8 powder and aluminium metal using dynamically modified reversed phase high pressure liquid chromatography (RP-HPLC) and using precolumn chromogenic agent viz. curcumin for complexing boron. The complex was separated from the excess of reagent and determined by HPLC. The boron curcumin complex (rosocyanin) was formed after extraction of boron with 2-ethyl-1,3-hexane diol (EHD). Linear calibration curves for boron amounts in the range of 0.02 μg to 0.5 μg were developed and used for the determination of boron in aluminium and uranium samples. (author)

  9. Formation and characterization of iron-binding phosphorylated human-like collagen as a potential iron supplement

    Energy Technology Data Exchange (ETDEWEB)

    Deng, Jianjun; Chen, Fei; Fan, Daidi, E-mail: fandaidi@nwu.edu.cn; Zhu, Chenhui; Ma, Xiaoxuan; Xue, Wenjiao

    2013-10-01

    Iron incorporated into food can induce precipitation and unwanted interaction with other components in food. Iron-binding proteins represent a possibility to avoid these problems and other side effects, as the iron is protected. However, there are several technical problems associated with protein–iron complex formation. In this paper, the iron-binding phosphorylated human-like collagen (Fe-G6P-HLC) was prepared under physiological conditions through phosphorylated modification. One molecule of Fe-G6P-HLC possesses about 24 atoms of Fe. Spectroscopy analysis, differential scanning calorimetry (DSC) and equilibrium dialysis techniques were employed to investigate the characteristics of the Fe-G6P-HLC. The binding sites (n{sub b}) and apparent association constant (K{sub app}) between iron and phosphorylated HLC were measured at n{sub b} = 23.7 and log K{sub app} = 4.57, respectively. The amount of iron (Fe{sup 2+} sulfate) binding to phosphorylated HLC was found to be a function of pH and phosphate content. In addition, the solubility and thermal stability of HLC were not significantly affected. The results should facilitate the utilization of HLC as a bioactive iron supplement in the food and medical industry and provide an important theoretical evidence for the application of HLC chelates. - Highlights: • The iron-binding phosphorylated human-like collagen (Fe-G6P-HLC) was prepared. • One molecule of Fe-G6P-HLC possesses about 24 atoms of Fe. • The binding properties could be modulated through alterations in pH and phosphate content presented in HLC. • A novel strategy for preparing iron-binding proteins was provided.

  10. G5..., G6..., G7..., G8..., G?

    OpenAIRE

    Monteiro, António

    2001-01-01

    O G8 tem as suas raízes no primitivo embrião do G5 quando, em 1973, o então Secretário de Estado do Tesouro americano, George Schultz, convocou os Ministros das Finanças da França, Japão, Reino Unido e República Federal da Alemanha para uma reunião. O objectivo era analisar como fazer face à primeira crise do petróleo da OPEC e subsequente recessão económica nos países mais industrializados, ao colapso do sistema monetário das taxas de câmbio de paridades fixas de Bretton-Woods e ao alargamen...

  11. HPLC Method for Simultaneous Quantitative Detection of Quercetin and Curcuminoids in Traditional Chinese Medicines

    Directory of Open Access Journals (Sweden)

    Lee Fung Ang

    2014-12-01

    Full Text Available Objectives: Quercetin and curcuminoids are important bioactive compounds found in many herbs. Previously reported high performance liquid chromatography ultraviolet (HPLC-UV methods for the detection of quercetin and curcuminoids have several disadvantages, including unsatisfactory separation times and lack of validation according the standard guidelines of the International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use. Methods: A rapid, specific, reversed phase, HPLC-UV method with an isocratic elution of acetonitrile and 2% v/v acetic acid (40% : 60% v/v (pH 2.6 at a flow rate of 1.3 mL/minutes, a column temperature of 35°C, and ultraviolet (UV detection at 370 nm was developed. The method was validated and applied to the quantification of different types of market available Chinese medicine extracts, pills and tablets. Results: The method allowed simultaneous determination of quercetin, bisdemethoxycurcumin, demethoxycurcumin and curcumin in the concentration ranges of 0.00488 ─ 200 μg/mL, 0.625 ─ 320 μg/mL, 0.07813 ─ 320 μg/mL and 0.03906 ─ 320 μg/mL, respectively. The limits of detection and quantification, respectively, were 0.00488 and 0.03906 μg/mL for quercetin, 0.62500 and 2.50000 μg/mL for bisdemethoxycurcumin, 0.07813 and 0.31250 μg/mL for demethoxycurcumin, and 0.03906 and 0.07813 μg/mL for curcumin. The percent relative intra day standard deviation (% RSD values were 0.432 ─ 0.806 μg/mL, 0.576 ─ 0.723 μg/ mL, 0.635 ─ 0.752 μg/mL and 0.655 ─ 0.732 μg/mL for quercetin, bisdemethoxycurcumin, demethoxycurcumin and curcumin, respectively, and those for intra day precision were 0.323 ─ 0.968 μg/mL, 0.805 ─ 0.854 μg/mL, 0.078 ─ 0.844 μg/mL and 0.275 ─ 0.829 μg/mL, respectively. The intra day accuracies were 99.589% ─ 100.821%, 98.588% ─ 101.084%, 9.289% ─ 100.88%, and 98.292% ─ 101.022% for quercetin, bisdemethoxycurcumin

  12. HPLC method for simultaneous quantitative detection of quercetin and curcuminoids in traditional chinese medicines.

    Science.gov (United States)

    Ang, Lee Fung; Yam, Mun Fei; Fung, Yvonne Tan Tze; Kiang, Peh Kok; Darwin, Yusrida

    2014-12-01

    Quercetin and curcuminoids are important bioactive compounds found in many herbs. Previously reported high performance liquid chromatography ultraviolet (HPLC-UV) methods for the detection of quercetin and curcuminoids have several disadvantages, including unsatisfactory separation times and lack of validation according the standard guidelines of the International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use. A rapid, specific, reversed phase, HPLC-UV method with an isocratic elution of acetonitrile and 2% v/v acetic acid (40% : 60% v/v) (pH 2.6) at a flow rate of 1.3 mL/minutes, a column temperature of 35°C, and ultraviolet (UV) detection at 370 nm was developed. The method was validated and applied to the quantification of different types of market available Chinese medicine extracts, pills and tablets. The method allowed simultaneous determination of quercetin, bisdemethoxycurcumin, demethoxycurcumin and curcumin in the concentration ranges of 0.00488 ─ 200 μg/mL, 0.625 ─ 320 μg/mL, 0.07813 ─ 320 μg/mL and 0.03906 ─ 320 μg/mL, respectively. The limits of detection and quantification, respectively, were 0.00488 and 0.03906 μg/mL for quercetin, 0.62500 and 2.50000 μg/mL for bisdemethoxycurcumin, 0.07813 and 0.31250 μg/mL for demethoxycurcumin, and 0.03906 and 0.07813 μg/mL for curcumin. The percent relative intra day standard deviation (% RSD) values were 0.432 ─ 0.806 μg/mL, 0.576 ─ 0.723 μg/mL, 0.635 ─ 0.752 μg/mL and 0.655 ─ 0.732 μg/mL for quercetin, bisdemethoxycurcumin, demethoxycurcumin and curcumin, respectively, and those for intra day precision were 0.323 ─ 0.968 μg/mL, 0.805 ─ 0.854 μg/mL, 0.078 ─ 0.844 μg/mL and 0.275 ─ 0.829 μg/mL, respectively. The intra day accuracies were 99.589% ─ 100.821%, 98.588% ─ 101.084%, 9.289% ─ 100.88%, and 98.292% ─ 101.022% for quercetin, bisdemethoxycurcumin, demethoxycurcumin and curcumin, respectively, and the

  13. 12 CFR 723.5 - How do you implement a member business loan program?

    Science.gov (United States)

    2010-01-01

    ... with the type of lending the credit union will be engaging in. The experience must provide the credit.... However, the actual decision to grant a loan must reside with the credit union. (b) Conflicts of Interest... program? 723.5 Section 723.5 Banks and Banking NATIONAL CREDIT UNION ADMINISTRATION REGULATIONS AFFECTING...

  14. BSN723T Prevents Atherosclerosis and Weight Gain in ApoE Knockout Mice Fed a Western Diet

    OpenAIRE

    Williams, Jarrod; Ensor, Charles; Gardner, Scott; Smith, Rebecca; Lodder, Robert

    2015-01-01

    Objective This study tests the hypothesis that BSN723T can prevent the development of hyperlipidemia and atherosclerosis in ApoE-/- knockout mice fed a Western (high fat, high cholesterol, and high sucrose) diet. BSN723T is a combination drug therapy consisting of D-tagatose and dihydromyricetin (BSN723). Background D-tagatose has an antihyperglycemic effect in animal and human studies and shows promise as a treatment for type 2 diabetes and obesity. Many claims regarding BSN723's pharmacolog...

  15. In vitro study of DNA Adduct 8-OHdG Formation by using Bisphenol A in Calf Thymus DNA and 2’-Deoxyguanosine

    Science.gov (United States)

    Budiawan; Cahaya Dani, Intan; Bakri, Ridla; Handayani, Sri; Ratna Dewi, Evi

    2018-01-01

    The in vitro study of DNA Adduct 8-OHdG Formation due to BisphenolA (BPA) as xenobiotics has been conducted by using calf thymus DNA and 2’deoxyguanosine. The method of study was conducted by incubating calf thymus DNA and 2’dG with compounds trigger to radicals in the variation of pH (7.4 and 8.4), temperature (37°C and 60°C), and BPA concentrations (2 ppm and 10 ppm). To represent the work of CYP 450 enzyme in metabolic process of xenobiotics in the body and the effect of metal presence to the formation of radicals that can lead to 8-OHdG formation, we used iron(II) solution and also fenton reagent (Fe(II) and H2O2). The DNA used has 1.8 purity ratio (checked at λ260/λ280 by using Spectrophotometry UV-Vis). The results by using HPLC method showed that BPA could interact with DNA and DNA base (represent as calf thymus and 2’dG) and potentially induced 8-OHdG formation. The presence of iron(II) metal and Fenton reagent also induced the higher 8-OHdG formation. The higher of pH, temperature and concentrations also lead to 8-OHdG formation (ranger between 4 - 70 ppb).

  16. Simultaneous determination of sesquiterpenes and pyrrolizidine alkaloids from the rhizomes of Petasites hybridus (L.) G.M. et Sch. and dietary supplements using UPLC-UV and HPLC-TOF-MS methods.

    Science.gov (United States)

    Avula, Bharathi; Wang, Yan-Hong; Wang, Mei; Smillie, Troy J; Khan, Ikhlas A

    2012-11-01

    UPLC-UV and HPLC-TOF-MS methods have been developed for the analysis of major sesquiterpenes and pyrrolizidine alkaloids from rhizomes of Petasites hybridus (L.) G.M. et Sch. (Family, Asteracea) and dietary supplements claiming to contain P. hybridus. The best results were obtained with Acquity UPLC™ HSS T3 (100 mm × 2.1 mm, I.D., 1.8 μm) column system using a gradient elution with a mobile phase consisting of ammonium formate (50mM) and acetonitrile (0.05% formic acid) at a constant flow rate of 0.25 mL/min via UPLC-UV. The newly developed method was validated according to the ICH guidelines with respect to specificity, linearity, accuracy and precision. The limits of detection were found to be 5 μg/mL and 0.1 μg/mL for pyrrolizidine alkaloids and sesquiterpenes, respectively by UPLC-UV and 0.001 and 0.01 μg/mL, respectively using HPLC-TOF-MS. The methods were successfully used to analyze different P. hybridus market products, as well as to distinguish between two other Petasites species. The total content of petasins was found to be in the range of 0.02-11.6 mg/dosage form for 15 dietary supplements and no petasins were detected in an additional six dietary supplements. Additionally, pyrrolizidine alkaloids, which are considered to be toxic for the liver, were detected in seven dietary supplements. The amount of petasin in seven dietary supplements was found to be within limits of label claim and no pyrrolizidine alkaloids were detected. HPLC-mass spectrometry coupled with electrospray ionization (ESI) interface method is described for the identification and confirmation of sesquiterpenes and pyrrolizidine alkaloids from plant extracts and dietary supplements that claim to contain P. hybridus as well as different species of Petasites. Copyright © 2012 Elsevier B.V. All rights reserved.

  17. Recent G8, G20 Inclusive Multilevel Food Governance

    Directory of Open Access Journals (Sweden)

    John Kirton

    2014-11-01

    Full Text Available Innovative, integrative, local, and business-inclusive governance for food, agriculture, nutrition, health and wealth can be strengthened through informal global institutions led by the Group of Eight (G8 and the Group of Twenty (G20. Their regular summits include the most important countries’ leaders and have a comprehensive, synergistic agenda, and impulse, as well as the flexibility and authority to link issues, factors, and actors in new ways. The G8 has increasingly addressed food, agriculture, nutrition, health, and the link among them, involved business, civil society, and low-income countries, and made decisions intended to affect the lives of the poor in many locales. The G20 has contributed to some degree in such ways too. Of particular promise is the G8’s New Alliance on Food Security and Nutrition, launched in May 2012, and the G20’s AgResults program built on commitments made in June 2010. Yet there remains much that both institutions can and should do to meet the combined, complex, food-health-wealth challenge now confronting the global community, before the next food crisis comes.

  18. Identification and determination of flavonoids, carotenoids and chlorophyll concentration in Cynodon dactylon (L.) by HPLC analysis.

    Science.gov (United States)

    Muthukrishnan, Saradha Devi; Kaliyaperumal, Ashokkumar; Subramaniyan, Annapoorani

    2015-01-01

    Cynodon dactylon (L.) is a potent medicinal plant in the traditional and current Indian medicinal systems. The objective of this research was to find out the levels of flavonoids, carotenoids and chlorophyll b in C. dactylon leaves by high-performance liquid chromatography (HPLC) equipped with a diode array detector. HPLC analysis revealed that total carotenoid and total flavonoid concentration were 62 mg/100 g and 249.1 μg/g, respectively. The mean chlorophyll b was 85.1 mg/100 g in C. dactylon. Among the flavonoids, quercetin (164.7 μg/g) was the major flavonoid followed by kaempferol (48.2 μg/g), rutin (18.4 μg/g), catechin (12.1 μg/g) and myricetin (5.7 μg/g). Of the carotenoids, β-carotene (35.2 mg/100 g) was predominant followed by lutein (17.0 mg/100 g), violaxanthin (5.8 mg/100 g) and zeaxanthin (4.2 mg/100 g). Chlorophyll b concentration was 85.1 mg/100 g in C. dactylon. The results of this investigation should be useful information for further pharmacological studies.

  19. 12 CFR 723.20 - How can a state supervisory authority develop and enforce a member business loan regulation?

    Science.gov (United States)

    2010-01-01

    ... state regulation minimizes the risk and accomplishes the overall objectives of NCUA's member business... and enforce a member business loan regulation? 723.20 Section 723.20 Banks and Banking NATIONAL CREDIT UNION ADMINISTRATION REGULATIONS AFFECTING CREDIT UNIONS MEMBER BUSINESS LOANS § 723.20 How can a state...

  20. Formation and characterization of iron-binding phosphorylated human-like collagen as a potential iron supplement.

    Science.gov (United States)

    Deng, Jianjun; Chen, Fei; Fan, Daidi; Zhu, Chenhui; Ma, Xiaoxuan; Xue, Wenjiao

    2013-10-01

    Iron incorporated into food can induce precipitation and unwanted interaction with other components in food. Iron-binding proteins represent a possibility to avoid these problems and other side effects, as the iron is protected. However, there are several technical problems associated with protein-iron complex formation. In this paper, the iron-binding phosphorylated human-like collagen (Fe-G6P-HLC) was prepared under physiological conditions through phosphorylated modification. One molecule of Fe-G6P-HLC possesses about 24 atoms of Fe. Spectroscopy analysis, differential scanning calorimetry (DSC) and equilibrium dialysis techniques were employed to investigate the characteristics of the Fe-G6P-HLC. The binding sites (nb) and apparent association constant (Kapp) between iron and phosphorylated HLC were measured at nb=23.7 and log Kapp=4.57, respectively. The amount of iron (Fe(2+) sulfate) binding to phosphorylated HLC was found to be a function of pH and phosphate content. In addition, the solubility and thermal stability of HLC were not significantly affected. The results should facilitate the utilization of HLC as a bioactive iron supplement in the food and medical industry and provide an important theoretical evidence for the application of HLC chelates. © 2013.

  1. HepG2 cells biospecific extraction and HPLC-ESI-MS analysis for screening potential antiatherosclerotic active components in Bupeuri radix.

    Science.gov (United States)

    Liu, Shuqiang; Tan, Zhibin; Li, Pingting; Gao, Xiaoling; Zeng, Yuaner; Wang, Shuling

    2016-03-20

    HepG2 cells biospecific extraction method and high performance liquid chromatography-electrospray ionization-mass spectrometry (HPLC-ESI-MS) analysis was proposed for screening of potential antiatherosclerotic active components in Bupeuri radix, a well-known Traditional Chinese Medicine (TCM). The hypothesis suggested that when cells are incubated together with the extracts of TCM, the potential bioactive components in the TCM should selectively combine with the receptor or channel of HepG2 cells, then the eluate which contained biospecific component binding to HepG2 cells was identified using HPLC-ESI-MS analysis. The potential bioactive components of Bupeuri radix were investigated using the proposed approach. Five compounds in the saikosaponins of Bupeuri radix were detected as these components selectively combined with HepG2 cells, among these compounds, two potentially bioactive compounds namely saikosaponin b1 and saikosaponin b2 (SSb2) were identified by comparing with the chromatography of the standard sample and analysis of the structural clearance characterization of MS. Then SSb2 was used to assess the uptake of DiI-high density lipoprotein (HDL) in HepG2 cells for antiatherosclerotic activity. The results have showed that SSb2, with indicated concentrations (5, 15, 25, and 40 μM) could remarkably uptake dioctadecylindocarbocyanine labeled- (DiI) -HDL in HepG2 cells (Vs control group, *PESI-MS analysis is a rapid, convenient, and reliable method for screening potential bioactive components in TCM and SSb2 may be a valuable novel drug agent for the treatment of atherosclerosis. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Sensitive detectors in HPLC

    International Nuclear Information System (INIS)

    Anon.

    1992-01-01

    Detection of sample components in HPLC is difficult for many reasons; the key difficulty is the mobile phase which usually has properties similar to the solute. A variety of detectors have been developed for use in HPLC based on one of the above approaches; however, the search is still continuing for an ideal or universal detector. A universal detector should have the following characteristics: (1) responds to all solutes or has predictable specificity; (2) high detectability and the same predictable response; (3) fast response; (4) wide range of linearity; (5) unaffected by changes in temperature and mobile-phase flow; (6) responds independently of the mobile phase; (7) makes no contribution to extracolumn band broadening; (8) reliable and convenient to use; (9) nondestructive to the solute; (10) provides qualitative information on the detected peak. Unfortunately, no available HPLC detector possesses all these properties. 145 refs

  3. A novel thiolated human-like collage zinc complex as a promising zinc supplement: physicochemical characteristics and biocompatibility.

    Science.gov (United States)

    Zhu, Chenhui; Ma, Xiaoxuan; Wang, Yonghui; Mi, Yu; Fan, Daidi; Deng, Jianjun; Xue, Wenjiao

    2014-11-01

    To improve zinc binding ability to human-like collagen (HLC) and stability of metal complex, HLC was thiolated by mercaptosuccinylation reaction with S-acetylmercaptosuccinic anhydride (S-AMSA) at pH8.0. One mole of thiolated HLC-Zn (SHLC-Zn) complex possessed 24.3mol zinc ions when pH was 8.0 and zinc concentration was 15 mM. The physicochemical properties and biocompatibility of thiolated HLC-Zn (SHLC-Zn) complex were investigated by UV-vis, CD, electrophoresis analysis, differential scanning calorimetry (DSC) and cell viability assay, respectively. The results showed that SHLC-Zn complex(1) exhibited higher zinc ions than that of native HLC and still maintained the secondary structure of HLC though interaction occurred between SHLC and zinc ions, (2) increased the apparent molecular weight when compared with native HLC, (3) exhibited greater thermal stability than native HLC, and (4) presented toxicity free for BHK cells. This study suggests that the SHLC-Zn complex is a potential nutrition as well as zinc supplement in the medical application. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. Development and Validation of a UV Spectrophotometric and a RP-HPLC Methods for Moexipril Hydrochloride in Pure Form and Pharmaceutical Dosage Form

    International Nuclear Information System (INIS)

    Mastiholimath, V.S.; Gupte, P.P.; Mannur, V.S.

    2012-01-01

    A simple and reliable UV spectrophotometric and high-performance liquid chromatography (HPLC) methods were developed and validated for Moexipril hydrochloride in pure form and pharmaceutical dosage form. The RP-HPLC method was developed on agilant eclipse C 18 , (150 mm x 4.6 mm, 5 μm) with a mobile phase gradient system of 60 % (methanol:acetonitrile (70:30 % v/v)) : 40 % 20 mM ammonium acetate buffer pH 4.5 (v/v) and UV spectrophotometric method was developed in phosphate buffer pH 6.8. The effluent was monitored by SPD-M20A, prominence PDA detector at 210 nm. Calibration curve was linear over the concentration range of 10-35 μg/ml and 1-9 μg/ml for RP-HPLC and UV with a regression coefficient of 0.999. For RP-HPLC method Inter-day and intra-day precision % RSD values were found to be 1.00078 % and 1.49408 % respectively. For UV method 0.73386 % to 1.44111 % for inter day 0.453864 to 1.15542 intra-day precision. Recovery of Moexipril hydrochloride was found to be in the range of 99.8538 % to 101.5614 % and 100.5297586 % to 100.6431587 % for UV and RP-HPLC respectively. The limits of detection (LOD) and quantification (LOQ) for HPLC were 0.98969 and 2.99907 μg/ml, respectively. The developed RP-HPLC and UV spectrophotometric method was successfully applied for the quantitative determination of Moexipril hydrochloride in pharmaceutical dosage. (author)

  5. The preparation and characterization of novel human-like collagen metal chelates

    Energy Technology Data Exchange (ETDEWEB)

    Zhu, Chenhui; Sun, Yan [Shaanxi Key Laboratory of Degradable Biomedical Materials, School of Chemical Engineering Northwest University, Xi' an 710069 (China); Shaanxi R and D Center of Biomaterials and Fermentation Engineering, Xi' an 710069 (China); Wang, Yaoyu [Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of the Ministry of Education, Xi' an 710069 (China); Luo, Yane, E-mail: luoyane@nwu.edu.cn [Shaanxi Key Laboratory of Degradable Biomedical Materials, School of Chemical Engineering Northwest University, Xi' an 710069 (China); Shaanxi R and D Center of Biomaterials and Fermentation Engineering, Xi' an 710069 (China); Fan, Daidi, E-mail: fandaidi@nwu.edu.cn [Shaanxi Key Laboratory of Degradable Biomedical Materials, School of Chemical Engineering Northwest University, Xi' an 710069 (China); Shaanxi R and D Center of Biomaterials and Fermentation Engineering, Xi' an 710069 (China)

    2013-07-01

    In order to develop the nutritional trace elements which could be absorbed and utilized effectively, protein chelates were adopted. Calcium, copper and manganese were considered based on their physiological functions, and the new chelates of HLC-Ca, HLC-Cu and HLC-Mn were formed in MOPS or MES buffer and purified by gel chromatography, and then freeze-dried. And they were detected and analyzed by atomic absorption spectrophotometry, ultraviolet–visible absorption (UV–vis) spectroscopy, Fourier transform infrared (FTIR) spectroscopy, fluorescence quenching method, circular dichroism (CD) and differential scanning calorimetry (DSC). The results showed that some chemical reactions happened between HLC and the three metal ions to form new chemical compounds. The thermodynamic parameters, ∆H, ∆G and ∆S, showed that the chelation process between HLC and metal ions was performed spontaneously. Fluorescence quenching spectra of HLC indicated that the quenching mechanism was static in nature. According to the data of DSC, the new chelates were more stable than the free HLC. And HLC-metal complex was non-toxic to the BHK21 cell through MTT assay. - Highlights: ► HLC-Ca, HLC-Cu and HLC-Mn were new chemical compounds and different to free HLC. ► Possible sites for Ca{sup 2+}, Cu{sup 2+} and Mn{sup 2+} to bind with HLC were presented. ► The chelation process between HLC and metal ions was performed spontaneously. ► The thermodynamic stability of the new chelates was higher than that of free HLC.

  6. G-index: A new metric to describe dynamic refractive index effects in HPLC absorbance detection.

    Science.gov (United States)

    Kraiczek, Karsten G; Rozing, Gerard P; Zengerle, Roland

    2018-09-01

    High performance liquid chromatography (HPLC) with a solvent gradient and absorbance detection is one of the most widely used methods in analytical chemistry. The observed absorbance baseline is affected by the changes in the refractive index (RI) of the mobile phase. Near the limited of detection, this complicates peak quantitation. The general aspects of these RI-induced apparent absorbance effects are discussed. Two different detectors with fundamentally different optics and flow cell concepts, a variable-wavelength detector equipped with a conventional flow cell and a diode-array detector equipped with a liquid core waveguide flow cell, are compared with respect to their RI behavior. A simple method to separate static - partly unavoidable - RI effects from dynamic RI effects is presented. It is shown that the dynamic RI behavior of an absorbance detector can be well described using a single, relatively easy-to-determine metric called the G-index. The G-index is typically in the order of a few seconds and its sign depends on the optical flow cell concept. Copyright © 2018 Elsevier B.V. All rights reserved.

  7. 47 CFR 90.723 - Selection and assignment of frequencies.

    Science.gov (United States)

    2010-10-01

    ... 220-222 MHz Band § 90.723 Selection and assignment of frequencies. (a) Phase II applications for frequencies in the 220-222 MHz band shall specify whether their intended use is for 10-channel nationwide... medical use. Phase II applicants for frequencies for public safety/mutual aid use or emergency medical use...

  8. Endobronchial administration of iodine-131 B72.3 monoclonal antibody in patients with lung cancer

    International Nuclear Information System (INIS)

    Del Vecchio, S.; Mansi, L.; Petrillo, A.; Camera, L.; Salvatore, M.; Sofia, M.; Marra, A.; Carratu, L.

    1991-01-01

    We tested the feasibility of endobronchial administration of radiolabelled monoclonal antibodies (MoAbs) and the biodistribution of the radiotracer. Ten patients with histological confirmed adenocarcinoma or squamous cell carcinoma were studied. Nine received 470 μCi (103 μg) of 131 I-B72.3, a monoclonal antibody reacting against TAG 72 antigen, while one patient received 502 μCi (291 μg) of 131 I-4C4, an indifferent antibody used for comparison in a negative control study. The radiolabelled antibody was administered through a flexible fiberoptic bronchoscope and placed on the tumour mass under visual monitoring. Scans with a large field-of-view gamma-camera showed retention of 131 I-B72.3 at the tumour site up to 6-9 days in six of eight patients. No other organs were visualized with the exception of faint activity in the gastrointestinal tract, bladder and thyroid. On the contrary, the indifferent antibody 131 I-4C4 was not retained at the tumour site 6 days after MoAbs administration, and more prominent activity was found in the gastrointestinal tract. In one patient the study was not technically adequate because of failure of the delivery system. The vascular compartment contained less than 3% of the administered dose. We conclude that endobronchial administration is a feasible technique and allows stable and specific targetting of bronchial tumours. Furthermore, the low activity found in the plasma and other organs suggests that this approach may be used to deliver therapeutic doses of MoAbs to lung cancers. (orig.)

  9. 40 CFR 141.723 - Requirements to respond to significant deficiencies identified in sanitary surveys performed by EPA.

    Science.gov (United States)

    2010-07-01

    ... deficiencies identified in sanitary surveys performed by EPA. 141.723 Section 141.723 Protection of Environment... performed by EPA, systems must respond in writing to significant deficiencies identified in sanitary survey... will address significant deficiencies noted in the survey. (d) Systems must correct significant...

  10. Isothermal Bainite Processing of ASTM A723 Components

    Science.gov (United States)

    1993-09-01

    4 List of Illustrations 1. Photograph of typical cylinders used in the present study ................................. 7 2. CCT diagram for... CCT ) diagram obtained by thermal and magnetic analyses for the high nickel (-3 percent) ASTM A723 steel. The bainite knee for the 2 percent nickel...block. Also shown is the slope giving the average cooling rate in the critical region of the CCT diagram . This average rate happens to approximately

  11. Echinococcus canadensis (Cestoda: Taeniidae) is a valid species consisting of the mitochondrial genotypes G6, G7, G8 and G10

    Science.gov (United States)

    The species status of Echinococcus canadensis has long been controversial, mainly because it consists of the mitochondrial genotypes G6, G7, G8 and G10 with different host affinity: G6 (camel strain) and G7 (pig strain) with domestic cycles and G8 (cervid strain) and G10 (Fennoscandian cervid strain...

  12. G-8 leaders tackle global energy security

    International Nuclear Information System (INIS)

    Quevenco, R.

    2006-01-01

    Leaders of the Group of 8 countries backed the IAEA's work at their annual summit held 15-17 July 2006 in St. Petersburg, Russia. A concluding summary statement endorsed IAEA programmes and initiatives in areas of nuclear safety, security, and safeguards. The G8 nations adopted a St. Petersburg Plan of Action to increase transparency, predictability and stability of the global energy markets, improve the investment climate in the energy sector, promote energy efficiency and energy saving, diversify energy mix, ensure physical safety of critical energy infrastructure, reduce energy poverty and address climate change and sustainable development. In a statement on global energy security, the G8 said countries who have or are considering plans for nuclear energy believe it will contribute to global energy security while reducing air pollution and addressing climate change. The G8 said it acknowledged the efforts made in development by the Generation IV International Forum (GIF) and the IAEA's International Project on Innovative Nuclear Reactors and Fuel Cycles (INPRO). GIF and INPRO both bring together countries to develop next generation nuclear energy systems, including small reactors, very high temperature reactors and supercritical water-cooled reactors. The G8 reaffirmed its full commitment to all three pillars of the NPT and called on all States to comply with their NPT obligations, including IAEA safeguards as well as developing effective measures aimed at preventing trafficking in nuclear equipment, technology and materials. The G8 is seeking universal adherence to IAEA comprehensive safeguards agreements and is actively engaged in efforts to make comprehensive safeguards agreements together with an Additional Protocol the universally accepted verification standard. The G8 noted that an expansion of the peaceful use of nuclear energy must be carried forward in a manner consistent with nuclear non-proliferation commitments and standards. It discussed concrete

  13. IEA policies-G8 recommendations and an afterwards

    International Nuclear Information System (INIS)

    Onoda, Takao

    2009-01-01

    In response to threats posed to the future supply of energy and to the environment, the G8 leaders, in Gleneagles, UK in 2005, agreed to an initiative called the Gleneagles Plan of Action (GPOA) which addresses climate change, clean energy and sustainable development. In the GPOA, G8 leaders pledged to encourage the development of cleaner, more efficient and lower-emitting vehicles, and to promote their deployment by, among other means, asking the IEA to review existing standards and codes for vehicle efficiency and to identify best practices. In order to properly response to the above-mentioned requests from G8 leaders, the IEA has launched, among other activities, study on policies for 'transforming the way we use energy' focusing on end-use efficiency including the one in transport sector and made a comprehensive response to the GPOA at the 2008 G8 Summit Meeting in Japan with 25 recommendations on energy efficiency. Regarding these recommendations, the G8 leaders have proclaimed, in the G8 Hokkaido Toyako Summit Leaders Declaration, that they would maximize implementation of the IEA's 25 recommendations. This paper summarizes the IEA activities in transport sector regarding the GPOA and their findings and recommendations.

  14. G8 SUMMIT MEETING AT EVIAN

    CERN Multimedia

    2003-01-01

    The Swiss and French authorities have informed CERN that plans are in hand for the safety and traffic arrangements associated with the G8 Summit Meeting, which will be held in Evian between 1 and 3 June 2003. Detailed information will be communicated in the coming weeks. However, changes to traffic arrangements on certain sections of the road network in the Canton of Geneva (particularly the left bank) and the neighbouring parts of France (specially Haute-Savoie) from 22 May 2003 can already be predicted. All pertinent information and any recommendations by the authorities concerned will be brought to the attention of the personnel as soon as possible. In the mean time, those concerned can consult the various Web sites devoted to this event, especially: - http://www.g8.fr/evian/english/home.html (French site); - http://www.g8info.ch/accueil.htm (Swiss site). Relations with the Host States Service http://www.cern.ch/relations/ Tel. 72848

  15. Using a simple HPLC approach to identify the enzymatic products of UTL-5g, a small molecule TNF-α inhibitor, from porcine esterase and from rabbit esterase.

    Science.gov (United States)

    Swartz, Kenneth; Zhang, Yiguan; Valeriote, Frederick; Chen, Ben; Shaw, Jiajiu

    2013-12-01

    UTL-5g is a novel small-molecule chemoprotector that lowers hepatotoxicity, nephrotoxicity, and myelotoxicity induced by cisplatin through TNF-α inhibition among other factors. As a prelude to investigating the metabolites of UTL-5g, we set out to identify the enzymatic products of UTL-5g under the treatment of both porcine liver esterase (PLE) and rabbit liver esterase (RLE). First, a number of mixtures made by UTL-5g and PLE were incubated at 25°C. At predetermined time points, individual samples were quenched by acetonitrile, vortexed, and centrifuged. The supernatants were then analyzed by reversed-phase HPLC (using a C18 column). The retention times and UV/vis spectra of individual peaks were compared to those of UTL-5g and its two postulated enzymatic products; thus the enzymatic products of UTL-5g were tentatively identified. Secondly, a different HPLC method (providing different retentions times) was used to cross-check and to confirm the identities of the two enzymatic products. Based on the observations, it was concluded that under the treatment of PLE, the major enzymatic products of UTL-5g were 5-methyliosxazole-3-carboxylic acid (ISOX) and 2,4-dichloroaniline (DCA). Treatment of UTL-5g by RLE also provided the same enzymatic products of UTL-5g from esterase. These results indicate that the peptide bond in UTL-5g was cleaved by PLE/RLE. Michaelis-Menten kinetics showed that the Km values of UTL-5g were 2.07mM with PLE and 0.37mM with RLE indicating that UTL-5g had a higher affinity with RLE. In summary, by a simple HPLC approach, we have concluded that the peptide bond in UTL-5g was cleaved by esterase from either porcine liver or rabbit liver in vitro and afforded DCA (at a mole ratio of 1:1) and ISOX. However, further studies are needed in order to determine whether UTL-5g is metabolized by microsomal enzymes to produce ISOX and DCA. Copyright © 2013 Elsevier B.V. All rights reserved.

  16. G8 Regional Security Governance through Sanctions and Force

    Directory of Open Access Journals (Sweden)

    John Kirton

    2014-11-01

    Full Text Available Why do the Group of Eight (G8 members approve its members’ use of material sanctions in some regional conflicts but military force in others?2 As an informal security institution composed of major democratic powers from North America, Europe and Asia, the G8 has often chosen sanctions, notably on Iran in 1980, Afghanistan in 1980, Sudan in 2004, North Korea in 2006, and Syria in 2011. It has increasingly chosen military force, notably in Iraq in 1990, Kosovo in 1999, the USSR over Afghanistan in 2001, Libya in 2011, and Mali in 2013. Yet the G8’s choice, initiation, commitment, compliance, implementation and effectiveness of both sanctions and force has varied. Force was chosen and used effectively only in the post cold war period, primarily where the target was close to southern Europe. A high relative-capability predominance of G8 members over the target country strongly produces the G8’s choice of force, but a high, direct, deadly threat from the target state to G8 countries does not. Geographic proximity and the connectivity coming from the former colonial relationship between G8 members and the target country only weakly cause the G8 to choose force. Support from the most relevant regional organization – the North Atlantic Treaty Organization – and support from the United Nations in the form of an authorizing UN Security Council or General Assembly resolution have a strong, positive effect on the G8’s choice of force. Accompanying accountability mechanisms from the G8 itself have a variable impact, as leaders’ iteration of the issue at subsequent summits does not increase compliance with G8 commitments on force-related cases, but their foreign ministers’ follow up does to a substantial degree.

  17. G8 global partnership. 2004-2005-2006 activity report; Partenariat mondial du G8. Rapport d'activite 2004-2005-2006

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2007-07-01

    The Global Partnership Against the Spread of Weapons and Materials of Mass Destruction was launched by the heads of state and government of the G8 at the G8 summit in Kananaskis in June 2002. Fourteen other countries have since joined this G8 initiative. The aim of this partnership is to 'prevent terrorists, or those who harbor them, from acquiring or developing nuclear, chemical radiological and biological weapons, missiles, and related materials, equipment and technology'. Within the framework of the Partnership, the participants have agreed to support cooperation projects, starting with Russia, to promote non-proliferation, disarmament, the fight against terrorism and nuclear safety. The destruction of chemical weapons, the dismantling of decommissioned nuclear submarines, the disposal of fissile materials and the employment of former weapons scientists are among the priority concerns expressed. Ukraine has also been a beneficiary of this partnership since 2004. The participants in this initiative have agreed to contribute up to 20 billion dollars (up to 750 million euros from France) to support these projects over a period of ten years from 2002. A group of experts from the G8 on the Global Partnership (the GPWG = Global Partnership Working Group) meets regularly and gives an account of the progress made with this initiative in its annual report to the G8. These annual reports are published at the G8 summits. This document is the 2004 to 2006 activity report of the G8 global partnership.

  18. 20 CFR 404.723 - When evidence of marriage is required.

    Science.gov (United States)

    2010-04-01

    ... 20 Employees' Benefits 2 2010-04-01 2010-04-01 false When evidence of marriage is required. 404... DISABILITY INSURANCE (1950- ) Evidence Evidence of Age, Marriage, and Death § 404.723 When evidence of marriage is required. If you apply for benefits as the insured person's husband or wife, widow or widower...

  19. Qualitative and Quantitative Analysis of Lignan Constituents in Caulis Trachelospermi by HPLC-QTOF-MS and HPLC-UV

    Directory of Open Access Journals (Sweden)

    Xiao-Ting Liu

    2015-05-01

    Full Text Available A high-performance liquid chromatography coupled with quadrupole tandem time-of-flight mass (HPLC-QTOF-MS and ultraviolet spectrometry (HPLC-UV was established for simultaneous qualitative and quantitative analysis of the major chemical constituents in Caulis Trachelospermi, respectively. The analysis was performed on an Agilent Zorbax Eclipse Plus C18 column (4.6 mm × 150 mm, 5 μm using a binary gradient system of water and methanol, with ultraviolet absorption at 230 nm. Based on high-resolution ESI-MS/MS fragmentation behaviors of the reference standards, the characteristic cleavage patterns of lignano-9, 9'-lactones and lignano-8'-hydroxy-9, 9'-lactones were obtained. The results demonstrated that the characteristic fragmentation patterns are valuable for identifying and differentiating lignano-9,9'-lactones and lignano-8'-hydroxy-9,9'-lactones. As such, a total of 25 compounds in Caulis Trachelospermi were unambiguously or tentatively identified via comparisons with reference standards or literature. In addition, 14 dibenzylbutyrolatone lignans were simultaneously quantified in Caulis Trachelospermi by HPLC-UV method. The method is suitable for the qualitative and quantitative analyses of dibenzylbutyrolatone lignans in Caulis Trachelospermi.

  20. Evaluation of XD/A Plus and ST8G films for cephalometric radiography with Grenex G8 and BH-III screens.

    Science.gov (United States)

    Wakoh, M; Farman, A G; Scarfe, W C; Shibuya, H; Nishikawa, K; Kuroyanagi, K

    1997-02-01

    Sensitometric properties, clinical image quality, and patient dose requirements are important considerations when selecting film for cephalometrics. Two recently released films, XD/A Plus and ST 8G green sensitive films, were studied. The films were each combined with Grenex G8 (Fuji Medical) green-fluorescing matched and BH-III (Kasei Optonix) blue-fluorescing mismatched intensifying screens. The density response and resolution for each screen-film combination were evaluated by use of the characteristic curve and modulation transfer function. The kilovoltage settings providing clinically acceptable images were assessed individually by 12 observers. Clinically acceptable images for each combination were also compared, and the skin entrance doses in the temporomandibular joint region were determined. The average contrast at the most effective density range was found to be slightly higher for the BH-III group than for the G8 group. The modulation transfer function for the BH-III group was inferior to that for the G8 screens. There were no significant differences in diagnostically acceptable image quality among the four combinations; nevertheless the BH-III screen group required two to three times more exposure than the G8 screen group. XD/A Plus and ST8G films provide acceptable image detail for cephalometrics. To minimize the patient dose they should be used with green-emitting screens.

  1. Comparison of piracetam measured with HPLC-DAD, HPLC-ESI-MS, DIP-APCI-MS, and a newly developed and optimized DIP-ESI-MS.

    Science.gov (United States)

    Lenzen, Claudia; Winterfeld, Gottfried A; Schmitz, Oliver J

    2016-06-01

    The direct inlet probe-electrospray ionization (DIP-ESI) presented here was based on the direct inlet probe-atmospheric pressure chemical ionization (DIP-APCI) developed by our group. It was coupled to an ion trap mass spectrometer (MS) for the detection of more polar compounds such as degradation products from pharmaceuticals. First, the position of the ESI tip, the gas and solvent flow rates, as well as the gas temperature were optimized with the help of the statistic program Minitab® 17 and a caffeine standard. The ability to perform quantitative analyses was also tested by using different concentrations of caffeine and camphor. Calibration curves with a quadratic calibration regression of R (2) = 0.9997 and 0.9998 for caffeine and camphor, respectively, were obtained. The limit of detection of 2.5 and 1.7 ng per injection for caffeine and camphor were determined, respectively. Furthermore, a solution of piracetam was used to compare established analytical methods for this drug and its impurities such as HPLC-diode array detector (DAD) and HPLC-ESI-MS with the DIP-APCI and the developed DIP-ESI. With HPLC-DAD and 10 μg piracetam on column, no impurity could be detected. With HPLC-ESI-MS, two impurities (A and B) were identified with only 4.6 μg piracetam on column, while with DIP-ESI, an amount of 1.6 μg piracetam was sufficient. In the case of the DIP-ESI measurements, all detected impurities could be identified by MS/MS studies. Graphical Abstract Scheme of the DIP-ESI principle.

  2. Clinical and Molecular Characteristics of Human Rotavirus G8P[8] Outbreak Strain, Japan, 2014.

    Science.gov (United States)

    Kondo, Kenji; Tsugawa, Takeshi; Ono, Mayumi; Ohara, Toshio; Fujibayashi, Shinsuke; Tahara, Yasuo; Kubo, Noriaki; Nakata, Shuji; Higashidate, Yoshihito; Fujii, Yoshiki; Katayama, Kazuhiko; Yoto, Yuko; Tsutsumi, Hiroyuki

    2017-06-01

    During March-July 2014, rotavirus G8P[8] emerged as the predominant cause of rotavirus gastroenteritis among children in Hokkaido Prefecture, Japan. Clinical characteristics were similar for infections caused by G8 and non-G8 strains. Sequence and phylogenetic analyses suggest the strains were generated by multiple reassortment events between DS-1-like P[8] strains and bovine strains from Asia.

  3. Gradient Scouting in Reversed-Phase HPLC Revisited

    Science.gov (United States)

    Alcazar, A.; Jurado, J. M.; Gonzalez, A. G.

    2011-01-01

    Gradient scouting is the best way to decide the most suitable elution mode in reversed-phase high-performance liquid chromatography (RP-HPLC). A simple rule for this decision involves the evaluation of the ratio [delta]t/t[subscript G] (where [delta]t is the difference in the retention time between the last and the first peak and t[subscript G] is…

  4. Ratio of involved/uninvolved immunoglobulin quantification by Hevylite™ assay: clinical and prognostic impact in multiple myeloma

    Directory of Open Access Journals (Sweden)

    Koulieris Efstathios

    2012-04-01

    Full Text Available Abstract Background HevyLite™ is a new, recently developed method that facilitates separate quantification of the kappa- and lambda-bounded amounts of a given immunoglobulin (Ig. Using this method, we measured intact immunoglobulin (heavy/light chain; HLC IgG-kappa, IgG-lambda, IgA-kappa, IgA-lambda individually, as well as their deriving ratios (HLCR in a series of IgG or IgA multiple myeloma (MM patients, to investigate and assess the contribution of these tests to disease evaluation. Patients and methods HevyLite™ assays were used in sera from 130 healthy individuals (HI and 103 MM patients, at time of diagnosis. In patients, the level of paraprotein was IgG in 78 (52 IgG-kappa, 26 IgG-lambda and IgΑ in 25 (13 IgΑ-kappa, 12 IgΑ-lambda. Durie-Salmon and International Staging System stages were evenly distributed. Symptomatic patients (n = 77 received treatment while asymptomatic ones (n = 26 were followed. Patients' median follow-up was at 32.6 months. HLCR was calculated with the involved Ig (either G or A as numerator. Results In HI, median IgG-kappa was 6.85, IgG-lambda 3.81, IgA-kappa 1.19 and IgA-lambda 0.98 g/L. The corresponding median involving HLC values in MM patients were 25.8, 23.45, 28.9 and 36.4 g/L. HLC-IgG related to anemia, high serum free light chain ratio and extensive bone marrow infiltration, while high HLCR correlated with the same plus increased β2-microglobulin. In addition, increased HLCR and the presence of immunoparesis correlated with time to treatment. Patients with high HLCR had a significantly shorter survival (p = 0.022; HLCR retained its prognostic value in multivariate analysis. Conclusions HLC and HLCR quantify the precise amount of the involved immunoglobulin more accurately than other methods; moreover, they carry prognostic information regarding survival in MM patients.

  5. The mutation frequency of 8-oxo-7,8 dihydroguanine (8-oxoG) situated in a multiply damaged site: comparison of a single and two closely opposed 8-oxodG in Escherichia coli

    International Nuclear Information System (INIS)

    Malyarchuk, S.G.; Youngblood, R.C.; Landry, A.M.; Quillin, E.; Harrison, L.

    2003-01-01

    Full text: A multiply damaged site (MDS) is defined as >= two lesions within a distance of 10-15 base pairs (bp). MDS generated by ionizing radiation contains oxidative base damage, and in vitro studies have indicated that if the base damage is less than 3 bp apart, repair of one lesion is inhibited until repair of the lesion in the opposite strand is completed. Inhibition of repair could result in an increase in the mutation frequency of the base damage. We have designed an assay to determine whether a closely opposed lesion causes an increase in adenine insertion opposite an 8-oxodG in bacteria. The double-stranded oligonucleotides (with no damage, each single 8-oxodG or the MDS) were ligated into the firefly luciferase coding region of a reporter vector and transformed into wild type or MutY-deficient bacteria. The MDS contained an 8-oxodG in the transcribed strand (T) and a second 8-oxodG immediately 5' to this lesion in the non-transcribed strand (NT). During two rounds of replication, insertion of adenine opposite the 8-oxodG in the T or NT strand results in a translation termination codon at position 444 or 445, respectively. In wild-type bacteria, we detected a translation stop at a frequency of 0.15% (codon 444) and 0.09% (codon 445) with a single 8-oxodG in the T or NT strand, respectively. This was enhanced ∼3 fold when single lesions were replicated in MutY-deficient bacteria. Positioning an 8-oxodG in the T strand within the MDS enhanced the mutation frequency by ∼2 fold in wild-type bacteria and 8 fold in Mut Y-deficient bacteria, while the mutation frequency of the 8-oxodG in the NT strand increased by 6 fold in Mut Y-deficient bacteria. This enhancement of mutation frequency supports the in vitro MDS studies, which demonstrated the inability of base excision repair to completely repair closely opposed lesions

  6. 8-Hydroxydeoxyguanosine as a urinary biomarker of oxidative DNA damage

    DEFF Research Database (Denmark)

    Loft, S; Fischer-Nielsen, A; Jeding, I B

    1993-01-01

    and in various laboratory animals, including dog, pig, and rat. Previously, other groups have used comparable HPLC methods or gas chromatography-mass spectrometry with selective ion monitoring for measuring the excretion of 8OHdG in humans, rats, mice, and monkeys. In the 169 humans studied so far, the average 8...

  7. Ilves : mida põrgut teeb Venemaa G8-s?

    Index Scriptorium Estoniae

    2007-01-01

    President Toomas Hendrik Ilves viibis Prahas 4. ja 5. juunil 2007 toimunud konverentsil "Demokraatia ja julgeolek", kus ta seadis kahtluse alla selle, kas Euroopat rakettidega ähvardava Venemaa koht on ikka G8-s ja Euroopa Nõukogus. Ilmunud ka: Eesti Elu 8. juuni 2007, lk. 1,4, pealk.: Mida teeb Venemaa G8-s?, ingl. k. lk. 9, pealk.: Ilves: what is Russia doing in the G8? Vabariigi President töövisiidil Prahasse 4.-6.06.2007

  8. G8 global partnership. 2004-2005-2006 activity report

    International Nuclear Information System (INIS)

    2007-01-01

    The Global Partnership Against the Spread of Weapons and Materials of Mass Destruction was launched by the heads of state and government of the G8 at the G8 summit in Kananaskis in June 2002. Fourteen other countries have since joined this G8 initiative. The aim of this partnership is to 'prevent terrorists, or those who harbor them, from acquiring or developing nuclear, chemical radiological and biological weapons, missiles, and related materials, equipment and technology'. Within the framework of the Partnership, the participants have agreed to support cooperation projects, starting with Russia, to promote non-proliferation, disarmament, the fight against terrorism and nuclear safety. The destruction of chemical weapons, the dismantling of decommissioned nuclear submarines, the disposal of fissile materials and the employment of former weapons scientists are among the priority concerns expressed. Ukraine has also been a beneficiary of this partnership since 2004. The participants in this initiative have agreed to contribute up to 20 billion dollars (up to 750 million euros from France) to support these projects over a period of ten years from 2002. A group of experts from the G8 on the Global Partnership (the GPWG = Global Partnership Working Group) meets regularly and gives an account of the progress made with this initiative in its annual report to the G8. These annual reports are published at the G8 summits. This document is the 2004 to 2006 activity report of the G8 global partnership

  9. How to effectively design public health interventions: Implications from the interaction effects between socioeconomic status and health locus of control beliefs on healthy dietary behaviours among US adults.

    Science.gov (United States)

    Jang, Kyungeun; Baek, Young Min

    2018-04-16

    This study investigated whether individuals with different socioeconomic status (SES) should be provided differently tailored health messages to promote healthy dietary behaviour (HDB). Prior research has suggested that people with different SESs tend to exhibit different types of beliefs about health, but it remains unclear how SES interacts with these beliefs to influence health outcomes. To better understand the differences in HDB between high- and low-SES populations and propose effective intervention strategies, we examined (i) how SES is associated with HDB, (ii) how internal health locus of control (HLC) and powerful others HLC are associated with HDB, and (iii) how SES interacts with internal and powerful others HLC to influence HDB. Using data from the Annenberg National Health Communication Survey, collected from 2005 to 2012 (N = 6,262) in the United States, hierarchical multiple regression analyses were conducted. Education level was found to be positively associated with HDB, while income level was not. Both internal and powerful others HLC beliefs were positively associated with HDB. The positive relationship between internal HLC and HDB strengthened as the level of education and income increased, whereas the positive relationship between powerful others HLC and HDB weakened as respondents' education level increased. These results suggest that the design and delivery of communication messages should be tailored to populations' specific SES and HLC beliefs for effective public health interventions. For example, messages enhancing internal HLC (e.g. providing specific skills and knowledge about health behaviours) might be more helpful for the richer and more-educated, while messages appealing to one's powerful others HLC beliefs (e.g. advice on health lifestyles given by well-known health professionals) might be more effective for less-educated people. © 2018 John Wiley & Sons Ltd.

  10. Determination of boron in nuclear materials at subppm levels by high pressure liquid chromatography (HPLC)

    International Nuclear Information System (INIS)

    Rao, Radhika M.; Aggarwal, S.K.

    2002-11-01

    Experiments were conducted for the determination of boron in U 3 O 8 powder, aluminium metal and milliQ water using dynamically modified Reversed Phase High Pressure Liquid Chromatography (RP-HPLC) and using two precolumn chromogenic agents viz. chromotropic acid and curcumin for complexing boron. The complex was separated from the excess of reagent and determined by HPLC. When present in subppm levels, chromotropic acid was used successfully only for determination boron in water samples. For determination of boron at subppm levels in uranium and aluminium samples, curcumin was used as the precolumn chromogenic agent. The boron curcumin complex (rosocyanin) was formed after extraction of boron with 2-ethyl-l, 3-hexane diol (EHD). The rosocyanin complex was then separated from excess curcumin by displacement chromatography. Linear calibration curves for boron amounts in the range of 0.02 μg to 0.5 μg were developed with correlation coefficients varying from 0.997 to 0.999 and were used for the determination of boron in aluminium and uranium samples. Precision of about 10% was achieved in samples containing less than 1 ppmw of boron. Detection limit of this method is 0.01 μg boron. (author)

  11. Stability-Indicating Validated HPLC Method for Analysis of Berberine Hydrochloride and Trimethoprim in Pharmaceutical Dosage Form

    Directory of Open Access Journals (Sweden)

    Jing-Chun Wang

    2013-01-01

    Full Text Available A stability-indicating HPLC method was developed and validated for the determination of berberine hydrochloride and trimethoprim in pharmaceutical dosage form in the presence of degradation products. The proposed RP-HPLC method utilizes an Agilent TC-C18, 4.6 mm × 250 mm, 5 μm, column using a mobile phase consisting of acetonitrile-50 mM potassium dihydrogen phosphate (30 : 70, v/v, pH adjusted to 3 with orthophosphoric acid at a flow rate of 1.0 mL/min and UV detection at 271 nm. The linearity of berberine hydrochloride and trimethoprim was in the range of 2 to 60 μg/mL (r=0.9996 and 1 to 30 μg/mL (r=0.9995, respectively. Repeatability and intermediate precisions were also determined with percentage relative standard deviation (% RSD less than 2.0%. The limits of detection were found to be 9.8 ng/mL for berberine hydrochloride and 2.5 ng/mL for trimethoprim. The mean recoveries for berberine hydrochloride and trimethoprim were 99.8 and 98.8%, respectively. The stability of the two drugs was determined under different conditions and the proposed method has shown effective separation for their degradation products. And the proposed assays method can thus be considered stability-indicating.

  12. HPLC analysis of 4',5'-monoadduct formation in calf thymus DNA and synthetic polynucleotides treated with UVA and 8-methoxypsoralen

    International Nuclear Information System (INIS)

    Gasparro, F.P.; Bagel, J.; Edelson, R.L.

    1985-01-01

    8-methoxypsoralen monoadduct formation in calf thymus DNA irradiated with subbands of ultraviolet A light has been quantitated by HPLC analysis of the enzymatic hydrolysates of the DNA. Normalization of the yield of monoadducts for the variation in source output and the absorptivity of 8-MOP at each of the irradiating wavelengths showed that the 4',5'-furan monoadduct was the principal photoproduct and the efficiency of its formation was independent of irradiating wavelength. Synthetic polynucleotides irradiated with ultraviolet A light demonstrated a base composition and sequence dependence for 8-MOP photoreactivity: (poly(dAdT.dAdT)>poly(dA.dT)>poly(dGdC.dGdC) in both the B and Z forms>poly(dT). (author)

  13. HPLC assay for 2-(3-aminopropylamino)ethanethiol (WR-1065) in plasma

    International Nuclear Information System (INIS)

    McGovern, E.P.; Swynnerton, N.F.; Steele, P.D.; Mangold, D.J.

    1984-01-01

    A high pressure liquid chromatography (HPLC) plasma assay for WR-1065 is described which is both precise and accurate throughout the concentration range from 1 to 500 μg/mL of plasma. The analyte is separated by HPLC and detected with a thiol specific electrochemical transducer cell. The detector response is linear over the ranges 1 to 10 μg/mL, 10 to 100 μg/mL, and 100 to 500 μg/mL. The absolute retention times for WR-1065 and WT-1729 are 9 and 12 minutes, respectively. The assay uses 100 μL of plasma and requires a total chromatography cycle time of 40 minutes. The method has been found suitable for the determination of WR-1065 in plasma from a beagle dog after i.v. administration of S-2-(3-aminopropylamino)ethyl phosphorothioate (WR-2721)

  14. Russkije idut, no eto skoreje G7, a ne G8 / Brian Love

    Index Scriptorium Estoniae

    Love, Brian

    2005-01-01

    Venemaa ületab takistuse maailma suurriigina tunnustamises 2006. a. jaanuaris, kui ta aastaks saab G8 eesistujaameti. Vaatamata toimunud muutustele on Venemaa endiselt külaline, kui kohtuvad G7 rahandusministrid ja keskpankade juhid

  15. 12 CFR 563g.8 - Use of the offering circular.

    Science.gov (United States)

    2010-01-01

    ... 12 Banks and Banking 5 2010-01-01 2010-01-01 false Use of the offering circular. 563g.8 Section 563g.8 Banks and Banking OFFICE OF THRIFT SUPERVISION, DEPARTMENT OF THE TREASURY SECURITIES OFFERINGS § 563g.8 Use of the offering circular. (a) An offering circular or amendment declared effective by the...

  16. Investigating Pigment Radicals in Black Rice Using HPLC and Multi-EPR.

    Science.gov (United States)

    Nakagawa, Kouichi; Maeda, Hayato

    2017-01-01

    We investigated the location and distribution of paramagnetic species in black and white rice using electron paramagnetic resonance (EPR), X-band (9 GHz) EPR imaging (EPRI), and HPLC. EPR primarily detected two paramagnetic species in black rice, which were identified as a stable radical and Mn 2+ species, based on the g values and hyperfine components of the EPR signals. The signal from the stable radical appeared at g ≈ 2.00 and was relatively strong and stable. Subsequent noninvasive two-dimensional (2D) EPRI revealed that this stable radical was primarily located in the pigmented region of black rice, while very few radicals were observed in the rice interior. Pigments extracted from black rice were analyzed using HPLC; the major compound was found to be cyanidin-3-glucoside. EPR and HPLC results indicate that the stable radical was only found within the pigmented region of the rice, and that it could either be cyanidin-3-glucoside, or one of its oxidative decomposition products.

  17. A fatal forensic intoxication with fenarimol: analysis by HPLC/DAD/MSD.

    Science.gov (United States)

    Proença, P; Pinho Marques, E; Teixeira, H; Castanheira, F; Barroso, M; Avila, S; Vieira, D N

    2003-04-23

    Fenarimol (Rubigan) is a pyrimidine ergosterol biosynthesis inhibitor used as a systemic fungicide. The authors present a fatal fenarimol intoxication case analysed in the Forensic Toxicology Service of the National Institute of Legal Medicine. The results were used to compare two different HPLC techniques, regarding selectivity and sensitivity: an HPLC system with a diode array detector (DAD) and an HPLC system with a DAD and a mass spectrometry detector (MSD) with an electrospray interface. All biological samples were submitted to a solid-phase extraction procedure. The detection and quantification limits of fenarimol, linearity, precision and accuracy were evaluated. The fenarimol concentration levels determined were of 89.0 mg/ml in gastric contents, 1.9 mg/g in liver and 0.4 mg/g in kidney. Blood was not available at autopsy. No published data related to fenarimol self-poisoning were found, so it was not possible to interpret the results obtained by comparison with toxic/lethal levels.

  18. Reversed Phase HPLC-DAD Profiling of Carotenoids, Chlorophylls and Phenolic Compounds in Adiantum capillus-veneris Leaves

    Science.gov (United States)

    Zeb, Alam; Ullah, Fareed

    2017-04-01

    Adiantum capillus-veneris is important endangered fern species with several medicinal properties. In this study, the leaves samples were extracted and separated using reversed phase HPLC with DAD for carotenoids, chlorophylls and phenolic compounds. Separation of carotenoids and chlorophylls were carried out using a tertiary gradient system of water, MTBE and methanol-water, while a binary gradient system of methanol-water-acetic acid was used for phenolic profiling. Results revealed eight carotenoids, four pheophytins and two chlorophylls. Lutein (806.0 µg/g), chlorophyll b' (410.0 µg/g), chlorophyll a (162.4 µg/g), 9'-Z-neoxanthin (142.8 µg/g) and all-E-violaxanthin (82.2 µg/g)) were present in higher amounts. The relatively high amounts of lutein may be one of the key indicator of beneficial antioxidant properties. The phenolic profile revealed a total of thirteen compounds, namely p-hydroxybenzoic acid, chlorogenic acid, caftaric acid, kaempferol glycosides, p-coumaric acid, rosmarinic acid, 5-caffeoylquinic acid, and quercetin glycosides. Kaempferol-3-sophorotrioside (58.7 mg/g), chlorogenic acid (28.5 mg/g), 5-O-caffeoylquinic acid (18.7 mg/g), coumaric acid (11.2 mg/g) and its derivative (33.1 mg/g) were present in high amounts. These results suggest that the reversed phase HPLC profiling of adiantum leaves provides a better understanding in to the actual composition of bioactive compounds, which may be responsible for possible medicinal properties. Adiantum leaves rich in important bioactive phytochemicals can be used as a potential source of nutraceuticals or as a functional food ingredient.

  19. Reversed Phase HPLC-DAD Profiling of Carotenoids, Chlorophylls and Phenolic Compounds in Adiantum capillus-veneris Leaves

    Directory of Open Access Journals (Sweden)

    Alam Zeb

    2017-04-01

    Full Text Available Adiantum capillus-veneris is important endangered fern species with several medicinal properties. In this study, the leaves samples were extracted and separated using reversed phase HPLC with DAD for carotenoids, chlorophylls and phenolic compounds. Separation of carotenoids and chlorophylls were carried out using a tertiary gradient system of water, MTBE and methanol-water, while a binary gradient system of methanol-water-acetic acid was used for phenolic profiling. Results revealed eight carotenoids, four pheophytins, and two chlorophylls. Lutein (806.0 μg/g, chlorophyll b′ (410.0 μg/g, chlorophyll a (162.4 μg/g, 9′-Z-neoxanthin (142.8 μg/g and all-E-violaxanthin (82.2 μg/g were present in higher amounts. The relatively high amounts of lutein may be one of the key indicator of beneficial antioxidant properties. The phenolic profile revealed a total of 13 compounds, namely 4-hydroxybenzoic acid, chlorogenic acid, caftaric acid, kaempferol glycosides, p-coumaric acid, rosmarinic acid, 5-caffeoylquinic acid, and quercetin glycosides. Kaempferol-3-sophorotrioside (58.7 mg/g, chlorogenic acid (28.5 mg/g, 5-O-caffeoylquinic acid (18.7 mg/g, coumaric acid (11.2 mg/g, and its derivative (33.1 mg/g were present in high amounts. These results suggest that the reversed phase HPLC profiling of Adiantum leaves provides a better understanding in to the actual composition of bioactive compounds, which may be responsible for the potential medicinal properties. Adiantum leaves rich in important bioactive phytochemicals can be used as a possible source of nutraceuticals or as a functional food ingredient.

  20. Effect of Tris-acetate buffer on endotoxin removal from human-like collagen used biomaterials

    International Nuclear Information System (INIS)

    Zhang, Huizhi; Fan, Daidi; Deng, Jianjun; Zhu, Chenghui; Hui, Junfeng; Ma, Xiaoxuan

    2014-01-01

    Protein preparation, which has active ingredients designated for the use of biomaterials and therapeutical protein, is obtained by genetic engineering, but products of genetic engineering are often contaminated by endotoxins. Because endotoxin is a ubiquitous and potent proinflammatory agent, endotoxin removal or depletion from protein is essential for researching any biomaterials. In this study, we have used Tris-acetate (TA) buffer of neutral pH value to evaluate endotoxins absorbed on the Pierce high-capacity endotoxin removal resin. The effects of TA buffer on pH, ionic strength, incubation time as well as human-like collagen (HLC) concentration on eliminating endotoxins are investigated. In the present experiments, we design an optimal method for TA buffer to remove endotoxin from recombinant collagen and use a chromogenic tachypleus amebocyte lysate (TAL) test kit to measure the endotoxin level of HLC. The present results show that, the endotoxins of HLC is dropped to 8.3 EU/ml at 25 mM TA buffer (pH 7.8) with 150 mM NaCl when setting incubation time at 6 h, and HLC recovery is about 96%. Under this experimental condition, it is proved to exhibit high efficiencies of both endotoxin removal and collagen recovery. The structure of treated HLC was explored by Transmission Electron Microscopy (TEM), demonstrating that the property and structure of HLC treated by TA buffer are maintained. Compared to the most widely used endotoxin removal method, Triton X-114 extraction, using TA buffer can obtain the non-toxic HLC without extra treatment for removing the toxic substances in Triton X-114. In addition, the present study aims at establishing a foundation for further work in laboratory animal science and providing a foundation for medical grade biomaterials. - Graphical abstract: The processes of endotoxins adsorbed from HLC. - Highlights: • TA buffer is a mild buffer system for endotoxins removal of HLC. • TA buffer may facilitate endotoxins adsorbed on the

  1. 12 CFR 723.3 - What are the requirements for construction and development lending?

    Science.gov (United States)

    2010-01-01

    ... AFFECTING CREDIT UNIONS MEMBER BUSINESS LOANS § 723.3 What are the requirements for construction and... following additional requirements. (a) The aggregate of the net member business loan balances for all... associated member-borrowers, irrespective of the existence of a contractual commitment from a prospective...

  2. Mucins CA 125, CA 19.9, CA 15.3 and TAG-72.3 as tumor markers in patients with lung cancer: comparison with CYFRA 21-1, CEA, SCC and NSE.

    Science.gov (United States)

    Molina, Rafael; Auge, Jose Maria; Escudero, Jose Miguel; Marrades, Ramon; Viñolas, Nuria; Carcereny, Emilio; Ramirez, Jose; Filella, Xavier

    2008-01-01

    Tumor marker serum levels were prospectively studied in 289 patients with suspected, but unconfirmed, lung cancer and in 513 patients with lung cancer [417 non-small cell lung cancer (NSCLC) patients and 96 small cell lung cancer (SCLC) patients]. In patients with benign disease, abnormal serum levels were found for the following tumor markers: CEA (in 6.6% of patients); CA 19.9 (6.2%); CA 125 (28.7%); NSE (0.7%); CYFRA (8.7%); TAG-72.3 (4.2%); SCC (3.5%), and CA 15.3 (3.5%). Excluding patients with renal failure or liver diseases, tumor marker specificity improved with abnormal levels in 0.5% for NSE, 0.9% for SCC, 2.8% for CEA, CA 15.3 and TAG-72.3, 3.8% for CA 19.9, 4.2% for CYFRA and 21.4% for CA 125. Excluding CA 125, one of the markers was abnormal in 15% of patients without malignancy. Tumor marker sensitivity was related to cancer histology and tumor extension. NSE had the highest sensitivity in SCLC and CYFRA and CEA in NSCLC. Significantly higher concentrations of CEA, SCC, CA 125, CA 15.3 and TAG-72.3 were found in NSCLC than in SCLC. Likewise, significantly higher CEA (p tumors. Using a combination of 3 tumor markers (CEA, CYFRA 21-1 in all histologies, SCC in squamous tumors and CA 15.3 in adenocarcinomas), a high sensitivity may be achieved in all histological types. Tumor markers may be useful in the histological differentiation of NSCLC and SCLC. Using specific criteria for the differentiation of SCLC and NSCLC, the sensitivity was 84.2 and 68.8%, the specificity was 93.8 and 99.7%, the positive predictive value was 98.3 and 98.5% and the negative predictive value was 57.7 and 93.3%, respectively. Copyright 2008 S. Karger AG, Basel.

  3. Analysis of xanthophylls in corn by HPLC.

    Science.gov (United States)

    Moros, E E; Darnoko, D; Cheryan, M; Perkins, E G; Jerrell, J

    2002-10-09

    An HPLC method was developed using the C-30 carotenoid column to separate and identify the major xanthophylls in corn (lutein, zeaxanthin, and beta-cryptoxanthin). A photodiode array detector and a mobile phase consisting of methyl tert-butyl ether/methanol/water was used. All three xanthophylls eluted in less than 25 min. Yellow dent corn had a total xanthophyll content of 21.97 microg/g with lutein content of 15.7 microg/g, zeaxanthin content of 5.7 microg/g, and beta-cryptoxanthin of 0.57 microg/g. Commercial corn gluten meal had a 7 times higher concentration of xanthophylls (145 microg/g), and deoiled corn contained 18 microg/g, indicating that the xanthophylls are probably bound to the zein fraction of corn proteins.

  4. Urinary 8-oxo-7,8-dihydro-2'-deoxyguanosine analysis by an improved ELISA: An inter-laboratory comparison study

    Czech Academy of Sciences Publication Activity Database

    Rössner ml., Pavel; Orhan, H.; Koppen, G.; Sakai, K.; Santella, R. M.; Ambrož, Antonín; Rössnerová, Andrea; Šrám, Radim; Ciganek, M.; Neca, J.; Arzuk, E.; Mutlu, N.; Cooke, M.S.

    2016-01-01

    Roč. 95, č. 2016 (2016), s. 169-179 ISSN 0891-5849 R&D Projects: GA ČR(CZ) GA13-13458S; GA MŠk(CZ) LO1508; GA ČR(CZ) GA16-14631S Institutional support: RVO:68378041 Keywords : 8-OxodG * ELISA * HPLC-MS/MS Subject RIV: DN - Health Impact of the Environment Quality Impact factor: 5.606, year: 2016

  5. Simultaneous Determination of 8 kinds of Biogenic Amines in Soy Sauce by HPLC%高效液相色谱法同时测定酱油中的8种生物胺

    Institute of Scientific and Technical Information of China (English)

    邹阳; 赵谋明; 赵海锋

    2012-01-01

    本文建立了高效液相色谱法同时检测酱油中色胺、苯乙胺、腐胺、尸胺、组胺、酪胺、亚精胺和精胺的方法.采用5%三氯乙酸溶液为样品提取溶剂,提取液经丹璜酰氯柱前衍生30 min,最终HPLC进行定性和定量分析.本方法中8种生物胺的线性范围为1.0~50μg/mL,相关系数R2大于0.99,检出限(S/N=3)为0.075~0.3 μg/mL.在添加水平为1.00和5.00 μg/mL时,样品的平均回收率在83%-111%之间,相对标准偏差为0.43%~19.0%.本方法具有线性范围广,灵敏度和准确度高等优点,适用于酱油中生物胺的检测.采用本方法对市售10种酱油进行检测,总生物胺含量的范围为50.82~1898.17 μg/mL,其中酪胺、腐胺和苯乙胺是酱油样品中含量最多的生物胺.%An analytical method for simultaneous determination of trypatamine, phenylethylamine, putrescine, cadaverine, histamine, tyramine, spermidine and spermine in soy sauce by HPLC was developed Biogenic amines in soy sauce were extracted with a mixture of 5% TCA, and then derived with dansyl chloride for 30 min, HPLC was used to qualitative and quantitative analysis. Under the optimal conditions, linear range was 1.0~50 μg/mL for biogenic amines and the correlation coefficient (R2) was greater than 0.99. The limits of detection were in the range of 0.075-0.3 μg/mL. At the spiked levels of 1.00 and 5.00 μg/mL, the average recoveries were 83%~111% with the relative standard deviations of 0.43 %~ 19%. The results showed that the proposed method has a good linearity and sensitivity which is suitable to detect biogenic amines in soy sauce. The established method has been successfully applied to determine biogenic amines in 10 commercial soy sauce samples, and the values of total biogenic amines were in the range of 50.82~1898.17 μg/mL. Tyramine, putrescin and phenylethylamine were found to be predominant amines in soy sauce samples.

  6. An improved HPLC method for determination of colocynthin in colocynth

    Directory of Open Access Journals (Sweden)

    M. Shekarchi

    2015-10-01

    Full Text Available Background and objectives: Colocynthin is the major active secondary metabolite of colocynth, Citrullus colocynthis (L. Schrad, which has been used in traditional and ethno medicine of many countries.  It could be considered as an active marker for quality control of colocynth and its herbal products. Analysis and standardization of colocynth and its herbal preparations are a critical issue for their safe applications in phytotherapy and traditional medicine. In the present work, a simple and efficient sample preparation was developed and optimized through combination of matrix solid phase dispersion and ultrasonic assisted extraction. In addition, analytical reversed-phase HPLC method was optimized for analyzing the concentration of colocynthin in colocynth pulp. Methods: Powdered colocynth pulp was grinded with diatomaceous earth to obtain a homogenous mixture. The blend was mixed with methanol and extracted by sonication, followed by centrifugation and filtration. The analytical chromatographic separation was carried out using Luna C18 in isocratic elution with methanol: isopropanol: water: triflouroacetic acid (30:10:60:0.1 v/v. The method was validated as well.  Results: The validation parameters were determines as follows, linear range (r2 = 0.999, 75-500 μg/mL, precision (intra-day < 2.7%, inter-day = 4.4% and accuracy measured via determination of recovery (90-107%. The limit of detection and quantization were calculated 8.5 and 25.7 μg/mL, respectively. Conclusion: Regarding the relatively high content of colocynthin in colocynth pulp, the validated HPLC method could be applied for quality control of colocynth pulp used in Traditional Persian Medicine.

  7. Progress with Implementing Energy Efficiency Policies in the G8

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2009-07-01

    At the 2008 G8 Summit in Hokkaido, leaders reaffirmed the critical role improved energy efficiency can play in addressing energy security, environmental and economic objectives. They went even farther than in previous Summits and committed to maximising implementation of the 25 IEA energy efficiency recommendations prepared for the G8. The imperative to enhance energy efficiency remains a priority for all countries. To support governments with their implementation of energy efficiency, the IEA recommended the adoption of a broad range of specific energy efficiency policy measures to the G8 Summits in 2006, 2007 and 2008. The consolidated set of recommendations from these Summits covers 25 fields of action across seven priority areas: cross-sectoral activity, buildings, appliances, lighting, transport, industry and power utilities. If governments want to significantly improve energy efficiency, the IEA considers that no single policy implemented in isolation will be effective at achieving this aim. The IEA Secretariat recommends that governments implement a full set of appropriate measures. The IEA estimates that if implemented globally without delay, the proposed actions could save around 8.2 GtCO2/yr by 2030 -- equivalent to twice the EU's yearly emissions. This report evaluates the progress of the G8 countries in implementing energy efficiency policy, including the 25 G8/IEA recommendations. Information in this report is current up to 31 March 2009.

  8. Relationship between Health Locus of Control and Risky Sexual Behaviors among Nigerian Adolescents.

    Science.gov (United States)

    Pharr, Jennifer; Enejoh, Victor; Mavegam, Bertille Octavie; Olutola, Ayodotun; Karick, Haruna; Ezeanolue, Echezona E

    2015-06-01

    HIV/AIDS knowledge has been rated as the most important factor for HIV prevention. However, studies have also shown that knowledge alone does not always translate into reduced risky sexual behavior (RSB). Health locus of control (HLC) categorized as perceived control over health status (internal locus of control) or attribution of health status to chance or fate (external health locus of control) is a psychological construct that has been shown to impact health outcomes including RSB. This study thus investigated the relationship between HLC and RSB among Nigerian adolescents. A cross-sectional survey design was employed among 361 adolescents from nine senior secondary schools selected through stratified random sampling from Jos, Plateau State Nigeria. Data were collected between August and October of 2008. Health Locus of Control Scale was used to categorize individuals into having either an internal or external HLC. RSB was assessed using the Brief HIV Screener (BHS). Descriptive statistics were computed and Mann-Whitney U test was used to determine differences in BHS scores by HLC categories. Odds ratios and adjusted odds ratios were calculated for individual BHS question responses based on HLC. Participants were 169 males (46.8%) and 192 females (53.2%) with a mean age of 16.9. When grouped into HLC categories, 141 were internal and 220 were external. The mean score on the BHS showed statistically significant difference based on HLC (p=0.01). Odds for using a condom during sexual intercourse were higher for adolescents with an internal HLC while adolescents with an external HLC had significantly higher RSB scores. Prevention programs targeted at adolescents should also aim to internalize their HLC.

  9. Phytosterol Feeding Causes Toxicity in ABCG5/G8 Knockout Mice

    Science.gov (United States)

    McDaniel, Allison L.; Alger, Heather M.; Sawyer, Janet K.; Kelley, Kathryn L.; Kock, Nancy D.; Brown, J. Mark; Temel, Ryan E.; Rudel, Lawrence L.

    2014-01-01

    Plant sterols, or phytosterols, are very similar in structure to cholesterol and are abundant in typical diets. The reason for poor absorption of plant sterols by the body is still unknown. Mutations in the ABC transporters G5 and G8 are known to cause an accumulation of plant sterols in blood and tissues (sitosterolemia). To determine the significance of phytosterol exclusion from the body, we fed wild-type and ABCG5/G8 knockout mice a diet enriched with plant sterols. The high-phytosterol diet was extremely toxic to the ABCG5/G8 knockout mice but had no adverse effects on wild-type mice. ABCG5/G8 knockout mice died prematurely and developed a phenotype that included high levels of plant sterols in many tissues, liver abnormalities, and severe cardiac lesions. This study is the first to report such toxic effects of phytosterol accumulation in ABCG5/G8 knockout mice. We believe these new data support the conclusion that plant sterols are excluded from the body because they are toxic when present at high levels. PMID:23380580

  10. Sugar microanalysis by HPLC with benzoylation: improvement via introduction of a C-8 cartridge and a high efficiency ODS column.

    Science.gov (United States)

    Miyagi, Michiko; Yokoyama, Hirokazu; Hibi, Toshifumi

    2007-07-01

    An HPLC protocol for sugar microanalysis based on the formation of ultraviolet-absorbing benzoyl chloride derivatives was improved. Here, samples were prepared with a C-8 cartridge and analyzed with a high efficiency ODS column, in which porous spherical silica particles 3 microm in diameter were packed. These devices allowed us to simultaneously quantify multiple sugars and sugar alcohols up to 10 ng/ml and to provide satisfactory separations of some sugars, such as fructose and myo-inositol and sorbitol and mannitol. This protocol, which does not require special apparatuses, should become a powerful tool in sugar research.

  11. 16 CFR Appendix G8 to Part 305 - Boilers-Electric

    Science.gov (United States)

    2010-01-01

    ... 16 Commercial Practices 1 2010-01-01 2010-01-01 false Boilers-Electric G8 Appendix G8 to Part 305 Commercial Practices FEDERAL TRADE COMMISSION REGULATIONS UNDER SPECIFIC ACTS OF CONGRESS RULE CONCERNING... Part 305—Boilers—Electric Manufacturer's rated heating capacities (Btu's/hr.) Range of annual fuel...

  12. Development and validation of a stability-indicating RP–HPLC method for estimation of atazanavir sulfate in bulk

    Directory of Open Access Journals (Sweden)

    S. Dey

    2017-04-01

    Full Text Available A stability-indicating reverse phase–high performance liquid chromatography (RP–HPLC method was developed and validated for the determination of atazanavir sulfate in tablet dosage forms using C18 column Phenomenix (250 mm×4.6 mm, 5 μm with a mobile phase consisting of 900 mL of HPLC grade methanol and 100 mL of water of HPLC grade. The pH was adjusted to 3.55 with acetic acid. The mobile phase was sonicated for 10 min and filtered through a 0.45 μm membrane filter at a flow rate of 0.5 mL/min. The detection was carried out at 249 nm and retention time of atazanavir sulfate was found to be 8.323 min. Linearity was observed from 10 to 90 μg/mL (coefficient of determination R2 was 0.999 with equation, y=23.427x+37.732. Atazanavir sulfate was subjected to stress conditions including acidic, alkaline, oxidation, photolysis and thermal degradation, and the results showed that it was more sensitive towards acidic degradation. The method was validated as per ICH guidelines.

  13. Analysis of aldehydes in human exhaled breath condensates by in-tube SPME-HPLC.

    Science.gov (United States)

    Wang, ShuLing; Hu, Sheng; Xu, Hui

    2015-11-05

    In this paper, polypyrrole/graphene (PPy/G) composite coating was prepared by a facile electrochemical polymerization strategy on the inner surface of a stainless steel (SS) tube. Based on the coating tube, a novel online in-tube solid-phase microextraction -high performance liquid chromatography (IT-SPME-HPLC) was developed and applied for the extraction of aldehydes in the human exhaled breath condensates (EBC). The hybrid PPy/G nanocomposite exhibits remarkable chemical and mechanical stability, high selectivity, and satisfactory extraction performance toward aldehyde compounds. Moreover, the proposed online IT-SPME-HPLC method possesses numerous superiorities, such as time and cost saving, process simplicity, high precision and sensitivity. Some parameters related to extraction efficiency were optimized systematically. Under the optimal conditions, the recoveries of the aldehyde compounds at three spiked concentration levels varied in the range of 85%-117%. Good linearity was obtained with excellent correlation coefficients (R(2)) being larger than 0.994. The relative standard deviations (n = 5) of the method ranged from 1.8% to 11.3% and the limits of detection were between 2.3 and 3.3 nmol L(-1). The successful application of the proposed method in human EBC indicated that it is a promising approach for the determination of trace aldehyde metabolites in complex EBC samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. An Investigation Into HPLC Data Quality Problems

    Science.gov (United States)

    Hooker, Stanford B.; VanHeukelem, Laurie

    2011-01-01

    This report summarizes the analyses and results produced by a five-member investigative team of Government, university, and industry experts, established by NASA HQ. The team examined data quality problems associated with high performance liquid chromatography (HPLC) analyses of pigment concentrations in seawater samples produced by the San Diego State University (SDSU) Center for Hydro-Optics and Remote Sensing (CHORS). This report shows CHORS did not validate the methods used before placing them into service to analyze field samples for NASA principal investigators (PIs), even though the HPLC literature contained easily accessible method validation procedures, and the importance of implementing them, more than a decade ago. In addition, there were so many sources of significant variance in the CHORS methodologies, that the HPLC system rarely operated within performance criteria capable of producing the requisite data quality. It is the recommendation of the investigative team to a) not correct the data, b) make all the data that was temporarily sequestered available for scientific use, and c) label the affected data with an appropriate warning, e.g., "These data are not validated and should not be used as the sole basis for a scientific result, conclusion, or hypothesis--independent corroborating evidence is required."

  15. Online identification of chlorogenic acids, sesquiterpene lactones, and flavonoids in the Brazilian arnica Lychnophora ericoides Mart. (Asteraceae) leaves by HPLC-DAD-MS and HPLC-DAD-MS/MS and a validated HPLC-DAD method for their simultaneous analysis.

    Science.gov (United States)

    Gobbo-Neto, Leonardo; Lopes, Norberto P

    2008-02-27

    Lychnophora ericoides Mart. (Asteraceae, Vernonieae) is a plant, endemic to Brazil, with occurrence restricted to the "cerrado" biome. Traditional medicine employs alcoholic and aqueous-alcoholic preparations of leaves from this species for the treatment of wounds, inflammation, and pain. Furthermore, leaves of L. ericoides are also widely used as flavorings for the Brazilian traditional spirit "cachaça". A method has been developed for the extraction and HPLC-DAD analysis of the secondary metabolites of L. ericoides leaves. This analytical method was validated with 11 secondary metabolites chosen to represent the different classes and polarities of secondary metabolites occurring in L. ericoides leaves, and good responses were obtained for each validation parameter analyzed. The same HPLC analytical method was also employed for online secondary metabolite identification by HPLC-DAD-MS and HPLC-DAD-MS/MS, leading to the identification of di- C-glucosylflavones, coumaroylglucosylflavonols, flavone, flavanones, flavonols, chalcones, goyazensolide, and eremantholide-type sesquiterpene lactones and positional isomeric series of chlorogenic acids possessing caffeic and/or ferulic moieties. Among the 52 chromatographic peaks observed, 36 were fully identified and 8 were attributed to compounds belonging to series of caffeoylferuloylquinic and diferuloylquinic acids that could not be individualized from each other.

  16. Validation of HPLC-ESI-MS/MS Protocol to Analyze EtG in Hair for Assessment of Chronic Excessive Alcohol Use in Thailand in Conjunction with AUDIT.

    Science.gov (United States)

    Thananchai, Thiwaphorn; Junkuy, Anongphan; Kittirattanapaiboon, Phunnapa; Sribanditmongkol, Pongruk

    2016-06-01

    Hair analysis for chronic excessive alcohol (ethanol) use has focused on ethyl glucuronide (EtG), a minor metabolite of ethanol. Preferred methods have involved high-performance liquid chromatography (HPLC) combined with tandem mass spectrometry (MS/MS) in line with an electrospray ionization (ESI) source. EtG analysis in hair has not yet been introduced to Thailand To validate an in-house HPLC-ESI-MS/MS hair analysis protocol for EtG and to apply it to a field sample of alcohol drinkers to assess different risk levels of alcohol consumption as measured by the Alcohol Use Disorders Identification Test (AUDIT). Validation procedures followed guidelines of the US Food and Drug Administration, the European Medicines Agency, and the Scientific Working Group for Forensic Toxicology. One hundred twenty subjects reported consuming alcohol during a 3-month period prior to enrollment. After taking the Thai-language version of AUDIT, subjects were divided on the basis of test scores into low, medium, and high-risk groups for chronic excessive alcohol use. The protocol satisfied the international standards for selectivity, specificity, accuracy, precision, and calibration curve. There was no significant matrix effect. Limits of detection and quantification (LOD/LOQ) were set at 15 pg of EtG per mg of hair. The protocol was not able to detect EtG in low-risk subjects (n = 38). Detection rates for medium-risk (n = 42) and high-risk subjects (n = 40) were 14.3% and 85%, respectively. The median of EtG concentration between these two groups were significantly different. Sensitivity and specificity were both more than 90% when EtG concentrations of high-risk subjects were compared with the 30 pg/mg cutoff recommended by the Society of Hair Testing (SoHT) for diagnosing chronic excessive alcohol consumption, based on an average ethanol daily intake greater than 60 g. The in-house protocol for EtG analysis in hair was validated according to international standards. The protocol is a

  17. Can the Afinion HbA1c Point-of-Care instrument be an alternative method for the Tosoh G8 in the case of Hb-Tacoma?

    Science.gov (United States)

    Lenters-Westra, Erna; Strunk, Annuska; Campbell, Paul; Slingerland, Robbert J

    2017-02-01

    Hb-variant interference when reporting HbA1c has been an ongoing challenge since HbA1c was introduced to monitor patients with diabetes mellitus. Most Hb-variants show an abnormal chromatogram when cation-exchange HPLC is used for the determination of HbA1c. Unfortunately, the Tosoh G8 generates what appears to be normal chromatogram in the presence of Hb-Tacoma, yielding a falsely high HbA1c value. The primary aim of the study was to investigate if the Afinion HbA1c point-of-care (POC) instrument could be used as an alternative method for the Tosoh G8 when testing for HbA1c in the presence of Hb-Tacoma. Whole blood samples were collected in K 2 EDTA tubes from individuals homozygous for HbA (n = 40) and heterozygous for Hb-Tacoma (n = 20). Samples were then immediately analyzed with the Afinion POC instrument. After analysis, aliquots of each sample were frozen at -80 °C. The frozen samples were shipped on dry ice to the European Reference Laboratory for Glycohemoglobin (ERL) and analyzed with three International Federation of Clinical Chemistry and Laboratory Medicine (IFCC) and National Glycohemoglobin Standardization Program (NGSP) Secondary Reference Measurement Procedures (SRMPs). The Premier Hb9210 was used as the reference method. When compared to the reference method, samples with Hb-Tacoma yielded mean relative differences of 31.8% on the Tosoh G8, 21.5% on the Roche Tina-quant Gen. 2 and 16.8% on the Afinion. The Afinion cannot be used as an alternative method for the Tosoh G8 when testing for HbA1c in the presence of Hb-Tacoma.

  18. Determination of (E)-10-hydroxy-2-decenoic acid content in pure royal jelly: a comparison between a new CZE method and HPLC.

    Science.gov (United States)

    Ferioli, Federico; Marcazzan, Gian Luigi; Caboni, Maria Fiorenza

    2007-05-01

    A new CZE method was developed and compared with HPLC for the determination of (E)-10-hydroxy-2-decenoic acid (10-HDA) in royal jelly (RJ) samples of different geographical origin. The results obtained with the CZE method were highly correlated with those of HPLC (p HDA/mL), a good sensitivity (LOD and LOQ were 0.002 and 0.004 mg/mL, respectively) and a satisfactory instrumental repeatability with respect to migration time and peak area (RSD% less than 1.0 and 2.0% on migration time for intra- and interday assay, respectively and less than 2.0 and for 4.0% on peak area for intra- and interday assay, respectively). The 10-HDA content in RJ ranged from 0.8 to 3.2 g/100 g of RJ and a significant difference (p < 0.05) was found between the Italian and extra-European average values: 2.5 and 1.6 g/100 g of RJ, respectively, according to the CZE data. The possibility of application of CZE for routine analyses on RJ and RJ based products to verify their authenticity is highlighted here.

  19. Oral live attenuated human rotavirus vaccine (RotarixTM offers sustained high protection against severe G9P[8] rotavirus gastroenteritis during the first two years of life in Brazilian children

    Directory of Open Access Journals (Sweden)

    Maria Cleonice A Justino

    2012-11-01

    Full Text Available In a large Phase III trial conducted in 10 Latin American countries, the safety and efficacy of the live attenuated monovalent rotavirus vaccine RIX4414 was evaluated in 15,183 healthy infants followed up during the first two years of life. Belém was the only site in Brazil included in this multicentre trial. The study in Belém included a subset of 653 infants who were followed up until 24 months of age for protection against severe rotavirus gastroenteritis. These subjects were randomly assigned in a 1:1 ratio to receive two doses of vaccine (n = 328 or two doses of placebo (n = 325 at approximately two and four months of age. Of the 653 enrolled infants, 23 dropped out during the study period. For the combined two-year period, the efficacy of RIX4414 was 72.3% [95% confidence interval (CI 37.5-89.1%] against severe rotavirus-related gastroenteritis, reaching a protection rate of 81.8% (95% CI 36.4-96.6% against circulating wild-type G9 rotavirus strains. It is concluded that two doses of RIX4414 are highly efficacious against severe rotavirus gastroenteritis in Belém during the first two years of life and provide high protection against the worldwide emergence and spread of G9P[8] strains.

  20. HPLC PROFILING OF PHENOLIC ACIDS AND FLAVONOIDS AND EVALUATION OF ANTI-LIPOXYGENASE AND ANTIOXIDANT ACTIVITIES OF AQUATIC VEGETABLE LIMNOCHARIS FLAVA.

    Science.gov (United States)

    Ooh, Keng-fei; Ong, Hean-Chooi; Wong, Fai-Chu; Chai, Tsun-Thai

    2015-01-01

    Limnocharis flava is an edible wetland plant, whose phenolic acid and flavonoid compositions as well as bioactivities were underexplored. This study analyzed the profiles of selected hydroxybenzoic acids, hydroxycinnamic acids and flavonoids in the aqueous extracts of L. flava leaf, rhizome and root by high performance liquid chromatography (HPLC). Anti-lipoxygenase and antioxidant (iron chelating, 2,2-diphenyl-l-picrylhydrazyl (DPPH) radical scavenging, and nitric oxide (NO) scavenging) activities of the extracts were also evaluated. Leaf extract had the highest phenolic contents, being most abundant in p-hydroxybenzoic acid (3861.2 nmol/g dry matter), ferulic acid (648.8 nmol/g dry matter), and rutin (4110.7 nmol/g dry matter). Leaf extract exhibited the strongest anti-lipoxygenase (EC50 6.47 mg/mL), iron chelating (EC50 6.65 mg/mL), DPPH scavenging (EC50 15.82 mg/mL) and NO scavenging (EC50 3.80 mg/mL) activities. Leaf extract also had the highest ferric reducing ability. This is the most extensive HPLC profiling of phenolic acids and flavonoids in L.flava to date. In conclusion, L. flava leaf is a source of health-promoting phenolics, anti-lipoxygenase agents and antioxidants.

  1. Conventional high-performance liquid chromatography versus derivative spectrophotometry for the determination of 1,3,6-pyrenetrisulfonic acid trisodium salt and 1,3,6,8-pyrenetetrasulfonic acid tetrasodium salt in the color additive D&C Green No. 8 (Pyranine).

    Science.gov (United States)

    Jitian, Simion; White, Samuel R; Yang, H-H Wendy; Weisz, Adrian

    2014-01-10

    Specifications in the U.S. Code of Federal Regulations for the color additive D&C Green No. 8 (Colour Index No. 59040) limit the levels of the subsidiary colors 1,3,6-pyrenetrisulfonic acid trisodium salt (P3S) and 1,3,6,8-pyrenetetrasulfonic acid tetrasodium salt (P4S). The present paper describes a comparative study of two possible methods to replace the currently used multi-step TLC/spectrophotometry method of separating and quantifying the minor components P3S and P4S in G8. One of the new approaches uses conventional high-performance liquid chromatography (HPLC) and the other, derivative spectrophotometry. While the derivative spectrophotometric method was shown to be inadequate for the analysis of minor components overwhelmed by components of much higher concentration, the HPLC method was proven highly effective. The closely related, very polar compounds P3S and P4S were separated by the new HPLC method in less than 4 min using a conventional HPLC instrument. P3S and P4S were quantified by using five-point calibration curves with data points that ranged from 0.45 to 7.63% and from 0.13 to 1.82%, by weight, for P3S and P4S, respectively. The HPLC method was applied to the analysis of test portions from 20 batches of D&C Green No. 8 submitted to the U.S. Food and Drug Administration for certification. Published by Elsevier B.V.

  2. Simultaneous determination of arsenic, selenium and antimony species using HPLC/ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Lindemann, T.; Prange, A.; Neidhart, B. [GKSS-Forschungszentrum Geesthacht GmbH (Germany). Inst. fuer Physikalische und Chemische Analytik; Dannecker, W. [Univ. of Hamburg (Germany). Inst. for Inorganic and Applied Chemistry

    1999-07-01

    A new method for the simultaneous separation and determination of four arsenic species [As(III), As(V), monomethylarsonic acid and dimethylarsinic acid], three selenium species [Se(IV), Se(VI) and selenomethionine] as well as Sb(III) and Sb(V) is presented. The speciation was achieved by on-line coupling of anion exchange high-performance liquid chromatography (HPLC) with inductively coupled plasma mass spectrometry (ICP-MS). Chromatographic parameters such as the composition and pH of the mobile phase were optimised. Limits of detection are below 4.5 {mu}g L{sup -1} (as element) for Sb(III) and the selenium species and below 0.5 {mu}g L{sup -1} for the other species. Precisions of retention times were better than 2% RSD and of peak areas better than 8% RSD for all the species investigated. (orig.) With 5 figs., 3 tabs., 41 refs.

  3. Preclinical evaluation of intravenously administered 111In-and 90Y-labeled B72.3 immunoconjugate (GYK-DTPA) in beagle dogs

    International Nuclear Information System (INIS)

    Quadri, S.M.; Vriesendorp, H.M.; Yi Shao; Blum, J.E.; Leichner, P.K.; Williams, J.R.

    1993-01-01

    B72.3, a monoclonal antibody with reactivity against human adenocarcinomas was obtained from the Cytogen Corporation in the form of an immunoconjugate coupled with linker-chelator GYK-DTPA by using proprietary carbohydrate directed site specific chemistry. The immunoconjugate was radiolabeled with indium-111 or yttrium-90. A preclinical analysis was performed in 10 normal beagle dogs. The pharmacokinetics of intravenously administered indium- and yttrium-labeled immunoconjugates were compared serially in blood, bone marrow and urine samples. Compared to 90 Y less of the 111 In label ended up in urine and more was found in blood and bone marrow. Indium-labeled B72.3 GYK-DTPA had relatively higher uptake in most glandular tissues than 111 In-labeled antiferritin immunoconjugate. Bone marrow toxicity was the dose limiting side effect after intravenous infusion of 90 Y-labeled B72.3 GYK-DTPA. Toxicity was also observed in the liver but not in other organ systems. Recently other investigators obtained similar results with these immunoconjugates in human patients. A preclinical pharmacokinetic analysis of radioimmunoconjugates in beagle dogs provided useful information regarding bone marrow toxicity, liver toxicity and in vivo instability of the immunoconjugate. Data suggest that for future trials in human patients, a more stable chelated immunoconjugate for yttrium is needed to achieve less liver uptake and a better correlation with the 111 In-labeled product than the 90 Y-labeled B72.3 GYK-DTPA used in this investigation. (Author)

  4. Dual High-Resolution α-Glucosidase and Radical Scavenging Profiling Combined with HPLC-HRMS-SPE-NMR for Identification of Minor and Major Constituents Directly from the Crude Extract of Pueraria lobata

    DEFF Research Database (Denmark)

    Liu, Bingrui; Kongstad, Kenneth Thermann; Qinglei, Sun

    2015-01-01

    The crude methanol extract of Pueraria lobata was investigated by dual high-resolution α-glucosidase inhibition and radical scavenging profiling combined with hyphenated HPLC-HRMS-SPE-NMR. Direct analysis of the crude extract without preceding purification was facilitated by combining chromatograms...... from two analytical-scale HPLC separations of 120 and 600 μg on-column, respectively. High-resolution α-glucosidase and radical scavenging profiles were obtained after microfractionation of the eluate in 96-well microplates. This allowed full bioactivity profiling of individual peaks in the HPLC...... chromatogram of the crude methanol extract. Subsequent HPLC-HRMS-SPE-NMR analysis allowed identification of 21 known compounds in addition to two new compounds, i.e., 3′-methoxydaidzein 8-C-[α-d-apiofuranosyl-(1→6)]-β-d-glucopyranoside and 6″-O-malonyl-3′-methoxydaidzin, as well as an unstable compound...

  5. Effect of 60Co-irradiation on penicillin G procaine in veterinary mastitis products

    International Nuclear Information System (INIS)

    Tsuji, K.; Goetz, J.F.; Vanmeter, W.

    1979-01-01

    The effect of 60 Co-irradation on penicillin G procaine in a peanut oil-based veterinary mastitis product was examined by reversed-phase high-performance liquid chromatography (HPLC). The HPLC method is capable of separating and quantifiying procaine, penicillin G, and various degradation compounds. Values obtained by the HPLC method on the product irradiated and stored at various temperatures correlated well with those of the microbiological assay. No significant decrease in the procaine was detected even after 4.0-Mrad irradiation. The HPLC method is applicable for analysis of other beta-lactam antibiotics

  6. NMR structural studies of the ionizing radiation adduct 7-hydro-8-oxodeoxyguanosine (8-oxo-7H-dG) opposite deoxyadenosine in a DNA duplex. 8-oxo-7H-dG(syn)·dA(anti) alignment at lesion site

    International Nuclear Information System (INIS)

    Kouchakdjian, M.; Patel, D.J.; Bodepudi, V.; Shibutani, S.; Eisenberg, M.; Johnson, F.; Grollman, A.P.

    1991-01-01

    Proton NMR studies are reported on the complementary d(C1-C2-A3-C4-T5-A6-oxo-G7-T8-C9-A10-C11-C12)·d(G13-G14-T15-G16-A17-A18-T19-A20-G21-T22-G23-G24) dodecanucleotide duplex (designated 8-oxo-7H-dG·dA 12-mer), which contains a centrally located 7-hydro-8-oxodeoxyguanosine (8-oxo-7H-dG) residue, a group commonly found in DNA that has been exposed to ionizing radiation or oxidizing free radicals. From the NMR spectra it can be deduced that this moiety exists as two tautomers, or gives rise to two DNA conformations, that are in equilibrium and that exchange slowly. The present study focuses on the major component of the equilibrium that originates in the 6,8-dioxo tautomer of 8-oxo-7H-dG. The authors have assigned the exchangeable NH1, NH7, and NH 2 -2 base protons located on the Watson-Crick and Hoogsteen edges of 8-oxo-7H-dG7 in the 8-oxo-7H-dG·dA 12-mer duplex, using an analysis of one- and two-dimensional nuclear Overhauser enhancement (NOE) data in H 2 O solution. They were able to detect a set of intra- and interstrand NOEs between protons (exchangeable and nonexchangeable) on adjacent residues in the d(A6-oxo-G7-T8)·d(A17-A18-T19) trinucleotide segment centered about the lesion site that establishes stacking of the oxo-dG7(syn)·dA(anti) pair between stable Watson-Crick dA6·dT19 and dT8·A17 base pairs with minimal perturbation of the helix. The structural studies demonstrate that 8-oxo-7H-dG(syn)·dA(anti) forms a stable pair in the interior of the helix, providing a basis for the observed incorporation of dA opposite 8-oxo-7H-dG when readthrough occurs past this oxidized nucleoside base

  7. A highly sensitive fluorescence quenching method for perphenazine detection based on its catalysis of K{sub 2}S{sub 2}O{sub 8} oxidizing rhodamine 6G

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Lihong; Huang, Qitong; Lin, Changqing [Department of Food and Biological Engineering, Zhangzhou Institute of Technology, Zhangzhou, 363000 (China); Lin, Xiaofeng [College of Chemistry and Environment, Minnan Normal University, Zhangzhou, 363000 (China); Huang, Yiqun [Zhangzhou Affiliated Hospital of Fujian Medical University, Zhangzhou 363000 (China); Liu, Jiaming, E-mail: mnsdljm@163.com [College of Chemistry and Environment, Minnan Normal University, Zhangzhou, 363000 (China); Ma, Xudong, E-mail: maxudong005@hotmail.com [Zhangzhou Affiliated Hospital of Fujian Medical University, Zhangzhou 363000 (China)

    2014-12-15

    In this paper, the fluorescence spectra of Rhod 6G (rhodamine 6G)–K{sub 2}S{sub 2}O{sub 8}–PPH (perphenazine) were studied. We found that Rhod 6G existed in the form of Rhod 6G{sup +} under the conditions of 60 °C, 10 min and pH 5.42, and Rhod 6G{sup +} can emit strong and stable fluorescence. Further study showed that when PPH and Rhod 6G{sup +} coexisted, the ester exchange reaction carried out between -OH of PPH and -COOC{sub 2}H{sub 5} of Rhod 6G{sup +} to produced Rhod 6G{sup +}–PPH compound. More interestingly, K{sub 2}S{sub 2}O{sub 8} could oxidize Rhod 6G{sup +} and quench its RTP signal, while PPH was oxidized to red compound PPH′ by K{sub 2}S{sub 2}O{sub 8}, and Rhod 6G{sup +}–PPH′ and PPH were produced in the ester exchange reaction between the -OH of PPH′ and the -COOC{sub 2}H{sub 5} of Rhod 6G{sup +}–PPH. In the above process, PPH catalyzed K{sub 2}S{sub 2}O{sub 8} oxidizing Rhod 6G, which caused the fluorescence signal of the system to quench sharply. Hence, a catalytic fluorescence quenching method for the determination of residual PPH has been developed based on the its catalyzing K{sub 2}S{sub 2}O{sub 8} oxidize rhodamine 6G. This sensitive, accurate, simple and selective fluorescence quenching method was used to determine residual PPH in biological samples with the results consisting with those obtained by high performance liquid chromatography (HPLC), showing good accuracy. The structures of Rhod 6G{sup +}, PPH and Rhod 6G{sup +}–PPH were characterized by infrared spectra. The reaction mechanism of the determination of PPH was also discussed. - Highlights: • Fluorescence for the determination of perphenazine (PPH) had been established. • This method had high sensitivity (limit of detection was 3.3×10{sup −14} g mL{sup −1}). • This method had been applied to determination of PPH in biological samples. • Structures of Rhod 6G{sup +}, PPH and Rhod 6G{sup +}–PPH were characterized by infrared spectra. • Mechanism

  8. Detection and quantification of new psychoactive substances (NPSs) within the evolved "legal high" product, NRG-2, using high performance liquid chromatography-amperometric detection (HPLC-AD).

    Science.gov (United States)

    Zuway, Khaled Y; Smith, Jamie P; Foster, Christopher W; Kapur, Nikil; Banks, Craig E; Sutcliffe, Oliver B

    2015-09-21

    The global increase in the production and abuse of cathinone-derived New Psychoactive Substances (NPSs) has developed the requirement for rapid, selective and sensitive protocols for their separation and detection. Electrochemical sensing of these compounds has been demonstrated to be an effective method for the in-field detection of these substances, either in their pure form or in the presence of common adulterants, however, the technique is limited in its ability to discriminate between structurally related cathinone-derivatives (for example: (±)-4′-methylmethcathinone (4-MMC, 2a) and (±)-4′-methyl-N-ethylmethcathinone (4-MEC, 2b) when they are both present in a mixture. In this paper we demonstrate, for the first time, the combination of HPLC-UV with amperometric detection (HPLC-AD) for the qualitative and quantitative analysis of 4-MMC and 4-MEC using either a commercially available impinging jet (LC-FC-A) or custom-made iCell channel (LC-FC-B) flow-cell system incorporating embedded graphite screen-printed macroelectrodes. The protocol offers a cost-effective, reproducible and reliable sensor platform for the simultaneous HPLC-UV and amperometric detection of the target analytes. The two systems have similar limits of detection, in terms of amperometric detection [LC-FC-A: 14.66 μg mL(-1) (2a) and 9.35 μg mL(-1) (2b); LC-FC-B: 57.92 μg mL(-1) (2a) and 26.91 μg mL(-1) (2b)], to the previously reported oxidative electrochemical protocol [39.8 μg mL(-1) (2a) and 84.2 μg mL(-1) (2b)], for two synthetic cathinones, prevalent on the recreational drugs market. Though not as sensitive as standard HPLC-UV detection, both flow cells show a good agreement, between the quantitative electroanalytical data, thereby making them suitable for the detection and quantification of 4-MMC and 4-MEC, either in their pure form or within complex mixtures. Additionally, the simultaneous HPLC-UV and amperometric detection protocol detailed herein shows a marked improvement

  9. Triosephosphate isomerase gene promoter variation: -5G/A and -8G/A polymorphisms in clinical malaria groups in two African populations.

    Science.gov (United States)

    Guerra, Mónica; Machado, Patrícia; Manco, Licínio; Fernandes, Natércia; Miranda, Juliana; Arez, Ana Paula

    2015-06-01

    TPI1 promoter polymorphisms occur in high prevalence in individuals from African origin. Malaria-patients from Angola and Mozambique were screened for the TPI1 gene promoter variants rs1800200A>G, (-5G>A), rs1800201G>A, (-8G>A), rs1800202T>G, (-24T>G), and for the intron 5 polymorphism rs2071069G>A, (2262G>A). -5G>A and -8G>A variants occur in 47% and 53% in Angola and Mozambique, respectively while -24T>G was monomorphic for the wild-type T allele. Six haplotypes were identified and -8A occurred in 45% of the individuals, especially associated with the GAG haplotype and more frequent in non-severe malaria groups, although not significantly. The arising and dispersion of -5G>A and -8G>A polymorphisms is controversial. Their age was estimated by analyses of two microsatellite loci, CD4 and ATN1, adjacent to TPI1 gene. The -5G>A is older than -8G>A, with an average estimate of approximately 35,000 years. The -8A variant arose in two different backgrounds, suggesting independent mutational events. The first, on the -5G background, may have occurred in East Africa around 20,800 years ago; the second, on the -5A background, may have occurred in West Africa some 7500 years ago. These estimates are within the period of spread of agriculture and the malaria mosquito vector in Africa, which could has been a possible reason for the selection of -8A polymorphism in malaria endemic countries. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. Effect of Tris-acetate buffer on endotoxin removal from human-like collagen used biomaterials.

    Science.gov (United States)

    Zhang, Huizhi; Fan, Daidi; Deng, Jianjun; Zhu, Chenghui; Hui, Junfeng; Ma, Xiaoxuan

    2014-09-01

    Protein preparation, which has active ingredients designated for the use of biomaterials and therapeutical protein, is obtained by genetic engineering, but products of genetic engineering are often contaminated by endotoxins. Because endotoxin is a ubiquitous and potent proinflammatory agent, endotoxin removal or depletion from protein is essential for researching any biomaterials. In this study, we have used Tris-acetate (TA) buffer of neutral pH value to evaluate endotoxins absorbed on the Pierce high-capacity endotoxin removal resin. The effects of TA buffer on pH, ionic strength, incubation time as well as human-like collagen (HLC) concentration on eliminating endotoxins are investigated. In the present experiments, we design an optimal method for TA buffer to remove endotoxin from recombinant collagen and use a chromogenic tachypleus amebocyte lysate (TAL) test kit to measure the endotoxin level of HLC. The present results show that, the endotoxins of HLC is dropped to 8.3EU/ml at 25 mM TA buffer (pH7.8) with 150 mM NaCl when setting incubation time at 6h, and HLC recovery is about 96%. Under this experimental condition, it is proved to exhibit high efficiencies of both endotoxin removal and collagen recovery. The structure of treated HLC was explored by Transmission Electron Microscopy (TEM), demonstrating that the property and structure of HLC treated by TA buffer are maintained. Compared to the most widely used endotoxin removal method, Triton X-114 extraction, using TA buffer can obtain the non-toxic HLC without extra treatment for removing the toxic substances in Triton X-114. In addition, the present study aims at establishing a foundation for further work in laboratory animal science and providing a foundation for medical grade biomaterials. Copyright © 2014 Elsevier B.V. All rights reserved.

  11. Urinary 8-oxo-7,8-dihydroguanosine values determined by a modified ELISA improves agreement with HPLC-MS/MS

    Czech Academy of Sciences Publication Activity Database

    Rössner ml., Pavel; Mistry, V.; Singh, R.; Šrám, Radim; Cooke, M. S.

    2013-01-01

    Roč. 440, č. 4 (2013), s. 725-730 ISSN 0006-291X R&D Projects: GA ČR GAP503/11/0084; GA ČR GA13-13458S Institutional support: RVO:68378041 Keywords : 8-oxodG * urine * ELISA Subject RIV: DN - Health Impact of the Environment Quality Impact factor: 2.281, year: 2013

  12. Inverting the G-Tetrad Polarity of a G-Quadruplex by Using Xanthine and 8-Oxoguanine.

    Science.gov (United States)

    Cheong, Vee Vee; Lech, Christopher Jacques; Heddi, Brahim; Phan, Anh Tuân

    2016-01-04

    G-quadruplexes are four-stranded nucleic acid structures that are built from consecutively stacked guanine tetrad (G-tetrad) assemblies. The simultaneous incorporation of two guanine base lesions, xanthine (X) and 8-oxoguanine (O), within a single G-tetrad of a G-quadruplex was recently shown to lead to the formation of a stable G⋅G⋅X⋅O tetrad. Herein, a judicious introduction of X and O into a human telomeric G-quadruplex-forming sequence is shown to reverse the hydrogen-bond polarity of the modified G-tetrad while preserving the original folding topology. The control exerted over G-tetrad polarity by joint X⋅O modification will be valuable for the design and programming of G-quadruplex structures and their properties. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Tensile and low cycle fatigue properties of EUROFER97-steel after 16.3 dpa neutron irradiation at 523, 623 and 723 K

    Energy Technology Data Exchange (ETDEWEB)

    Materna-Morris, E., E-mail: edeltraud.materna-morris@kit.edu; Möslang, A., E-mail: anton.moeslang@kit.edu; Schneider, H.-C., E-mail: hans-christian.schneider@kit.edu

    2013-11-15

    Neutron-irradiated specimens of the reduced-activation tempered martensitic steel EUROFER97 were tested by tensile and low cycle conditions to detect the impact of irradiation on strength and lifetime. The irradiation temperature ranged from 523 to 723 K with an accumulated dose of up to 16.3 dpa. Tensile tests revealed a significant irradiation-induced hardening below 673 K with a peak of ∼430 MPa at 573 K but none was seen at 723 K, as expected. Despite the significant irradiation-induced reduction of uniform elongation, the total elongation is only reduced by about 50% below 673 K. Post-irradiation strain-controlled fatigue tests have been carried out at T{sub irrad} = T{sub test} = 523, 623 and 723 K. Pronounced cyclic softening was observed in all specimens. At 623 and 723 K, neutron irradiation had no effect on fatigue life within the data scatter. A significant lifetime increase has been observed at T{sub irrad} = T{sub test} = 523 K that advances with decreasing stress amplitude Δε (1% → 0.5%) up to a factor of ten. Scanning electron microscopy (SEM) analysis revealed ductile fracture and fatigue striations on the fracture surfaces. After push–pull fatigue testing, transmission electron microscopy (TEM) investigations showed the typical sub-cell formation, even at T{sub irrad} = T{sub test} = 523 K.

  14. Improving the ecological relevance of toxicity tests on scleractinian corals: Influence of season, life stage, and seawater temperature

    Science.gov (United States)

    Hedouin, Laetitia; Wolf, Ruth E.; Phillips, Jeff; Gates, Ruth D.

    2016-01-01

    Metal pollutants in marine systems are broadly acknowledged as deleterious: however, very little data exist for tropical scleractinian corals. We address this gap by investigating how life-history stage, season and thermal stress influence the toxicity of copper (Cu) and lead (Pb) in the coral Pocillopora damicornis. Our results show that under ambient temperature, adults and larvae appear to tolerate exposure to unusually high levels of copper (96 h-LC50 ranging from 167 to 251 μg Cu L−1) and lead (from 477 to 742 μg Pb L−1). Our work also highlights that warmer conditions (seasonal and experimentally manipulated) reduce the tolerance of adults and larvae to Cu toxicity. Despite a similar trend observed for the response of larvae to Pb toxicity to experimentally induced increase in temperature, surprisingly adults were more resistant in warmer condition to Pb toxicity. In the summer adults were less resistant to Cu toxicity (96 h-LC50 = 175 μg L−1) than in the winter (251 μg L−1). An opposite trend was observed for the Pb toxicity on adults between summer and winter (96 h-LC50 of 742 vs 471 μg L−1, respectively). Larvae displayed a slightly higher sensitivity to Cu and Pb than adults. An experimentally induced 3 °C increase in temperature above ambient decreased larval resistance to Cu and Pb toxicity by 23–30% (96 h-LC50 of 167 vs 129 μg Cu L−1 and 681 vs 462 μg Pb L−1).

  15. Vitamin D status assessed by a validated HPLC method: within and between variation in subjects supplemented with vitamin D3

    DEFF Research Database (Denmark)

    Jakobsen, Jette; Bysted, Anette; Andersen, Rikke

    2009-01-01

    Objective. The aim of this study was to develop and validate a high-pressure liquid chromatography (HPLC) method for assessing vitamin D status as 25-hydroxyvitamin D2 (S-25OHD2) and 25-hydroxyvitamin D3 (S-25OHD3) in serum. Material and methods. We assessed the within- and between-subject variat......Objective. The aim of this study was to develop and validate a high-pressure liquid chromatography (HPLC) method for assessing vitamin D status as 25-hydroxyvitamin D2 (S-25OHD2) and 25-hydroxyvitamin D3 (S-25OHD3) in serum. Material and methods. We assessed the within- and between......-subject variation of vitamin D status in serum samples from four different dietary intervention studies in which subjects (n=92) were supplemented with different doses of vitamin D3 (5-12 g/day) and for different durations (4-20 months). Results. The HPLC method was applicable for 4.0-200 nmol S-25OHD/L, while...... the within-day and between-days variations were 3.8 % and 5.7 %, respectively. There was a concentration-dependent difference between results obtained by a commercial radioimmunoassay and results from the HPLC method of -5 to 20 nmol 25OHD/L in the range 10-100 nmol 25OHD/L. The between-subject variation...

  16. Quantification of fenoxaprop-p-ethyl herbicide in soil and vegetable samples by microwave-assisted solvent extraction and HPLC method

    International Nuclear Information System (INIS)

    Shahzad, F.U.N.; Shah, J.; Jan, M.R.; Muhammad, M.

    2012-01-01

    A simple HPLC procedure for the determination of fenoxaprop-p-ethyl herbicide in environmental samples is described. The chromatographic analysis was carried out by HPLC, on a C18 packed capillary column (4x4 mm,4.6 X 150 mm, 5mm particle size) with 20 macro l injection volume and UV detector at 280 nm. HPLC-grade acetonitrile and methanol were used as mobile phase with flow rate of 1mL min-1. Samples were spiked with amount between 5 - 20 micro g g-1 of herbicide and were isolated from samples by applying microwave assisted extraction (MASE) at ambient temperature. Percent recoveries were improved by optimizing solvent types, solvent volume, extraction temperature and time. Calibration curve range determined by HPLC was 0.5-16 micro g mL-1. The interaction of different variables for maximum % recovery response was checked by applying factorial design and was found to be in range of 91.22+-0.01-99.32+-0.01 with good precision (< 5% ). Application of this procedure to the analysis of herbicide in ester and acid form showed the effectiveness of the proposed approach. (author)

  17. Evaluation of Bio-Rad D-100 HbA1c analyzer against Tosoh G8 and Menarini HA-8180V

    Directory of Open Access Journals (Sweden)

    José María Maesa

    2016-08-01

    Full Text Available Objectives: To evaluate the Bio-Rad D-100®, an HPLC analyzer for glycated hemoglobin (HbA1c determination, and to compare its performance with the Menarini HA-8180V® and Sysmex G8®. Methods: Method comparison was performed according to Clinical and Laboratory Standards Institute (CLSI EP9-A2 guidelines. We selected 100 samples from the routine laboratory workload and analyzed them in duplicate with the three analyzers. The imprecision study was performed according to CLSI EP5-A2 guidelines for both inter-assay and intra-assay variability. Bias was assessed with external quality control material. To establish linearity, CLSI EP6-A protocol was followed. Results: Method comparison (95% confidence intervals in parentheses: D-100 vs G8: Passing-Bablok regression; y=0.973(0.963–0.983×−0.07(−0.07−0.069; r=0.9989. Bland-Altman mean difference: −0.229%HbA1c (−0.256: −0.202; Relative bias plot: D-100/G8 vs D100-G8 mean ratio=0.971(0.967−0.975. D-100 vs HA-8180V: Passing-Bablok regression; y=0.944(0.932–0.958×−0.078(0.024−0.173; r=0.9989. Bland-Altman mean difference: −0.363%HbA1c (−0.401: −0.325; Relative bias plot D-100/HA-8180V vs D100-HA-8180V mean ratio=0.955(0.952−0.958. Inter-assay coefficient of variation (CV: 0.81%. Intra-assay CV: 1.04% (low level, and 0.78% (high level. Bias against target value=2.332%. Linearity: r2=0.998 in the concentration range 4.4−13.9%HbA1c. Carry-over: 0.0024%. Conclusions: The Bio-Rad D-100 shows good correlation with G8 and HA-8180V. There is a small proportional systematic difference (2.7% and 5.6%, respectively in both comparisons. Inter and intra-assay CVs are both lower than the lowest CV obtained in studies performed with D-100 and other instruments. Keywords: Glycated hemoglobin, High performance liquid chromatography, Analyzer, Intra-assay variability, Inter-assay variability

  18. Radioimmunoguided surgery using iodine 125 B72.3 in patients with colorectal cancer

    International Nuclear Information System (INIS)

    Cohen, A.M.; Martin, E.W. Jr.; Lavery, I.; Daly, J.; Sardi, A.; Aitken, D.; Bland, K.; Mojzisik, C.; Hinkle, G.

    1991-01-01

    Preliminary data using B72.3 murine monoclonal antibody labeled with iodine 125 suggested that both clinically apparent as well as occult sites of colorectal cancer could be identified intraoperatively using a hand-held gamma detecting probe. We report the preliminary data of a multicenter trial of this approach in patients with primary or recurrent colorectal cancer. One hundred four patients with primary, suspected, or known recurrent colorectal cancer received an intravenous infusion of 1 mg of B72.3 monoclonal antibody radiolabeled with 7.4 x 10 Bq of iodine 125. Twenty-six patients with primary colorectal cancer and 72 patients with recurrent colorectal cancer were examined. Using the gamma detecting probe, 78% of the patients had localization of the antibody in their tumor; this included 75% of primary tumor sites and 63% of all recurrent tumor sites; 9.2% of all tumor sites identified represented occult sites detected only with the gamma detecting probe. The overall sensitivity was 77% and a predictive value of a positive detection was 78%. A total of 30 occult sites in 26 patients were identified. In patients with recurrent cancer, the antibody study provided unique data that precluded resection in 10 patients, and in another eight patients it extended the potentially curative procedure

  19. Development and Validation of Stability Indicating HPTLC and HPLC Methods for Simultaneous Determination of Telmisartan and Atorvastatin in Their Formulations

    Directory of Open Access Journals (Sweden)

    Kaliappan Ilango

    2013-01-01

    Full Text Available The present study describes development and subsequent validation of stability indicating HPLC and HPTLC methods for simultaneous estimation of Telmisartan (TLM and Atorvastatin (ATV in their combined formulation. The proposed RP-HPLC method utilizes a Phenomenex Luna C18 column using acetonitrile: 0.025 M ammonium acetate (38 : 52%, v/v as mobile phase (pH 3.8, flow rate of 1.0 mL/min. Quantification was achieved with UV detection at 281 nm over concentration range of 12 to 72 μg/mL for TLM and 3 to 18 μg/mL for ATV respectively. In HPTLC, separations were performed on silica gel 60 F254 using toluene-methanol-ethyl acetate-acetic acid (5 : 1 : 1 : 0.3, v/v as mobile phase. The compact bands of TLM and ATV at 0.37 ± 0.02 and 0.63 ± 0.01 respectively were scanned at 279 nm. Linear regression analysis revealed linearity in the range of 40 to 240 ng/band for TLM and 10 to 60 ng/band for ATV respectively. For both the methods, dosage form was exposed to thermal, photolytic, acid, alkali and oxidative stress. The methods distinctly separated the drugs and degradation products even in actual samples. In conclusion, the proposed HPLC and HPTLC methods were appropriate for routine quantification of TLM and ATV in tablet formulation.

  20. UPLC and HPLC of caffeoyl esters in wild and cultivated Arctium lappa L.

    Science.gov (United States)

    Haghi, Ghasem; Hatami, Alireza; Mehran, Mehdi

    2013-05-01

    Analytical methods including ultra-performance liquid chromatography (UPLC) and high-performance liquid chromatography (HPLC) with photodiode array (PDA) detector were developed for the analysis of caffeoylquinic acid derivatives in seeds, leaves and roots of Arctium lappa L. Separation was performed on C(18) column utilising 5% (v/v) acetic acid in water and acetonitrile at 330 nm. Both methodologies were validated in terms of linearity, precision, and recovery. The results showed that the major advantages of UPLC, over HPLC were the fast analysis, narrow peaks, high sensitivity, and reduction of solvent consumption. Subsequently the methods were applied for the identification and quantification of chlorogenic acid (5-CQA) and 1,5-dicaffeoylquinic acid (1,5-DCQA) as main compounds in samples. The total phenolic content of samples ranged from 3.93 to 14.13 g of 5-CQA equivalent/100g dry weight (DW). There was a significant variability from 89 to 571 mg/100g for 5-CQA and 48 to 486 mg/100g for 1,5-DCQA in dry material. Copyright © 2012 Elsevier Ltd. All rights reserved.

  1. Screening natural antioxidants in peanut shell using DPPH-HPLC-DAD-TOF/MS methods.

    Science.gov (United States)

    Qiu, Jiying; Chen, Leilei; Zhu, Qingjun; Wang, Daijie; Wang, Wenliang; Sun, Xin; Liu, Xiaoyong; Du, Fangling

    2012-12-15

    Peanut shell, a byproduct in oil production, is rich in natural antioxidants. Here, a rapid and efficient method using DPPH-HPLC-DAD-TOF/MS was used for the first time to screen antioxidants in peanut shell. The method is based on the hypothesis that upon reaction with 1, 1-diphenyl-2-picrylhydrazyl (DPPH), the peak areas of compounds with potential antioxidant activities in the HPLC chromatogram will be significantly reduced or disappeared, and the identity confirmation could be achieved by HPLC-DAD-TOF/MS technique. With this method, three compounds possessing potential antioxidant activities were found abundantly in the methanolic extract of peanut shell. They were identified as 5,7-dihydroxychromone, eriodictyol, and luteolin. The contents of these compounds were 0.59, 0.92, and 2.36 mg/g, respectively, and luteolin possessed the strongest radical scavenging capacity. DPPH-HPLC-DAD-TOF/MS assay facilitated rapid identification and determination of natural antioxidants in peanut shell, which may be helpful for value-added utilization of peanut processing byproducts. Copyright © 2012 Elsevier Ltd. All rights reserved.

  2. A technique to prepare boronated B72.3 monoclonal antibody for boron neutron capture therapy

    International Nuclear Information System (INIS)

    Ranadive, G.N.; Rosenzweig, H.S.; Epperly, M.W.

    1993-01-01

    B72.3 monoclonal antibody has been successfully boronated using mercaptoundecahydro-closo-dodecaborate (boron cage compound). The reagent was incorporated by first reacting the lysine residues of the antibody with m-maleimidobenzoyl succinimide ester (MBS), followed by Michael addition to the maleimido group by the mercapto boron cage compound to form a physiologically stable thioether linkage. Boron content of the antibody was determined by atomic absorption spectroscopy. For biodistribution studies, boronated antibody was radioiodinated with iodogen. 125 I-labeled and boronated B72.3 monoclonal antibody demonstrated clear tumor localization when administered via tail vein injections to athymic nude mice bearing LS174-T tumor xenografts. Boronated antibody was calculated to deliver 10 6 boron atoms per tumor cell. Although this falls short of the specific boron content originally proposed as necessary for boron neutron capture therapy (BNCT), recent calculations suggest that far fewer atoms of 10 B per tumor cell would be necessary to effect successful BNCT when the boron is targeted to the tumor cell membrane. (author)

  3. Future prospects of the international G-8 Global Partnership Programme

    International Nuclear Information System (INIS)

    Grigor'ev, A.V.; Esaulova, A.V.

    2012-01-01

    The Global Partnership Programme Against the Spread of Weapons and Materials of Mass Destruction was adopt at the Group-8 (G-8) summit on the 27-th of June 2002 for 10 years. At the G-8 summit in May 2011, the decision was made to extent the Global Partnership Programme to beyond 2012 and to expand its reach and geographical coverage. New areas for cooperation were named, such as: nuclear, radiological and biological safety, employment of scientists involved with sensitive industries and assistance to third countries in their compliance with the provisions of United Nations Security Council Resolution No 1540. The parties re-affirmed their commitment to completing a series of priority projects in Russia [ru

  4. Acquisition of HPLC-Mass Spectrometer

    Science.gov (United States)

    2015-08-18

    31-Jan-2015 Approved for Public Release; Distribution Unlimited Final Report: Acquisition of HPLC -Mass Spectrometer The views, opinions and/or findings...published in peer-reviewed journals: Final Report: Acquisition of HPLC -Mass Spectrometer Report Title The acquisition of the mass spectrometer has been a

  5. Comparison of GC-ICP-MS and HPLC-ICP-MS for species-specific isotope dilution analysis of tributyltin in sediment after accelerated solvent extraction

    International Nuclear Information System (INIS)

    Wahlen, Raimund; Wolff-Briche, Celine

    2003-01-01

    This study describes a direct comparison of GC and HPLC hyphenated to ICP-MS determination of tributyltin (TBT) in sediment by species-specific isotope dilution analysis (SS-IDMS). The certified reference sediment PACS-2 (NRC, Canada) and a candidate reference sediment (P-18/HIPA-1) were extracted using an accelerated solvent extraction (ASE) procedure. For comparison of GC and LC methods an older bottle of PACS-2 was used, whilst a fresh bottle was taken for demonstration of the accuracy of the methods. The data obtained show good agreement between both methods for both the PACS-2 sediment (LC-ICP-IDMS 828±87 ng g -1 TBT as Sn, GC-ICP-IDMS 848±39 ng g -1 TBT as Sn) and the P-18/ HIPA-1 sediment (LC-ICP-IDMS 78.0±9.7 ng g -1 TBT as Sn, GC-ICP-IDMS 79.2±3.8 ng g -1 TBT as Sn). The analysis by GC-ICP-IDMS offers a greater signal-to-noise ratio and hence a superior detection limit of 0.03 pg TBT as Sn, in the sediment extracts compared to HPLC-ICP-IDMS (3 pg TBT as Sn). A comparison of the uncertainties associated with both methods indicates superior precision of the GC approach. This is related to the better reproducibility of the peak integration, which affects the isotope ratio measurements used for IDMS. The accuracy of the ASE method combined with HPLC-ICP-IDMS was demonstrated during the international interlaboratory comparison P-18 organised by the Comite Consultatif pour la Quantite de Matiere (CCQM). The results obtained by GC-ICP-IDMS for a newly opened bottle of PACS-2 were 1087±77 ng g -1 Sn for DBT and 876±51 ng g -1 Sn for TBT (expanded uncertainties with a coverage factor of 2), which are in good agreement with the certified values of 1090±150 ng g -1 Sn and 980±130 ng g -1 Sn, respectively. (orig.)

  6. Synthesis and characterization of hyaluronic acid/human-like collagen hydrogels

    International Nuclear Information System (INIS)

    Zhang, Jingjing; Ma, Xiaoxuan; Fan, Daidi; Zhu, Chenhui; Deng, Jianjun; Hui, Junfeng; Ma, Pei

    2014-01-01

    Injectable hydrogel plays an important role in soft tissue filling and repair. We report an injectable hydrogel based on hyaluronic acid (HA) and human-like collagen (HLC), both with favorable biocompatibility and biodegradability. These two types of biomacromolecules were crosslinked with 1,4-butanediol diglycidyl ether to form a three-dimensional network. The redundant crosslinker was removed by dialysis and distillation. An HA-based hydrogel prepared by the same method was used as a control. The cytocompatibility was studied with a Cell Counting Kit-8 (CCK-8) test. Carbazole colorimetry was used to analyze the in vitro degradation rate. The histocompatibility was evaluated by hematoxylin and eosin (H and E) staining analysis and immunohistochemical analysis. The CCK-8 assay demonstrated that the HA/HLC hydrogel was less cytotoxic than the HA-based hydrogel and could promote baby hamster kidney cell (BHK) proliferation. The cell adhesion indicated that BHK could grow well on the surface of the materials and maintain good cell viability. The in vitro degradation test showed that the HA/HLC hydrogel had a longer degradation time and an excellent antienzyme ability. In vivo injection showed that there was little inflammatory response to HA/HLC after 1, 2, and 4 weeks. Therefore, the HA/HLC hydrogel is a promising biomaterial for soft tissue filling and repair. - Highlights: • Human-like collagen was used with hyaluronic acid to prepare soft tissue filling meterials. • 1,4-Butanediol diglycidyl ether (BDDE) was introduced to treat the hydrogels. • The addition of human-like collagen could improve the biological properties of hydrogels

  7. Synthesis and characterization of hyaluronic acid/human-like collagen hydrogels

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Jingjing; Ma, Xiaoxuan, E-mail: xiaoxuanma@163.com; Fan, Daidi, E-mail: fandaidi@nwu.edu.cn; Zhu, Chenhui; Deng, Jianjun; Hui, Junfeng; Ma, Pei

    2014-10-01

    Injectable hydrogel plays an important role in soft tissue filling and repair. We report an injectable hydrogel based on hyaluronic acid (HA) and human-like collagen (HLC), both with favorable biocompatibility and biodegradability. These two types of biomacromolecules were crosslinked with 1,4-butanediol diglycidyl ether to form a three-dimensional network. The redundant crosslinker was removed by dialysis and distillation. An HA-based hydrogel prepared by the same method was used as a control. The cytocompatibility was studied with a Cell Counting Kit-8 (CCK-8) test. Carbazole colorimetry was used to analyze the in vitro degradation rate. The histocompatibility was evaluated by hematoxylin and eosin (H and E) staining analysis and immunohistochemical analysis. The CCK-8 assay demonstrated that the HA/HLC hydrogel was less cytotoxic than the HA-based hydrogel and could promote baby hamster kidney cell (BHK) proliferation. The cell adhesion indicated that BHK could grow well on the surface of the materials and maintain good cell viability. The in vitro degradation test showed that the HA/HLC hydrogel had a longer degradation time and an excellent antienzyme ability. In vivo injection showed that there was little inflammatory response to HA/HLC after 1, 2, and 4 weeks. Therefore, the HA/HLC hydrogel is a promising biomaterial for soft tissue filling and repair. - Highlights: • Human-like collagen was used with hyaluronic acid to prepare soft tissue filling meterials. • 1,4-Butanediol diglycidyl ether (BDDE) was introduced to treat the hydrogels. • The addition of human-like collagen could improve the biological properties of hydrogels.

  8. Effects of hemoglobin variants HbJ Bangkok, HbE, HbG Taipei, and HbH on analysis of glycated hemoglobin via ion-exchange high-performance liquid chromatography.

    Science.gov (United States)

    Zhang, Xiu-Ming; Wen, Dong-Mei; Xu, Sheng-Nan; Suo, Ming-Huan; Chen, Ya-Qiong

    2018-01-01

    To explore the effects of HbJ Bangkok, HbE, HbG Taipei, and α-thalassemia HbH on the results of HbA1c assessment using ion-exchange high-performance liquid chromatography (IE-HPLC). We enrolled five patients in which the results of the IE-HPLC HbA1c assay were inconsistent with the average levels of FBG. We performed hemoglobin capillary (Hb) electrophoresis using whole-blood samples. We also sequenced the genes encoding Hb using dideoxy-mediated chain termination and analyzed HbA1c using borate affinity HPLC (BA-HPLC) and turbidimetric inhibition immunoassay (TINIA). Two patients had the HbJ Bangkok variant. Hb genotypes of these patients were β 41-42 /β J Bangkok and β N /β J Bangkok , and the content of HbJ Bangkok was 93.9% and 52.4%, respectively. The remaining three patients had the following: HbE (β N /β E Hb genotype, 23.6% HbE content), HbG Taipei (β N /β G Taipei Hb genotype, 39.4% HbG Taipei content), and α-thalassemia HbH (6.1% HbH content, 2.8% Hb Bart's content). In the patients with β-thalassemia and HbJ Bangkok variants, the presence of the variants interfered with the results of HbA1c analyses using IE-HPLC and TINIA; in the remaining four patients, there was interference with the results of HbA1c IE-HPLC but not with the TINIA assay. There was no interference with BA-HPLC HbA1c results. HbJ Bangkok, HbE, HbG Taipei Hb, and α-thalassemia HbH disease cause varying degrees of interference with the analysis of HbA1c using IE-HPLC. In these patients, we suggest using methods free from such interference for the analysis of HbA1c and other indicators to monitor blood glucose levels. © 2017 Wiley Periodicals, Inc.

  9. Functionalization of SU-8 photoresist surfaces with IgG proteins

    International Nuclear Information System (INIS)

    Blagoi, Gabriela; Keller, Stephan; Johansson, Alicia; Boisen, Anja; Dufva, Martin

    2008-01-01

    The negative epoxy-based photoresist SU-8 has a variety of applications within microelectromechanical systems (MEMS) and lab-on-a-chip systems. Here, several methods to functionalize SU-8 surfaces with IgG proteins were investigated. Fluorescent labeled proteins and fluorescent sandwich immunoassays were employed to characterize the binding efficiency of model proteins to bare SU-8 surface, SU-8 treated with cerium ammonium nitrate (CAN) etchant and CAN treated surfaces modified by aminosilanization. The highest binding capacity of antibodies was observed on bare SU-8. This explains why bare SU-8 in a functional fluorescent sandwich immunoassay detecting C-reactive protein (CRP) gave twice as high signal as compared with the other two surfaces. Immunoassays performed on bare SU-8 and CAN treated SU-8 resulted in detection limits of CRP of 30 and 80 ng/ml respectively which is sufficient for detecting CRP in clinical samples, where concentrations of 3-10 μg/ml are normal for healthy individuals. In conclusion, bare SU-8 and etched SU-8 can be modified with antibodies by a simple adsorption procedure which simplifies building lab-on-a-chip systems in SU-8. Additionally, we report the fabrication process and use of microwells created in a SU-8 layer with the same dimensions as a standard microscope glass slide that could fit into fluorescent scanners. The SU-8 microwells minimize the reagent consumption and are straightforward to handle compared to SU-8 coated microscope slides

  10. Use of small diameter column particles to enhance HPLC determination of histamine and other biogenic amines in seafood

    DEFF Research Database (Denmark)

    Simat, Vida; Dalgaard, Paw

    2011-01-01

    Pre-column and post-column HPLC derivatization methods were modified and evaluated for the identification and quantification of nine biogenic amines in seafood Two HPLC methods with column particles of 1 8 mu m or 3 mu m in diameter were modified and compared to classical methods using 5 mu m...... column particles Both pre-column derivatization with dansyl chloride and post-column derivatization with O-phthalaldehyde were studied The HPLC methods were compared with respect to the time of elution eluent consumption backpressure as well as separation sensitivity recovery and repeatability...... for determination of biogenic amines in lean canned tuna and fatty frozen herring The modified methods using smaller column particles of 1 8 mu m or 3 mu m allowed biogenic amines to be separated and quantified faster (23-59%) and with less eluent consumption (59-62%) than classical HPLC methods Backpressures were...

  11. A validated stability-indicating RP-HPLC method for paracetamol and lornoxicam: Application to pharmaceutical dosage forms

    Directory of Open Access Journals (Sweden)

    Karunakaran Kulandaivelu

    2014-01-01

    Full Text Available A new method for the simultaneous determination of paracetamol (PR and lornoxicam (LR has been developed by reversed phase HPLC from the combination drug product. The separation achieved on C18 column using acetonitrile and 0.02 M potassium dihydrogen phosphate was in the ratio of 35:65 (v/v as mobile phase at a flow rate of 1.0 mL/min. Both the components were monitored at a single wavelength at 260 nm and the column temperature was maintained at 30°C throughout the analysis. A linear response was found in the concentration range of 125-375 μg/mL for PR and 2-6 μg/mL for LR, with the correlation coefficient of more than 0.999. Although the tablet contained a high dose of PR (500 mg and a low dose of LR (8 mg, the single HPLC method was developed and the intra as well as inter day precision was obtained at less than 2% of RSD. The accuracy results obtained were between 98% and 102%. The drug was intentionally degraded under acidic, basic, peroxide, thermal, and photolytic conditions. The major degradation observed for both PR and LR under peroxide condition indicated that the drug product is susceptible to oxidation. The degraded peaks were properly resolved from PR and LR. Hence, the method is stability indicating.

  12. Distribution study of fatty acids (FAs) in sediments of Al-Kabeer Al-Shemali river estuary area using (HPLC) technique

    International Nuclear Information System (INIS)

    Nasser, M.; Ali, B.; Ali, A.

    2010-01-01

    Samples of sediments from fife sites of Al-kabeer Al-shemali river estuary area were collected during the period (22/2/2007-7/11/2007). The samples were extracted to determine their content of Fatty acids qualitatively and quantitatively by using ( HPLC) technique for determination resources of organic matter in studied sediments . The total concentrations of (FAs) varied from (0.36-1245.5μg/g dry weight).The saturated fatty acids were dominated in all samples (12.1 - 100 %) of total fatty acids. The levels of polyunsaturated fatty acids (PUFAs) were tested percent (0-18 %) of total fatty acids except one sample from surficial sediments in St 3 during 8/8/2007 .while the concentrations of monounsaturated fatty acids (MUFAs) were low (0 -21.6 %) of total fatty acids . We can use the saturated long chain fatty acid (C-22) as terrestrial biomarker. poly unsaturated fatty acid (C 1 8: 2ω6) as plankton biomarker and the Mono unsaturated fatty acid (C 1 8 : 1ω7) as bacterial biomarker.(author)

  13. Environmentally evaluated HPLC-ELSD method to monitor enzymatic synthesis of a non-ionic surfactant.

    Science.gov (United States)

    Gaber, Yasser; Akerman, Cecilia Orellana; Hatti-Kaul, Rajni

    2014-01-01

    N-Lauroyl-N-methylglucamide is a biodegradable surfactant derived from renewable resources. In an earlier study, we presented an enzymatic solvent-free method for synthesis of this compound. In the present report, the HPLC method developed to follow the reaction between lauric acid/methyl laurate and N-methyl glucamine (MEG) and its environmental assessment are described. Use of ultraviolet (UV) absorption or refractive index (RI) detectors did not allow the detection of N-methyl glucamine (MEG). With Evaporative light scattering detector ELSD, it was possible to apply a gradient elution, and detect MEG with a limit of detection, LOD = 0.12 μg. A good separation of the peaks: MEG, lauric acid, product (amide) and by-product (amide-ester) was achieved with the gradient program with a run time of 40 min. The setting of ELSD detector was optimized using methyl laurate as the analyte. LC-MS/MS was used to confirm the amide and amide-ester peaks. We evaluated the greenness of the developed method using the freely available software HPLC-Environmental Assessment Tool (HPLC-EAT) and the method got a scoring of 73 HPLC-EAT units, implying that the analytical procedure was more environmentally benign compared to some other methods reported in literature whose HPLC-EAT values scored up to 182. Use of ELSD detector allowed the detection and quantification of the substrates and the reaction products of enzymatic synthesis of the surfactant, N-lauroyl-N-methylglucamide. The developed HPLC method has acceptable environmental profile based on HPLC-EAT evaluation.

  14. G4beamline Simulations for H8

    CERN Document Server

    Thoresen, Freja

    2015-01-01

    Detailed simulations of the H8 beam line at the North Area, using the G4beamline software were performed in the framework of this study. The conventions used by the program are analysed. Having modelled precisely the beam line, several studies examining the beam transmission and composition were performed. The results were compared with measurements, where a satisfactory agreement was found. The muon production and transport is studied in details throughout the beam line.

  15. HPLC-DAD stability indicating determination of nizatidine in bulk and capsules dosage form

    Directory of Open Access Journals (Sweden)

    Tarek S. Belal

    2013-12-01

    Full Text Available This work describes the stability-indicating determination of the H2-receptor antagonist nizatidine in its bulk and capsules dosage form using high performance liquid chromatography coupled with diode array detector (HPLC-DAD. The developed method involved the use of Thermo Hypersil BDS-C8 (4.6 × 250 mm, 5 μm particle size column and a mobile phase composed of 0.05 M phosphoric acid and acetonitrile (50:50, v/v. The mobile phase was pumped at a flow rate of 1 mL/min. Quantification of nizatidine was based on measuring its peak area at 320 nm. The retention time for nizatidine was about 3.61 min. The reliability and analytical performance of the proposed HPLC procedure were statistically validated with respect to linearity, range, precision, accuracy, specificity, robustness, detection and quantification limits. Calibration curve of nizatidine was linear in the range of 5–50 μg/mL with correlation coefficient >0.9999. The drug was subjected to forced-degradation conditions of acidic and basic hydrolysis, oxidation, dry heat and UV photolysis where it showed considerable degradation in basic and oxidative conditions. The proposed method proved to be specific and stability-indicating by resolution of the drug from its forced-degradation products. The validated HPLC method was applied to the analysis of nizatidine in capsules dosage form where it was quantified with recoveries not less than 98.2%. Assay results were statistically compared to USP 2011 pharmacopeial method where no significant difference was observed between the proposed and reference methods.

  16. HPLC: Early and Recent Perspectives.

    Science.gov (United States)

    Karger, Barry L.

    1997-01-01

    Provides a perspective on what it was like in the early days of high-performance liquid chromatography (HPLC) and several of the key developments. Focuses on the advances in HPLC generally, and more specifically for the biological sciences, that were necessary for the method to reach the preeminent stage of today. Contains 20 references. (JRH)

  17. Simultaneous determination of phenolic acids and flavonoids in Chenopodium formosanum Koidz. (djulis) by HPLC-DAD-ESI-MS/MS.

    Science.gov (United States)

    Hsu, B Y; Lin, S W; Inbaraj, B Stephen; Chen, B H

    2017-01-05

    A high performance liquid chromatography-diode array detection-tandem mass spectrometry method (HPLC-DAD-MS/MS) was developed for simultaneous determination of phenolic acids and flavonoids in djulis (Chenopodium formosanum Koidz.), a traditional Chinese herb reported to possess vital biological activities. A high yield of phenolic acids and flavonoids was attained by employing 50% ethanol in water as the extraction solvent and shaking in a 60°C water bath for 3h. A total of 8 phenolic acids and 14 flavonoids were separated and identified within 55min by using a Poroshell 120 EC-C18 column with detection at 280nm, flow rate at 0.8mL/min, column temperature at 35°C, and a gradient solvent system of 0.1% formic acid in water and acetonitrile. Two internal standards caffeic acid and kaempferol-3-O-rutinoside were used for quantitation of phenolic acids and flavonoids in djulis respectively. The amounts of phenolic acids ranged from 11.5±0.8μg/g (caffeoyl-putrescine-derivative (2)) to 1855.3±16.9μg/g (hydroxylphenylacetic acid pentoside), while the flavonoids ranged from 19.93±2.29μg/g (quercetin-3-O-(coumaryl)-rutinoside-pentoside (1)) to 257.3±2.05μg/g (rutin-O-pentoside (2)). A high recovery (89.68-97.20%) and high reproducibility was obtained for both phenolic acids and flavonoids with the relative standard deviation (RSD) for the latter ranging from 0.09-8.22% (intra-day variability) and 0.80-8.48% (inter-day variability). This method may be applied to determination of both phenolic acids and flavonoids in food products and Chinese herbs. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Literatuuronderzoek HPLC-methoden voor vitamine E

    OpenAIRE

    Altena, A.; Hollman, P.C.H.

    1985-01-01

    Doel van dit onderzoek is: het inventariseren van HPLC-methoden voor vitamine E, eventueel in combinatie met vitamine A, in levensmiddelen. Een overzicht van de in de literatuur beschreven HPLC-methoden vanaf ca. 1977 wordt gegeven.

  19. G8 decision on fusion would herald nuclear future

    CERN Multimedia

    Starck, Peter

    2005-01-01

    Nuclear fusion as a future abundant energy source would receive a boost if G8 leaders agree next month on the site for the world's first fusion test reactor, two nuclear scientists said on Wednesday (1 page)

  20. An HPLC method for the determination of digoxin in dissolution samples

    Directory of Open Access Journals (Sweden)

    Milenković Miroslav Ž.

    2010-01-01

    Full Text Available An HPLC method for digoxin quantification in dissolution samples obtained as per the official British Pharmacopeia (BP method is presented in this paper. The chromatography was performed at 20 °C on a Symmetry C18; 3.5 ìm, 75 x 4.6 mm column with water - acetonitrile (72 : 28, v/v, as the mobile phase and UV detection at 220 nm. The method was found to be selective, linear, accurate and precise in the specified ranges. The LOD and LOQ were 0.015 μg mL-1 and 0.050 μg mL-1, respectively. Robustness testing was conducted to evaluate the impact of minor changes in the chromatographic parameters (i.e., acetonitrile fraction, flow rate of the mobile phase, column temperature and column length on the characteristics of the digoxin peak. A. full factorial design (24 was used to investigate the influence of the four variables The presented HPLC method was applied in quality and stability testing of Digoxin tablets 0.25 mg.

  1. G8+5 collaboration on energy efficiency and IPEEC: Shortcut to a sustainable future?

    International Nuclear Information System (INIS)

    Lesage, Dries; Van de Graaf, Thijs; Westphal, Kirsten

    2010-01-01

    In recent years, the G8+5 system has proven to be a major focal point of international cooperation in the field of energy efficiency. The G8 has set up multiple dialogues and collaborative frameworks with five emerging economies (China, India, Brazil, Mexico and South Africa) on energy and energy efficiency. The most prominent initiative so far is the creation of the International Partnership for Energy Efficiency Cooperation (IPEEC) in 2009. This article critically evaluates these joint efforts between the G8 and the 'Plus Five' on energy efficiency. More specifically, the purpose of this article is (1) to frame and explain the emergence of this kind of great-power cooperation; (2) to map G8+5 collaboration on energy efficiency; and (3) to provide a critical assessment of the relevance, impact and results of G8+5 initiated energy efficiency initiatives. The main conclusion is that the G8+5 system has performed better on the external dimension (steering global governance) than on the internal dimension (coordination of domestic policies) of global energy efficiency governance.

  2. Re-purification of labelled ferritin antigen with HPLC

    International Nuclear Information System (INIS)

    Zhang Haoyi; Jin Lichun

    2002-01-01

    Objective: To improve the quality of long-term stored labelled ferritin antigen with HPLC. Methods: The antigen was analyzed and purified with HPLC and again analyzed with RIA afterwards. Results: Ferritin antigen underwent significant polymerization after long-term (aggregation) storage. After re-purification with HPLC, its immuno-activity and labelled specific radioactivity were both significantly improved. Conclusion: Quality of stored ferritin RIA kit could be greatly improved after re-purification with HPLC

  3. HPLC for quality control of polyimides

    Science.gov (United States)

    Young, P. R.; Sykes, G. F.

    1979-01-01

    High Pressure Liquid Chromatography (HPLC) as a quality control tool for polyimide resins and prepregs are presented. A data base to help establish accept/reject criteria for these materials was developed. This work is intended to supplement, not replace, standard quality control tests normally conducted on incoming resins and prepregs. To help achieve these objectives, the HPLC separation of LARC-160 polyimide precursor resin was characterized. Room temperature resin aging effects were studied. Graphite reinforced composites made from fresh and aged resin were fabricated and tested to determine if changes observed by HPLC were significant.

  4. [Determination of aristolochic acid A in Radix Aristolociae and Herba Asari by RP-HPLC].

    Science.gov (United States)

    Jiang, Xu; Wang, Zhi-min; You, Li-shuan; Dai, Li-ping; Ding, Guang-zhi

    2004-05-01

    To develop a HPLC method to determine the contents of aristolochic A in aristolochia debilis and Asarun spp.. Methanol-water-formic acid extracts were separated on an Alltech C18 column with methanol-water-acetic acid (68:32:1) as mobile phase. The flow rate was 1.0 mL x min(-1). UV detection wavelength was 390 nm. Column temperature was 35 degrees C. Aristolochic acid A was separated well. The relationship of injection amounts and peak areas was linear (r = 0.9999) the range of 0.12-1.89 microg x g(-1) and the recovery rate was 101.8% (n = 5). 11 samples of aristolochia debilis which bought from different areas in China were determined, and the contents of aristolochic acid A varied from 0.9 to 2 mg x g(-1). The difference of the contents in Asarum spp. was obvious. The highest is 0.35, and aristolochic acid A couldn't be detected in one sample.

  5. HPLC profiling, antioxidant and in vivo anti-inflammatory activity of the ethanol extract of Syzygium jambos available in Bangladesh.

    Science.gov (United States)

    Hossain, Hemayet; Rahman, Shaikh Emdadur; Akbar, Proity Nayeeb; Khan, Tanzir Ahmed; Rahman, Md Mahfuzur; Jahan, Ismet Ara

    2016-03-28

    Syzygium jambos has been used as a traditional medicine for the treatment of inflammatory diseases in Bangladesh. The study investigates the high performance liquid chromatography (HPLC) profiling of phenolic compounds, and evaluates the antioxidant and anti-inflammatory activities of ethanol extract of S. jambos available in Bangladesh. The extract was subjected to HPLC for the identification and quantification of the major bioactive polyphenols present in S. jambos. Antioxidant activity was determined using 2, 2'-azino bis-3-ethylbenzothiazoline-6-sulfonic acid (ABTS) radical scavenging, reducing power assay, total antioxidant capacity, total phenolic and flavonoid content. Furthermore, the anti-inflammatory effect of the extract in rats for two different test models: carrageenan and histamine-induced paw edema was inspected. High levels of catechin hydrate and rutin hydrate (99.00 and 79.20 mg/100 g extract, respectively) and moderate amounts of ellagic acid and quercetin (59.40 and 69.30 mg/100 g extract, respectively) were quantified in HPLC. Catechin hydrate from this plant extract was determined for the first time through HPLC. For ABTS scavenging assay, the median inhibition concentration (IC50) value of S. jambos was 57.80 µg/ml, which was significant to that of ascorbic acid (12.01 µg/ml). The maximum absorbance for reducing power assay was found to be 0.4934. The total antioxidant capacity, phenolic and flavonoid contents were calculated to be 628.50 mg/g of ascorbic acid, 230.82 mg/g of gallic acid and 11.84 mg/g of quercetin equivalent, respectively. At a dose of 400 mg/kg, a significant acute anti-inflammatory activity (P antioxidant activities of S. jambos.

  6. Estimation of color of durum wheat. Comparison of WSB, HPLC, and reflectance colorimeter measurements.

    Science.gov (United States)

    Fratianni, Alessandra; Irano, Mario; Panfili, Gianfranco; Acquistucci, Rita

    2005-04-06

    Color is an important parameter involved in the definition of semolina and pasta quality. This character is mainly due to natural pigments (carotenoids) that are present at different levels in cereals and cereal products, due to botanical origin, growing conditions, distribution in the kernel, and technological processes. In food industries, color measurements are usually performed by means of automatic instruments that are rapid and safe, as alternatives to the chemical extraction methods. In this study, automatic measurements (CIE, color-space system L, a, b), water-saturated butanol (WSB), and HPLC determinations have been applied to evaluate the carotenoid content in whole meals and respective semolina samples produced from wheat cultivated in the years 2001 and 2002. In whole meals, total carotenoids, determined by HPLC, were about 3.0 microg/g (2001) and 3.5 microg/g (2002) calculated on dry weight (dw) and about 3.0 and 3.2 microg/g dw in corresponding semolina samples. The b values for the same period were 19.78 and 15.75, respectively, in raw materials and 20.03-21.67 in semolina. Results have confirmed lutein and beta-carotene as the main components mainly responsible for the yellow color in wheat grains. The ability of the index b to express natural dyeing was dependent on sample characteristics as demonstrated by the relationships found between this index and pigments, although the best correlation resulted between HPLC and WSB.

  7. Chemical characterization of neonicotinoids in surface waters by high performance liquid chromatography with Tandem Mass Spectrometry (HPLC MS/MS)

    International Nuclear Information System (INIS)

    Amaral, Priscila Oliveira

    2017-01-01

    The present study aimed to develop a method for the determination and validation of a method for the identification and quantification of Neonicotinoids in surface waters collected in the Bauru region, in the state of São Paulo. The analytical techniques studied for the development of this method were the high performance liquid chromatography with tandem mass spectrometry (HPLC - MS / MS), gas chromatography with mass spectrometry (GC / MS) and gas chromatography with electron capture detector (GC / ECD). The class of pesticides Neonicotinoids was chosen for this work because it is related to a sudden disappearance of bees in colonies around the world. This phenomenon is known as Colony Collapse Disorder (CCD) and it is characterized by a rapid loss in the population of adult bees. The Neonicotinoids used in this study were the compounds Clothianidin, Imidacloprid and Thiamethoxam which were banned in their use as pesticides in Europe by Implementing Regulation No. 540/2011. The samples were concentrated using solid phase extraction (SPE) and liquid liquid extraction (LLE) techniques and injected into HPLC-MS / MS, GC / MS and GC / ECD. The GC / ECD and GC / MS techniques were not satisfactory for determination in the water matrix because the detection limit (10 mg L -1 ) is above the maximum allowed by the US Environmental Protection Agency (0.6 μg L -1 ). The HPLC - MS / MS technique using the multiple reaction monitoring (MRM) proved to be adequate for this study because it obtained quantification limits between 5.89 and 8.06 μg L -1 and a linearity between 0.9963 and 0.9999 for the three compounds. (author)

  8. Glycyrrhiza glabra HPLC fractions: identification of Aldehydo Isoophiopogonone and Liquirtigenin having activity against multidrug resistant bacteria.

    Science.gov (United States)

    Rahman, Hazir; Khan, Ilyas; Hussain, Anwar; Shahat, Abdelaaty Abdelaziz; Tawab, Abdul; Qasim, Muhammad; Adnan, Muhammad; Al-Said, Mansour S; Ullah, Riaz; Khan, Shahid Niaz

    2018-05-02

    Medicinal plants have been founded as traditional herbal medicine worldwide. Most of the plant's therapeutic properties are due to the presence of secondary metabolites such as alkaloids, glycosides, tannins and volatile oil. The present investigation analyzed the High-Pressure Liquid Chromatography (HPLC) fractions of Glycyrrhiza glabra (Aqueous, Chloroform, Ethanol and Hexane) against multidrug resistant human bacterial pathogens (Escherichia coli, Acinetobacter baumannii, Staphylococcus aureus and Pseudomonas aeruginosa). All the fractions showed antibacterial activity, were subjected to LC MS/MS analysis for identification of bioactive compounds. Among total HPLC fractions of G. glabra (n = 20), three HPLC fractions showed potential activity against multidrug resistant (MDR) bacterial isolates. Fraction 1 (F1) of aqueous extracts, showed activity against A. baumannii (15 ± 0.5 mm). F4 from hexane extract of G. glabra showed activity against S. aureus (10 ± 0.2 mm). However, F2 from ethanol extract exhibited activity against S. aureus (10 ± 0.3 mm). These active fractions were further processed by LC MS/MS analysis for the identification of compounds. Ellagic acid was identified in the F1 of aqueous extract while 6-aldehydo-isoophiopogonone was present in F4 of hexane extract. Similarly, Liquirtigenin was identified in F2 of ethanol. Glycyrrhiza glabra extracts HPLC fractions showed anti-MDR activity. Three bioactive compounds were identified in the study. 6-aldehydo-isoophiopogonone and Liquirtigenin were for the first time reported in G. glabra. Further characterization of the identified compounds will be helpful for possible therapeutic uses against infectious diseases caused by multidrug resistant bacteria.

  9. Evaluation of the Sebia Capillarys 3 Tera and the Bio-Rad D-100 Systems for the Measurement of Hemoglobin A1c.

    Science.gov (United States)

    Herpol, Margaux; Lanckmans, Katrien; Van Neyghem, Stefaan; Clement, Pascale; Crevits, Stefanie; De Crem, Kim; Gorus, Frans K; Weets, Ilse

    2016-07-01

    We evaluated the Bio-Rad (Irvine, CA) D-100 and the Sebia (Lisses, France) Capillarys 3 Tera for the measurement of hemoglobin A1c (HbA1c) in venous blood samples. Whole-blood samples and control material were analyzed with the D-100 and Capillarys 3 Tera and compared with our routine method, HLC-723G7 (Tosoh, Tokyo, Japan). An evaluation protocol to test precision, trueness, linearity, carryover, and selectivity was set up according to Clinical and Laboratory Standards Institute guidelines. The results were presented in National Glycohemoglobin Standardization Program and International Federation of Clinical Chemistry (IFCC) units. Both systems showed excellent precision (total coefficients of variation hemoglobin (≤0.5 mmol/L potassium cyanate), hemoglobin variants, bilirubin (≤15 mg/dL), and triglycerides (≤3,360 mg/dL). The Bio-Rad D-100 and the Sebia Capillarys 3 Tera instruments performed well for the determination of HbA1c in terms of quality criteria as well as for sample throughput. © American Society for Clinical Pathology, 2016. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

  10. Screening of anti-HIV-1 inophyllums by HPLC-DAD of Calophyllum inophyllum leaf extracts from French Polynesia Islands.

    Science.gov (United States)

    Laure, Frédéric; Raharivelomanana, Phila; Butaud, Jean-François; Bianchini, Jean-Pierre; Gaydou, Emile M

    2008-08-22

    Various pyranocoumarins, calophyllolide, inophyllums B, C, G(1), G(2) and P, from Calophyllum inophyllum (Clusiaceae) leaves of French Polynesia (Austral, Marquesas, Society and Tuamotu archipelagos) have been determined in 136 leaf extracts using a high pressure liquid chromatography-UV-diode array detection (HPLC-UV-DAD) technique. Results show a wide range in chemical composition within trees growing on eighteen islands. The use of multivariate statistical analyses (PCA) shows geographical distribution of inophyllums and indicate those rich in HIV-1 active (+)-inophyllums. Inophyllum B and P contents (0.0-39.0 and 0.0-21.8 mg kg(-1), respectively) confirm the chemodiversity of this species within the large area of French Polynesia. The study suggests the presence of interesting chemotypes which could be used as plant source for anti-HIV-1 drugs.

  11. [Development of Tianma HPLC fingerprint and discriminant analysis].

    Science.gov (United States)

    Xiao, Jia-Jia; Huang, Hong; Lei, You-Cheng; Lin, Ting-Wen; Ma, Yue; Zhang, Jing; Zhang, Xing-Guo; Zhang, Da-Quan; Lv, Guang-Hua

    2017-07-01

    Tianma(the tuber of Gastrodia eleta) is a widely used and pricy Chinese herb. Its counterfeits are often found in herbal markets, which are the plant materials with similar macroscopic characteristics of Tianma. Moreover, the prices of Winter Tianma(cultivated Tianma) and Spring Tianma(mostly wild Tianma) have significant difference. However, it is difficult to identify the true or false, good or bad quality of Tianma samples. Thus, a total of 48 Tianma samples with different characteristics(including Winter Tianma, Spring Tianma, slice, powder, etc.) and 9 plant species 10 samples of Tianma counterfeits were collected and analyzed by HPLC-DAD-MS techniques. After optimizing the procedure of sample preparation, chromatographic and mass-spectral conditions, the HPLC chromatograms of all those samples were collected and compared. The similarities and Fisher discriminant analysis were further conducted between the HPLC chromatograms of Tianma and counterfeit, Winter Tianma and Spring Tianma. The results showed the HPLC chromatograms of 48 Tianma samples were similar at the correlation coefficient more than 0.848(n=48). Their mean chromatogram was simulated and used as Tianma HPLC fingerprint. There were 11 common peaks on the HPLC chromatograms of Tianma, in which 6 main peaks were chosen as characteristic peaks and identified as gastrodin, p-hydroxybenzyl alcohol, parishin A, parishin B, parishin C, parishin E, respectively by comparison of the retention time, UV and MS data with those of standard chemical compounds. All the six chemical compounds are bioactive in Tianma. However, the HPLC chromatograms of the 10 counterfeit samples were significantly different from Tianma fingerprint. The correlation coefficients between HPLC fingerprints of Tianma with the HPLC chromatograms of counterfeits were less than 0.042 and the characteristic peaks were not observed on the HPLC chromatograms of these counterfeit samples. It indicated the true or false Tianma can be

  12. The study of DNA adduct 8-hydroxy-2‧deoxyguanosine (8-OHdG) formation of butylated hydroxyanisole (BHA) and its metabolite ter-butyl hydroquinone (TBHQ) through in vitro reaction with Calf Thymus DNA and 2‧deoxyguanosine

    Science.gov (United States)

    Budiawan; Purwaningsih, S. S.; Cahaya, D. I.

    2017-04-01

    Butylated Hydroxyanisole (BHA) and its metabolite Tert-Butyl Hydroquinone (TBHQ) are synthetic antioxidants, commonly used as food and beverage preservatives. Although WHO declared their safety, the use of these preservatives are still controversial because some studies showed that BHA induced proliferative effects in animal testing and TBHQ is considered as carcinogenic and causes DNA cleavage. This study is aimed to analyze the interaction between Calf Thymus DNA with BHA and TBHQ which are mediated with Copper (II) Chloride. The result of the study in spectrophotometric showed there was bathochromic shift as much as 2-3 nm in DNA treated with TBHQ. The next analysis used HPLC method in stationary phase of ODS, mobile phase of 10mM Natrium Hydrogen Phosphate Buffer and Methanol (85 : 15) for DNA adduct formation, 8-Hydroxy-2-Deoxyguanosine (8-OHDG) as biomarker of risk cancer. The resultof the study showed the formation of DNA adduct 8-OHDG in the interaction between DNA and 20-500 ppm of TBHQ. The 8-OHdG formation was greatly increased by the higher concentration of TBHQ. The relative amount of 8 OHDG which formed was reached 946/105 deoxyguanosine in DNA bases. Confirmation test by LCMS/MS was characterized with the detection of mother ion peak (m/z 284); fragment ion peaks at m/z 167.9, and 139.9; at retention time 3.52 min. Meanwhile the interaction between DNA and 50-250 ppm BHA did not induce 8-OHDG.

  13. The southern molecular environment of SNR G18.8+0.3

    OpenAIRE

    Paron, S.; Peña, M. Celis; Ortega, M. E.; Petriela, A.; Dubner, G.; Giacina, E.; Rubio, M.

    2015-01-01

    In a previous paper we have investigated the molecular environment towardsthe eastern border of the SNR G18.8+0.3. Continuing with the study of thesurroundings of this SNR, in this work we focus on its southern border, whichin the radio continuum emission shows a very peculiar morphology with acorrugated corner and a very flattened southern flank. We observed two regionstowards the south of SNR G18.8+0.3 using the Atacama Submillimeter TelescopeExperiment (ASTE) in the 12CO J=3-2. One of thes...

  14. Speciation of selenoamino acids, selenonium ions and inorganic selenium by ion exchange HPLC with mass spectrometric detection and its application to yeast and algae

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Hansen, M.; Fan, T.

    2001-01-01

    Cation and anion exchange HPLC were used to separate a mixture of 12 selenium species comprising selenoamino acids, selenonium ions and inorganic selenium. The cationic species were separated from each other and from the co-injected anions using a cation exchange column with gradient elution...... by aqueous pyridinium formate at pH similar to 3 as the mobile phase. The anionic species were separated using an anion exchange column with isocratic elution by an aqueous salicylate-TRIS mobile phase at pH 8.5. The separated selenium species were detected as Se-80 by ICP-dynamic reaction cell (DRC...... acid extract of Chlorella algae contained dimethylselenonium propionate (DMSeP), which was verified by HPLC-ES-MS. Se-allylselenocysteine and selenoethionine was detected at the low ng g(-1) concentration level based on co-chromatography with the standard substances spiked to the algal extract....

  15. Determination of Arctiin and Arctigenin Contents in Arctium Tomentosum Mill. by HPLC Method

    Directory of Open Access Journals (Sweden)

    Xiaoying Zhou

    2011-01-01

    Full Text Available A simple, precise, rapid and accurate, binary-phase high performance liquid chromatographic method has been developed for the determination of arctiin and arctigenin contents in the Arctium tomentosumMill. with short run time. Chromatographic separation was achieved by using HPLC system, consisting of a Shimadzu LC-6AD and Kromasil C18 column (250×4.6 mm, 5 μm, with pre-column, the mobile phase consists of methanol and water (55: 45. Detection wavelength was 280 nm. The speed of flow was 1.0 mL/min. The specimen handing quantity was 10 μL. The arctiin’s linearity range was 1.575∼4.725 μg (r=0.9995. The arctigenin’s linearity range was 0.613, 3.063 μg (r = 0.9998 and the linear relationship was accurate. The average recovery (n=5 of arctiin and arctigenin were 101.55% (RSD=2.23% 101.63% (RSD =1.49 % respectively. The contents of arctiin and arctigenin in Arctium tomentosum Mill. were 10.69 mg/g and 0.15 mg/g, respectively. Therefore, the developed HPLC method can be applied to both in vitro studies of arctiin and arctigenin formulations as well as drug estimation in biological samples.

  16. HPLC ‘Multi-Analyte’ Detection Method

    Energy Technology Data Exchange (ETDEWEB)

    Dudar, E. [Plant Protection & Soil Conservation Service of Budapest, Budapest (Hungary)

    2009-07-15

    The application of multi-analyte methods for pesticides carrying chromophoric structures by HPLC is described. Details are given on the materials and methods used. Recorded UV spectra of active substances are presented for allowing the verification of purity and the confirmation of substances eluting from the HPLC column. (author)

  17. HPLC ANALYSIS FOR DETERMINATION OF CHARACTERISTICS OF FRUCTO-OLIGOSACCHARIDE SYRUPS EXTRACTED FROM JERUSALEM ARTICHOKE

    Directory of Open Access Journals (Sweden)

    Sibel (YİĞİTARSLAN YILDIZ

    2009-02-01

    Full Text Available Abstract: This study was aimed to assess the feasibility of extracting fructo-oligosaccharides (degree of polymerization of 3-6 from jerusalem artichoke tubers by solvent extraction. Together with harvest date, storage time, and peeling of the raw material it was also investigated the influence of some process parameters on final dry matter, degree of polymerization and product profile of the extracts: time (10-60 min, temperature (40-80 °C, amount of solvent (30-50 ml and citric acid concentration (0-39 mmol/L. HPLC analysis showed that the most functional extracts (2.33 were obtained with mid-February harvested, 20 day-stored whole jerusalem artichoke tubers extracted with 40 ml of water containing 26 mmol/L citric acid at 60 °C for 40 min. Under those conditions, syrups with 17g of dry matter and degree of polymerization of 6 were produced. The density, viscosity, darkness and color of the syrups were found as 0.98 g/ml, 1.1 mPa-s, 0.38, and 13.3, respectively. Keywords: Fructo-oligosaccharides, HPLC, inulin, extraction, jerusalem artichoke YER ELMASINDAN ÖZÜTLENEN FRÜKTO-OLİGOSAKKARİT ŞURUPLARININ KARAKTERİSTİK ÖZELLİKLERİNİN HPLC ANALİZİ İLE BELİRLENMESİ Özet: Bu çalışmada, yer elmasından, çözücü özütleme yöntemiyle frükto-oligosakkaritlerin (polimerizasyon derecesi 3-6 özütlenebilirliğinin fizibilitesinin tayini amaçlanmıştır. Hasat zamanı, depolama süresi ve ham maddenin soyulmasının etkilerinin yanı sıra diğer bazı proses parametrelerinin (zaman (10-60 dak, sıcaklık (40-80°C, çözücü miktarı (30-50 ml ve sitrik asit derişimi (0-39 mmol/L de sonuçtaki kuru madde, polimerizasyon derecesi ve özütteki ürün profili üzerindeki etkileri incelenmiştir. HPLC analizleri, en fonksiyonel özütün (2,33 Şubat ayı ortalarında hasat edilmiş, 20 gün depolanmış, soyulmamış yer elması yumrularının, 26 mmol/L sitrik asit içeren 40 ml suyla, 60 °C'de 40 dakika süreyle

  18. Development and validation of an rp-hplc method for simultaneous determination of Ramipril and Amlodipine in tablets

    Directory of Open Access Journals (Sweden)

    Shi-Ying Dai

    2013-12-01

    Full Text Available An rp-hplc method for the simultaneous determination of Ramipril (RP and Amlodipine (AL in tablets was developed and validated by Chinese Pharmacopoeia 2010. The linearity of the proposed method was investigated in the range of 0.01–0.25 mg/mL (r2=0.9998 for RP and 0.014–0.36 mg/mL (r2=0.9997 for AL. The limits of detection (LOD were 0.06 μg/mL and 0.02 μg/mL for RP and AL, and the limits of quantitation (LOQ were 0.2 μg/mL and 0.07 μg/mL, respectively. Some major impurities and degradation products did not disturb the detection of RP and AL and the assay can thus be considered stability-indicating. Keywords: Ramipril, Amlodipine, RP-HPLC, Stability-indicating

  19. Quantitative analysis of d,1-HMPAO and its freeze-dried kit with HPLC

    International Nuclear Information System (INIS)

    Chen Suzhen

    1993-05-01

    A quantitative analysis method, which uses RP-HPLC (reversed phase-high performance liquid chromatography), has been established to determine the stereoisomeric purity of HMPAO and d,1-HMPAO content for d,l-HMPAO freeze-dried kit. An opitmal mobile phase is selected for obtaining chromatographic parameters that are better than those published in the references. The theoretical tray height is less than 0.06 mm. At the flowrate of 1 ml/min the total separation time is 5.5. The resolution is greater than 5. The detectable limits of meso-HMPAO and d,l-HMPAO are 1 x 10 -8 g and 5 x 10 -7 g respectively. The precision is 5% and the additional recovery is 94% ∼ 107%. This method has many advantages such as accuracy, simplicity, rapidity and stability, and it is suitable for routine inspection. It has been successfully used to determine the HMPAO stereoisomer and d,1-HMPAO of freeze-dried kit produced by China Institute of Atomic Energy and same products imported from Amersham Company of United Kingdom

  20. 檀香叶中的γ-氨基丁酸的HPLC测定研究%Determination of γ-Aminobutyric Acid in Leaves of Santalum album L.by HPLC

    Institute of Scientific and Technical Information of China (English)

    杨艳; 贺丽苹; 高向阳

    2013-01-01

    A method was established by reversed-phase high performance liquid chromatography for determining the content of y-aminobutyric acid ( GABA) in leaves of Santalum album L. The sample was pretreated by soxhlet extraction to eliminate the pigments with ether, and then by water extraction and alcohol precipitation to eliminate sugar and protein. GABA was derivatized with dansyl chloride (Dns-Cl) and isolated by reversed-phase HPLC. GABA was detected quantitatively by HPLC with fluorescence detection. Nice linear relationship between peak area and concentration was obtained with the linear regression equation as y=475 211x+69 037,R2 =0.999 8. The recovery of standard addition was in the range of 112% to 120%. The detection limit of GABA was 7 μg/g. The established HPLC method is simple, economic, stable and accurate with good reproducibility. It can be applied on determination of GABA in leaves of Santalum album L.%建立了檀香叶中γ-氨基丁酸(GABA)含量的高效液相色谱检测方法.以乙醚为溶剂,采用索氏提取除去色素,水提醇沉去除糖类和蛋白质的净化方法,以丹酰氯为衍生剂,高效液相色谱法分离,荧光检测器测定,外标法定量.峰面积与浓度之间线性关系良好,回归方程为y=475 211x+ 69 037,R2=0.999 8,加标回收率为112 %~120%,检测限为7μg/g.该方法操作步骤简单,灵敏度高,用于檀香叶中GABA的检测,方法简便、准确、高效.

  1. HPLC-DAD-MS/MS profiling of phenolics from Securigera securidaca flowers and its anti-hyperglycemic and anti-hyperlipidemic activities

    Directory of Open Access Journals (Sweden)

    Rana M. Ibrahim

    Full Text Available Abstract Securigera securidaca (L. Degen & Döefl., Fabaceae, has been widely used in the Iranian, Indian and Egyptian folk medicine as antidiabetic and anti-hyperlipidemic remedy. Phenolic profiling of the ethanolic extract (90% of the flowers of S. securidaca was performed via HPLC-DAD-MS/MS analysis in the positive and negative ion modes. The total polyphenols and flavonoids in the flowers were determined colorimetrically, and the quantification of their components was carried out using HPLC-UV. Total phenolics and flavonoids estimated as gallic acid and rutin equivalents were 82.39 ± 2.79 mg/g and 48.82 ± 1.95 mg/g of the dried powdered flowers, respectively. HPLC-DAD-MS/MS analysis of the extract allowed the identification of 39 flavonoids and eight phenolic acids. Quantitative analysis of some flavonoids and phenolics (mg/100 g powdered flowers revealed the presence of isoquercetrin (3340 ± 2.1, hesperidin (32.09 ± 2.28, naringin (197.3 ± 30.16, luteolin (10.247 ± 0.594, chlorogenic acid (84.22 ± 2.08, catechin (3.94 ± 0.57 and protocatechuic acid (34.4 ± 0.15, in the extract. Moreover, the acute toxicity, hypoglycemic and hypolipidemic effects of the extract were investigated using alloxan induced diabetes in rats in a dose of 100, 200, and 400 mg/kg bwt. The ethanolic extract was safe up to a dose of 2000 mg/kg. All tested doses of the flower extract showed marked decrease in blood glucose level by 31.78%, 66.41% and 63.8% at 100, 200 and 400 mg/kg bwt, respectively, at p < 0.05. Regarding the anti-hyperlipidemic effect, a dose of 400 mg/kg of the flower extract showed the highest reduction in serum triacylglycerides and total cholesterol levels (68.46% and 51.50%, respectively at p < 0.05. The current study proved the folk use of the flowers of S. securidaca as anti-diabetic and anti-hyperlipidemic agent which could be attributed to its high phenolic content.

  2. 723-IJBCS-Article-Marie Nicole Chaungneu G.

    African Journals Online (AJOL)

    DR GATSING

    1 déc. 2005 ... 2 Musée Ecologique du Millénaire (Muséum d'histoire naturelle). ... Une telle approche de gestion pourrait être mise en application dans le cadre des concessions forestières, .... des ressources dans les espaces agroforestiers ..... autres PFNL à l'exemple de trois principaux ...... DUNOD: Paris, France.

  3. Phylogenetic analysis of G1P[8] and G12P[8] rotavirus A samples obtained in the pre- and post-vaccine periods, and molecular modeling of VP4 and VP7 proteins.

    Science.gov (United States)

    Almeida, Tâmera Nunes Vieira; de Sousa, Teresinha Teixeira; da Silva, Roosevelt Alves; Fiaccadori, Fabíola Souza; Souza, Menira; Badr, Kareem Rady; de Paula Cardoso, Divina das Dôres

    2017-09-01

    Reduction in morbimortality rates for acute gastroenteritis (AGE) by Rotavirus A (RVA) has been observed after the introduction of vaccines, however the agent continues to circulate. The present study described the genomic characterization of the 11 dsRNA segments of two RVA samples G1P[8] obtained in the pre- and post-vaccination periods and one of G12P[8] sample (post-vaccine), compared to Rotarix™ vaccine. Analysis by molecular sequencing of the samples showed that the three samples belonged to genogroup I. In addition, the analysis of VP7 gene revealed that the samples G1 (pre-vaccine), G1 (post-vaccine) and G12 were characterized as lineages II, I and III, respectively. Regarding to VP4 and NSP4 gene it was observed that all samples belonged to lineage III, whereas for VP6 gene, the sample of the pre- and post-vaccine belonged to the lineage IV and I, respectively. Considering the VP7 gene, it was observed high nucleotide and amino acid identity for the two G1 samples when compared to Rotarix™ vaccine and lesser identity for the G12 sample. In relation to antigenic epitope of VP7 greater modifications were observed for the G12 sample in the 7-2 epitope that was confirmed by molecular modeling. On the other hand, for VP4, some changes in the 8-1 and 8-3 antigenic epitopes was observed for the three samples. This data could be interpreted as a low selective pressure exerted by vaccination in relation to G1P[8] samples and lesser protection in relation to G12P[8]. Thus, the continuous monitoring of RVA circulating samples remains important. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Multidimensional health locus of control and depressive symptoms in the multi-ethnic population of the Netherlands.

    Science.gov (United States)

    van Dijk, Tobias K; Dijkshoorn, Henriëtte; van Dijk, Ad; Cremer, Stephan; Agyemang, Charles

    2013-12-01

    Ethnic inequalities in health in Western societies are well-documented but poorly understood. We examined associations between health locus of control (HLC) and depressive symptoms among native and non-native Dutch people in the Netherlands. We used hierarchical multiple linear regression analyses on a representative sample of the multi-ethnic population of Amsterdam and The Hague (n = 10,302). HLC was measured with the multidimensional health locus of control scale. Depressive symptoms were measured with the Kessler Psychological Distress scale. Multivariate analyses showed that HLC contributes to ethnic differences in the prevalence of depressive symptoms. Respondents who scored high on external locus of control (PHLC) were more likely to have depressive symptoms than those with a low score on PHLC (β = 0.133, p locus of control (IHLC) were less likely to have depressive symptoms compared to those scoring low on IHLC (β = -0.134, p < 0.001). The associations were most pronounced among Turkish-Dutch and Moroccan-Dutch respondents. Our findings suggest that HLC contributes to ethnic inequalities in depressive symptoms, especially among Turkish and Moroccan ethnic groups. Professionals (e.g. clinicians and policy makers) need to take HLC into account when assessing and treating depression among ethnic minority groups, particularly in Turkish and Moroccan populations. Future research should look further into the associations within these groups.

  5. H-2g, a glucose analog of blood group H antigen, mediates monocyte recruitment in vitro and in vivo via IL-8/CXCL8

    Directory of Open Access Journals (Sweden)

    Rabquer BJ

    2012-09-01

    Full Text Available Bradley J Rabquer,1,2 Yong Hou,1 Jeffrey H Ruth,1 Wei Luo,1 Daniel T Eitzman,1 Alisa E Koch,3,1 Mohammad A Amin11University of Michigan Medical School, Department of Internal Medicine, Ann Arbor, MI, USA; 2Albion College, Biology Department, Albion, MI, USA; 3VA Medical Service, Department of Veterans Affairs, Ann Arbor, MI, USAObjective: Monocyte (MN recruitment is an essential inflammatory component of many autoimmune diseases, including rheumatoid arthritis (RA. In this study we investigated the ability of 2-fucosyllactose (H-2g, a glucose analog of blood group H antigen to induce MN migration in vivo and determined if H-2g-induced interleukin-8 (IL-8/CXCL8 plays a role in MN ingress in RA.Methods: Sponge granuloma and intravital microscopy assays were performed to examine H-2g-induced in vivo MN migration and rolling, respectively. MNs were stimulated with H-2g, and the production of IL-8/CXCL8 was assessed by enzyme-linked immunosorbent assay and quantitative polymerase chain reaction. Lastly, in vitro MN migration assays and an in vivo RA synovial tissue severe combined immunodeficiency mouse model were used to determine the role of IL-8/CXCL8 in H-2g-induced MN migration.Results: In vivo, H-2g induced significantly greater MN migration compared to phosphate buffered saline. Intravital microscopy revealed that H-2g mediates MN migration in vivo by inducing MN rolling. In addition, H-2g induced MN production of IL-8/CXCL8, a process that was dependent on Src kinase. Moreover, we found that H-2g mediated MN migration in vitro, and in vivo migration was inhibited by a neutralizing anti-IL-8/CXCL8 antibody.Conclusion: These findings suggest that H-2g mediates MN recruitment in vitro and in vivo (in part via IL-8/CXCL8.Keywords: inflammation, rheumatoid arthritis, chemokine, migration

  6. The G8 global partnership against proliferation

    International Nuclear Information System (INIS)

    Devaux, O.

    2003-01-01

    Launched in 2002, the G8 global partnership against the proliferation of massive destruction weapons will contribute up to 20 billion dollars to the dismantling of the nuclear and chemical weapons of the former USSR (20000 nuclear warheads stored in 123 sites, 1350 tons of weapon grade plutonium and enriched uranium, 40000 tons of chemical agents, 190 decommissioned nuclear submarines etc..). This partnership, which has entered its realization phase, inaugurates a new cooperation with the Russian Federation. I could be used tomorrow in other regions of the world and become an instrument of the international community for the fight against proliferation. (J.S.)

  7. G8 global partnership. France's contribution

    International Nuclear Information System (INIS)

    2005-09-01

    During the G8 summit at Kananaskis (Canada) in June 2002, G8 Leaders decided to launch the Global Partnership against the Spread of Weapons and Materials of Mass Destruction. Under this initiative, partners support specific cooperation projects to address non-proliferation, disarmament, counter-terrorism and nuclear safety issues. Since then, thirteen other donor countries have joined the initiative from which the Ukraine may also now benefit. France intends to make an effective contribution, up to 750 million euros, to the implementation of this initiative, giving priority to a genuine partnership between France and Russia covering projects in the nuclear, chemical and biological fields. France intends to be involved in the various fields identified at Kananaskis: in the nuclear field, it is participating in nuclear submarine dismantling actions and contributes to the improvement of nuclear safety and security. It also supports the program for the disposition of Russian weapons-grade plutonium designated as no longer required for defence purposes. France is also involved in the destruction of chemical weapons and intends to develop responses to bio-terrorist threats, while promoting reemployment of scientists. To optimise its action, France has committed itself to both multilateral and bilateral programs. In the multilateral framework, France contributes to: - the NDEP fund (Northern Dimension Environment Partnership) which will finance projects related to the dismantling of nuclear submarines and remediation of the sites concerned; - the MPDG (Multilateral Plutonium Disposition Group), whose objective is to enable the disposition of Russian weapons-grade plutonium designated as no longer required for defence purposes; - the construction of the new Chernobyl shelter in the Ukraine. France is also developing bilateral cooperation, primarily with Russia: - in the nuclear field, the implementing agreement negotiated in the framework of the Multilateral Environmental

  8. Simplified RP-HPLC method for multi-residue analysis of abamectin, emamectin benzoate and ivermectin in rice.

    Science.gov (United States)

    Xie, Xianchuan; Gong, Shu; Wang, Xiaorong; Wu, Yinxing; Zhao, Li

    2011-01-01

    A rapid, reliable and sensitive reverse-phase high-performance liquid chromatography method with fluorescence detection (RP-FLD-HPLC) was developed and validated for simultaneous analysis of the abamectin (ABA), emamectin (EMA) benzoate and ivermectin (IVM) residues in rice. After extraction with acetonitrile/water (2 : 1) with sonication, the avermectin (AVMs) residues were directly derivatised by N-methylimidazole (N-NMIM) and trifluoroacetic anhydride (TFAA) and then analysed on RP-FLD-HPLC. A good linear relationship (r(2 )> 0.99) was obtained for three AVMs ranging from 0.01 to 5 microg ml(-1), i.e. 0.01-5.0 microg g(-1) in rice matrix. The limit of detection (LOD) and the limit of quantification (LOQ) were between 0.001 and 0.002 microg g(-1) and between 0.004 and 0.006 microg g(-1), respectively. Recoveries were from 81.9% to 105.4% and precision less than 12.4%. The proposed method was successfully applied to routine analysis of the AVMs residues in rice.

  9. Quantification of 3-nitrobenzanthrone-DNA adducts using online column-switching HPLC-electrospray tandem mass spectrometry.

    Science.gov (United States)

    Gamboa da Costa, Gonçalo; Singh, Rajinder; Arlt, Volker M; Mirza, Amin; Richards, Meirion; Takamura-Enya, Takeji; Schmeiser, Heinz H; Farmer, Peter B; Phillips, David H

    2009-11-01

    The aromatic nitroketone 3-nitrobenzanthrone (3-nitro-7H-benz[de]anthracen-7-one; 3-NBA) is an extremely potent mutagen and a suspected human carcinogen detected in the exhaust of diesel engines and in airborne particulate matter. 3-NBA is metabolically activated via reduction of the nitro group to the hydroxylamine (N-OH-3-ABA) to form covalent DNA adducts. Thus far, the detection and quantification of covalent 3-NBA-DNA adducts has relied solely on (32)P-postlabeling methodologies. In order to expand the range of available techniques for the detection and improved quantification of 3-NBA-DNA adducts, we have developed a method based upon online column-switching HPLC coupled to electrospray tandem mass spectrometry, with isotopic dilution of (15)N-labeled internal standards. This methodology was applied to the determination of three 3-NBA-derived adducts: 2-(2'-deoxyguanosin-N(2)-yl)-3-aminobenzanthrone (dG-N(2)-3-ABA), N-(2'-deoxyguanosin-8-yl)-3-aminobenzanthrone (dG-C8-N-3-ABA) and 2-(2'-deoxyguanosine-8-yl)-3-aminobenzanthrone (dG-C8-C2-3-ABA). Dose-dependent increases were observed for all three adducts when salmon testis DNA was reacted with N-acetoxy-3-aminobenzanthrone (N-AcO-3-ABA). dG-C8-C2-3-ABA was detected at much lower levels (overall 1%) than the other two adducts. DNA samples isolated from tissues of rats treated either intratracheally with 3-NBA or intraperitoneally with N-OH-3-ABA were analyzed by mass spectrometry, and the results compared to those obtained by (32)P-postlabeling. The method required 50 microg of hydrolyzed animal DNA on column and the limit of detection was 2.0 fmol for each adduct. dG-C8-C2-3-ABA was not observed in any of the samples providing confirmation that it is not formed in vivo. Linear regression analysis of the levels of dG-N(2)-3-ABA and dG-C8-N-3-ABA in the rat DNA showed a reasonable correlation between the two methods (R(2) = 0.88 and 0.93, respectively). In summary, the mass spectrometric method is a faster, more

  10. Functionalization of SU-8 Photoresist Surfaces with IgG Proteins

    DEFF Research Database (Denmark)

    Blagoi, Gabriela; Keller, Stephan Urs; Johansson, Alicia

    2008-01-01

    immunoassays were employed to characterize the binding efficiency of model proteins to bare SU-8 surface, SU-8 treated with cerium ammonium nitrate (CAN) etchant and CAN treated surfaces modified by aminosilanization. The highest binding capacity of antibodies was observed on bare SU-8. This explains why bare...... SU-8 in a functional fluorescent sandwich immunoassay detecting C-reactive protein (CRP) gave twice as high signal as compared with the other two surfaces. Immunoassays performed on bare SU-8 and CAN treated SU-8 resulted in detection limits of CRP of 30 and 80 ng/ml respectively which is sufficient...... for detecting CRP in clinical samples, where concentrations of 3–10 μg/ml are normal for healthy individuals. In conclusion, bare SU-8 and etched SU-8 can be modified with antibodies by a simple adsorption procedure which simplifies building lab-on-a-chip systems in SU-8. Additionally, we report the fabrication...

  11. Towards multimodal HPLC separations on humic acid-bonded aminopropyl silica: RPLC and HILIC behavior.

    Science.gov (United States)

    Gezici, Orhan; Kara, Hüseyin

    2011-09-15

    The stationary phase characteristics of the material obtained through immobilization of humic acid (HA) to aminopropyl silica (APS) via amide-bond formation were investigated. The material was characterized in terms of elemental analysis, FTIR, thermogravimetric analyses, pH point of zero charge measurements, potentiometric titrations, and contact angle measurements. Amount of HA bonded to APS was determined from the elemental analysis results, and found as 170 mgHA/gAPS. Stability of the material was studied in aqueous media at different pH values, and amount of HA released at pH=8 did not exceed 2% of the total immobilized HA. Stationary phase characteristics of the well-characterized material were investigated in an HPLC system by using some low-molecular weight polar compounds (i.e. some nucleosides and nucleobases) as test solutes. Effect of some experimental variables such as column conditioning, composition of mobile phase, and temperature on the chromatographic behavior of the studied compounds was studied. Role of ammonium solutions at different pH values on retentive properties of the species was also studied. Retention factors (k') versus volume percentage of organic modifier exhibited a U-curve, which was evaluated as an indication for RPLC/HILIC mixed-mode behavior of the stationary phase. Orthogonality between RPLC and HILIC modes was analyzed through geometric approach, and found as 48.5%. Base-line separation for the studied groups of compounds was achieved under each studied mode, and some differentiations were observed in elution order of the compounds depending on the HPLC mode applied. Chromatograms recorded under RPLC and HILIC modes were compared with those recorded on APS under similar conditions, and thus the influence/importance of HA immobilization process was evaluated in detail. In light of the obtained results, immobilized HA is represented as a useful stationary phase for HPLC separations. Copyright © 2011 Elsevier B.V. All rights

  12. Combined HPLC-CUPRAC (cupric ion reducing antioxidant capacity) assay of parsley, celery leaves, and nettle.

    Science.gov (United States)

    Yildiz, Leyla; Başkan, Kevser Sözgen; Tütem, Esma; Apak, Reşat

    2008-10-19

    This study aims to identify the essential antioxidant compounds present in parsley (Petroselinum sativum) and celery (Apium graveolens) leaves belonging to the Umbelliferae (Apiaceae) family, and in stinging nettle (Urtica dioica) belonging to Urticaceae family, to measure the total antioxidant capacity (TAC) of these compounds with CUPRAC (cupric ion reducing antioxidant capacity) and ABTS spectrophotometric methods, and to correlate the TAC with high performance liquid chromatography (HPLC) findings. The CUPRAC spectrophotometric method of TAC assay using copper(II)-neocuproine (2,9-dimethyl-1,10-phenanthroline) as the chromogenic oxidant was developed in our laboratories. The individual antioxidant constituents of plant extracts were identified and quantified by HPLC on a C18 column using a modified mobile phase of gradient elution comprised of MeOH-0.2% o-phosphoric acid and UV detection for polyphenols at 280 nm. The TAC values of HPLC-quantified antioxidant constituents were found, and compared for the first time with those found by CUPRAC. The TAC of HPLC-quantified compounds accounted for a relatively high percentage of the observed CUPRAC capacities of plant extracts, namely 81% of nettle, 60-77% of parsley (in different hydrolyzates of extract and solid sample), and 41-57% of celery leaves (in different hydrolyzates). The CUPRAC total capacities of the 70% MeOH extracts of studied plants (in the units of mmol trolox g(-1)plant) were in the order: celery leaves>nettle>parsley. The TAC calculated with the aid of HPLC-spectrophotometry did not compensate for 100% of the CUPRAC total capacities, because all flavonoid glycosides subjected to hydrolysis were either not detectable with HPLC, or not converted to the corresponding aglycons (i.e., easily detectable and quantifiable with HPLC) during the hydrolysis step.

  13. 48 CFR 1019.202-70-8 - Protégé firms.

    Science.gov (United States)

    2010-10-01

    ... multiple mentors unless approved, in writing, by the Director, Office of Small Business Development (OSBD... SOCIOECONOMIC PROGRAMS SMALL BUSINESS PROGRAMS Policies 1019.202-70-8 Protégé firms. (a) For selection as a protégé, a firm must be: (1) A small business, women-owned small business, small disadvantaged business...

  14. Expermental Studies of quantitative evaluation using HPLC

    Directory of Open Access Journals (Sweden)

    Ki Rok Kwon

    2005-06-01

    Full Text Available Methods : This study was conducted to carry out quantitative evaluation using HPLC Content analysis was done using HPLC Results : According to HPLC analysis, each BVA-1 contained approximately 0.36㎍ melittin, and BVA-2 contained approximately 0.54㎍ melittin. But the volume of coating was so minute, slight difference exists between each needle. Conclusion : Above results indicate that the bee venom acupuncture can complement shortcomings of syringe usage as a part of Oriental medicine treatment, but extensive researches should be done for further verification.

  15. Neutronic Analysis of the RSG-GAS Compact Core without CIP Silicide 3.55 g U/cc and 4.8 g U/cc

    International Nuclear Information System (INIS)

    Jati S; Lily S; Tukiran S

    2004-01-01

    Fuel conversion from U 3 O 8 -Al to U 3 Si 2 -Al 2.96 g U/cc density in the RSG-GAS core had done successfully step by step since 36 th core until 44 th core. So that, since the 45 th core until now (48 th core) had been using full of silicide 2.96 g U/cc. Even though utilization program of silicide fuel with high density (3.55 g U/cc and 4.8 g U/cc) and optimize operation of RSG-GAS core under research. Optimalitation of core with increasing operation cycle have been analyzing about compact core. The mean of compact core is the RSG-GAS core with decrease number of IP or CIP position irradiation. In this research, the neutronic calculation to cover RSG-GAS core and RSG-GAS core without CIP that are using U 3 Si 2 -Al 2.96 g U/cc, 3.55 g U/cc and 4.8 g U/cc had done. Two core calculation done at 15 MW power using SRAC-ASMBURN code. The calculation result show that fuel conversion from 2.96 g U/cc density to 3.55 g U/cc and 4.8 g U/cc will increasing cycle length for both RSG-GAS core and RSG-GAS compact core without CIP. However, increasing of excess reactivity exceeded from nominal value of first design that 9.2%. Change of power peaking factor is not show significant value and still less than 1.4. Core fuelled with U 3 Si 2 -Al 4.8 g U/cc density have maximum discharge burn-up which exceeded from licensing value (70%). RSG-GAS compact core without CIP fuelled U 3 Si 2 -Al 2.96 g U/cc have longer cycle operation then RSG-GAS core and fulfil limitation neutronic parameter at the first design value. (author)

  16. [Determination method of polysorbates in powdered soup by HPLC].

    Science.gov (United States)

    Takeda, Y; Abe, Y; Ishiwata, H; Yamada, T

    2001-04-01

    A method for qualitative and quantitative analyses of polysorbates in powdered soup by HPLC was studied. Polysorbates in samples were extracted with acetonitrile after rinsing with n-hexane to remove fats and oils. The extract was cleaned up using a Bond Elut silica gel cartridge (500 mg). The cartridge was washed with ethyl acetate and polysorbates were eluted with a small amount of acetonitrile-methanol (1:2) mixture. The eluate was treated with cobalt thiocyanate solution to form a blue complex with polysorbate. In order to determine polysorbate, the complex was subjected to HPLC with a GPC column, using a mixture of acetonitrile-water (95:5) as a mobile phase, with a detection wavelength of 620 nm. The recoveries of polysorbate 80 added to powdered soups were more than 75% and the determination limit was 0.04 mg/g. When the proposed method was applied to the determination of polysorbates in 16 commercial samples of powdered soup for instant noodles and seasoning consomme, no polysorbates were detected in any sample.

  17. Sensitive measurement of positron emitters eluted from HPLC

    International Nuclear Information System (INIS)

    Takei, Makoto; Kida, Takayo; Suzuki, Kazutoshi

    2001-01-01

    For sensitive analysis of the radioactive-metabolite in human PET, a radio-HPLC system coupled to a newly designed positron detector was constructed. The detector had the advantages of low noise level (1.7±1.0 cpm) and high sensitivity (32±1%) due to coincidence counting and large BGO crystals. Furthermore, the detector was easy to move, since a pair of the BGO housings coupled to photomultipliers was effectively arranged in parallel and a HPLC cell with different volume could be inserted between the BGO housing. This radio-HPLC system was useful for analyzing samples with low radioactivity. It was applied to the measurement of [ 11 C]FLB457 in plasma, having high affinity and high selectivity with dopamine D2 receptors. Extremely low radioactivity of [ 11 C]FLB457 (2500 dpm) could be analyzed by using the radio-HPLC system. The performance of this detector was compared with those of commercially available systems that had been used as sensitive detectors for HPLC

  18. Further identification of endogenous gibberellins in the shoots of pea, line G2

    International Nuclear Information System (INIS)

    Halinska, A.; Davies, P.J.; Lee, J.W.; Zhu, Yuxian

    1989-01-01

    To interpret the metabolism of radiolabeled gibberellins A 12 -aldehyde and A 12 in shoots of pea (Pisum sativum L.), the identity of the radiolabeled peaks has to be determined and the endogenous presence of the gibberellins demonstrated. High specific activity [ 14 C]GA 12 and [ 14 C]GA 12 -aldehyde were synthesized using a pumpkin endosperm enzyme preparation, and purified by high performance liquid chromatography (HPLC). [ 14 C]GA 12 was supplied to upper shoots of pea, line G2, to produce radiolabeled metabolites on the 13-OH pathway. Endogenous compounds copurifying with the [ 14 C]GAs on HPLC were analyzed by gas chromatography-mass spectrometry. The endogenous presence of GA 53 , GA 44 , GA 19 and GA 20 was demonstrated and their HPLC peak identity ascertained. The 14 C was progressively diluted in GAs further down the pathway, proportional to the levels found in the tissue and inversely proportional to the speed of metabolism, ranging from 63% in GA 53 to 4% in GA 20 . Calculated levels of GA 20 , GA 19 , GA 44 , and GA 53 were 42, 8, 10, and 0.5 nanograms/gram, respectively

  19. Characterization of incompletely typed rotavirus strains from Guinea-Bissau: identification of G8 and G9 types and a high frequency of mixed infections

    International Nuclear Information System (INIS)

    Fischer, T.K.; Page, N.A.; Griffin, D.D.; Eugen-Olsen, J.; Pedersen, A.G.; Valentiner-Branth, P.; Moelbak, K.; Sommerfelt, H.; Nielsen, N. Munk

    2003-01-01

    Among 167 rotavirus specimens collected from young children in a suburban area of Bissau, Guinea-Bissau, from 1996 to 1998, most identifiable strains belonged to the uncommon P[6], G2 type and approximately 50% remained incompletely typed. In the present study, 76 such strains were further characterized. Due to interprimer interaction during the standard multiplex PCR approach, modifications of this procedure were implemented. The modified analyses revealed a high frequency of G2, G8, and G9 genotypes, often combined with P[4] and/or P[6]. The Guinean G8 and G9 strains were 97 and 98%, respectively, identical to other African G8 and G9 strains. Multiple G and/or P types were identified at a high frequency (59%), including two previously undescribed mixed infections, P[4]P[6], G2G8 and P[4]P[6], G2G9. These mixed infections most likely represent naturally occurring reassortance of rotavirus strains. Detection of such strains among the previously incompletely typed strains indicates a potential underestimation of mixed infections, if only a standard multiplex PCR procedure is followed. Furthermore cross-priming of the G3 primer with the G8 primer binding site and silent mutations at the P[4] and P[6] primer binding sites were detected. These findings highlight the need for regular evaluation of the multiplex primer PCR method and typing primers. The high frequency of uncommon as well as reassortant rotavirus strains in countries where rotavirus is an important cause of child mortality underscores the need for extensive strain surveillance as a basis to develop appropriate rotavirus vaccine candidates

  20. HPLC-ESR techniques for detection of complex trapped radicals

    International Nuclear Information System (INIS)

    Tu Tiecheng; Dong Jirong; Lin Nianyun; Xie Leidong; Liu Rengzhong

    1992-01-01

    High performance liquid chromatography (HPLC) and ESR combined examination of radical species is an advanced techniques for separation and identification of complex radical species. At SRCL, Waters 990 HPLC has been used to separate the complex trapped radicals and Varian E-112 ESR spectrometer to record the spectra of single trapped radicals after HPLC separation. The advantages of the combined techniques are described as bellow: HPLC is used to separate the long-lived complex trapped radicals derived from reaction of short-lived radicals with spin trap. ESR spectra from single trapped radicals, obtained following HPLC separation of complex trapped radicals, are recorded one by one and well resolved. The structures of short-lived radicals can be inferred from the ESR spectra of the long-lived trapped radicals

  1. Deletion and aberrant CpG island methylation of Caspase 8 gene in medulloblastoma.

    Science.gov (United States)

    Gonzalez-Gomez, Pilar; Bello, M Josefa; Inda, M Mar; Alonso, M Eva; Arjona, Dolores; Amiñoso, Cinthia; Lopez-Marin, Isabel; de Campos, Jose M; Sarasa, Jose L; Castresana, Javier S; Rey, Juan A

    2004-09-01

    Aberrant methylation of promoter CpG islands in human genes is an alternative genetic inactivation mechanism that contributes to the development of human tumors. Nevertheless, few studies have analyzed methylation in medulloblastomas. We determined the frequency of aberrant CpG island methylation for Caspase 8 (CASP8) in a group of 24 medulloblastomas arising in 8 adult and 16 pediatric patients. Complete methylation of CASP8 was found in 15 tumors (62%) and one case displayed hemimethylation. Three samples amplified neither of the two primer sets for methylated or unmethylated alleles, suggesting that genomic deletion occurred in the 5' flanking region of CASP8. Our findings suggest that methylation commonly contributes to CASP8 silencing in medulloblastomas and that homozygous deletion or severe sequence changes involving the promoter region may be another mechanism leading to CASP8 inactivation in this neoplasm.

  2. Application of the Instrumental Neutron Activation Analysis and High Performance Liquid Chromatography (HPLC) in the rare earth elements determination in reference geological materials

    International Nuclear Information System (INIS)

    Figueiredo, Ana M.G.; Moraes, Noemia M.P. de; Shihomatsu, Helena M.

    1997-01-01

    Instrumental Neutron Activation Analysis (INAA) and High Performance Liquid Chromatography (HPLC) were applied to the determination of rare earth elements (REE) in the geological reference materials AGV-1, G-2 and GSP-1 (USGS). Results obtained by both techniques showed good agreement with certified values, giving relative errors less than 10%. The La, Ce, Nd, Sm, Eu, Tb, Yb and Lu REE elements were determined. All the REE except Dy and Y were determined by HPLC. The reference material G94, employed in the International Proficiency Test for Analytical Geochemistry Laboratories (GeoTP1) was analysed. The results obtained are a contribution to REE contents in this sample. The INAA and HPLC application to the determination of REE in this kind of matrix is also discussed. (author). 10 refs., 1 fig., 5 tabs

  3. Chemical fingerprinting and quantitative analysis of a Panax notoginseng preparation using HPLC-UV and HPLC-MS

    Directory of Open Access Journals (Sweden)

    Shao Qing

    2011-02-01

    Full Text Available Abstract Background Xuesaitong (XST injection, consisting of total saponins from Panax notoginseng, was widely used for the treatment of cardio- and cerebro-vascular diseases in China. This study develops a simple and global quality evaluation method for the quality control of XST. Methods High performance liquid chromatography-ultraviolet detection (HPLC-UV was used to identify and quantify the chromatographic fingerprints of the XST injection. Characteristic common peaks were identified using HPLC with photo diode array detection/electrospray ionization tandem mass spectrometry (HPLC-PDA/ESI-MSn. Results Representative fingerprints from ten batches of samples showed 27 'common saponins' all of which were identified and quantified using ten reference saponins. Conclusion Chemical fingerprinting and quantitative analysis identified most of the common saponins for the quality control of P. notoginseng products such as the XST injection.

  4. HPLC residues of enrofloxacin and ciprofloxacin in eggs of laying hens.

    Science.gov (United States)

    Gorla, N; Chiostri, E; Ugnia, L; Weyers, A; Giacomelli, N; Davicino, R; García Ovando, H

    1997-05-01

    Eggs of 12 laying hens with 5 mg/kg/day oral administration of 5% enrofloxacin (EFX) or ciprofloxacin (CFX) solution during 5 days contained residues from 0.02 to 1.98 microg/g (EFX) or 0.14 to 0.28 microg/g (CFX). At identical dosage regime High Performance Liquid Chromatograhy (HPLC) residues of EFX were 6-fold greater than CFX ones. Maximun concentrations were detected at the second day after the administration withdrawal. The limits of detection were 0.019 microg/g for EFX and 0.156 microg/g for CFX. The recovery was 36-50% for CFX and 49-85% for EFX. The withdrawal treatment periods in hens are six days for EFX and five days for CFX in order to avoid violative levels of egg residues.

  5. [Bifunctional chelates of Rh-105, Au-199, and other metallic radionuclides as potential radiotherapeutic agents

    International Nuclear Information System (INIS)

    1991-01-01

    Progress during this period is reported under the following headings: Diethylenetriamine based and related bifunctional chelating agents and their complexation with Rh-105, Au-198, Pd-109, cu-67, In-111, and Co-57; studies of Pd-109, Rh-105 and Tc-99m with bifunctional chelates based on phenylenediamine; establishment of an appropriate protein assay method for conjugated proteins; studies of new bifunctional Bi, Tri and tetradentate amine oxime ligands with Rh-105; IgG and antibody B72.3 conjugation studies by HPLC Techniques with bifunctional metal chelates; and progress on ligand systems for Au(III)

  6. [Bifunctional chelates of Rh-105, Au-199, and other metallic radionuclides as potential radiotherapeutic agents

    Energy Technology Data Exchange (ETDEWEB)

    1991-12-31

    Progress during this period is reported under the following headings: Diethylenetriamine based and related bifunctional chelating agents and their complexation with Rh-105, Au-198, Pd-109, cu-67, In-111, and Co-57; studies of Pd-109, Rh-105 and Tc-99m with bifunctional chelates based on phenylenediamine; establishment of an appropriate protein assay method for conjugated proteins; studies of new bifunctional Bi, Tri and tetradentate amine oxime ligands with Rh-105; IgG and antibody B72.3 conjugation studies by HPLC Techniques with bifunctional metal chelates; and progress on ligand systems for Au(III).

  7. (Bifunctional chelates of Rh-105, Au-199, and other metallic radionuclides as potential radiotherapeutic agents)

    Energy Technology Data Exchange (ETDEWEB)

    1991-01-01

    Progress during this period is reported under the following headings: Diethylenetriamine based and related bifunctional chelating agents and their complexation with Rh-105, Au-198, Pd-109, cu-67, In-111, and Co-57; studies of Pd-109, Rh-105 and Tc-99m with bifunctional chelates based on phenylenediamine; establishment of an appropriate protein assay method for conjugated proteins; studies of new bifunctional Bi, Tri and tetradentate amine oxime ligands with Rh-105; IgG and antibody B72.3 conjugation studies by HPLC Techniques with bifunctional metal chelates; and progress on ligand systems for Au(III).

  8. Identification and quantification of bio-actives and metabolites in physiological matrices by automated HPLC-MS

    NARCIS (Netherlands)

    van Platerink, C.J.

    2010-01-01

    Identification and quantification of bio-actives and metabolites in physiological matrices by automated HPLC-MS > Food plays an important role in human health. Nowadays there is an increasing interest in the health effects of so-calles functional foods, e.g. effects on blood pressure, cholesterol

  9. Urinary 8-hydroxydeoxyguanosine and urothelial carcinoma risk in low arsenic exposure area

    International Nuclear Information System (INIS)

    Chung, C.-J.; Huang, C.-J.; Pu, Y.-S.; Su, C.-T.; Huang, Y.-K.; Chen, Y.-T.; Hsueh, Y.-M.

    2008-01-01

    Arsenic is a well-documented human carcinogen and is known to cause oxidative stress in cultured cells and animals. A hospital-based case-control study was conducted to evaluate the relationship among the levels of urinary 8-hydroxydeoxyguanosine (8-OHdG), the arsenic profile, and urothelial carcinoma (UC). Urinary 8-OHdG was measured by using high-sensitivity enzyme-linked immunosorbent assay (ELISA) kits. The urinary species of inorganic arsenic and their metabolites were analyzed by high-performance liquid chromatography (HPLC) and hydride generator-atomic absorption spectrometry (HG-AAS). This study showed that the mean urinary concentration of total arsenics was significantly higher, at 37.67 ± 2.98 μg/g creatinine, for UC patients than for healthy controls of 21.10 ± 0.79 μg/g creatinine (p < 0.01). Urinary 8-OHdG levels correlated with urinary total arsenic concentrations (r = 0.19, p < 0.01). There were significantly higher 8-OHdG levels, of 7.48 ± 0.97 ng/mg creatinine in UC patients, compared to healthy controls of 5.95 ± 0.21 ng/mg creatinine. Furthermore, female UC patients had higher 8-OHdG levels of 9.22 ± 0.75 than those of males at 5.76 ± 0.25 ng/mg creatinine (p < 0.01). Multiple linear regression analyses revealed that high urinary 8-OHdG levels were associated with increased total arsenic concentrations, inorganic arsenite, monomethylarsonic acid (MMA), and dimethylarsenate (DMA) as well as the primary methylation index (PMI) even after adjusting for age, gender, and UC status. The results suggest that oxidative DNA damage was associated with arsenic exposure, even at low urinary level of arsenic

  10. Inhibition of a NEDD8 Cascade Restores Restriction of HIV by APOBEC3G.

    Directory of Open Access Journals (Sweden)

    David J Stanley

    2012-12-01

    Full Text Available Cellular restriction factors help to defend humans against human immunodeficiency virus (HIV. HIV accessory proteins hijack at least three different Cullin-RING ubiquitin ligases, which must be activated by the small ubiquitin-like protein NEDD8, in order to counteract host cellular restriction factors. We found that conjugation of NEDD8 to Cullin-5 by the NEDD8-conjugating enzyme UBE2F is required for HIV Vif-mediated degradation of the host restriction factor APOBEC3G (A3G. Pharmacological inhibition of the NEDD8 E1 by MLN4924 or knockdown of either UBE2F or its RING-protein binding partner RBX2 bypasses the effect of Vif, restoring the restriction of HIV by A3G. NMR mapping and mutational analyses define specificity determinants of the UBE2F NEDD8 cascade. These studies demonstrate that disrupting host NEDD8 cascades presents a novel antiretroviral therapeutic approach enhancing the ability of the immune system to combat HIV.

  11. Establishment of inherent stability on piracetam by UPLC/HPLC and development of a validated stability-indicating method

    Directory of Open Access Journals (Sweden)

    Kapendra Sahu

    2017-02-01

    Full Text Available A novel comparative force degradation UPLC assay method was developed and validated for Piracetam and its degradation products. Piracetam was subjected to acid (5 M HCl, neutral (water and alkaline (0.5 M NaOH hydrolytic conditions at 80 °C, as well as to oxidative decomposition (H2O2 at room temperature. Photolytic studies were carried out by exposing this drug into sunlight (60,000–70,000 lux for 2 d. Additionally, the solid drug was subjected to 50 °C for 60 days in a hot air oven for thermal degradation. The UPLC chromatographic separation was performed on Acquity UPLC BEH C18 column (1.7 μm, 2.1 mm × 150 mm using isocratic mode (ACN:water, 25:75 v/v at a flow rate of 0.15 mL min−1 and HPLC chromatographic separation was achieved on phenomenex C18 using isocratic mode (ACN:10 mM ammonium acetate, pH 5.0, 20:80 v/v at a flow rate of 0.9 mL/min. Piracetam was found to degrade only in the base and shows stable behavior under all stress conditions. The UPLC and HPLC linearity of the proposed method was investigated in the range of 10–50 μg mL−1. The r2 value of UPLC and HPLC was found to be 0.999 and 0.999, respectively. Method detection limit (MDL and Method quantification limit (MQL were found to be 0.180 μg mL−1and 1.10 μg mL−1 for UPLC and 0.500 μg mL−1and 1.700 μg mL−1 for HPLC respectively. The %RSD values for intra-day and inter-day precision were <1.2%, confirming that the method was sufficiently precise. The validation studies were carried out fulfilling ICH requirements. The developed method was simple, fast, accurate and precise and hence could be applied for routine quality control analysis of Piracetam in solid dosage forms.

  12. [Determination of 10-HDA in honeybee body by HPLC].

    Science.gov (United States)

    Fan, H; He, C; Han, H

    1999-05-01

    In the present work we found that in the honeybee body there exists an unsaturated fatty acid, trans-10-hydroxy-2-decenoic acid (10-HDA), which was known only to be present in royal jelly. We established the analytical method of 10-HDA in honeybee body by HPLC and simplified the extraction method of 10-HDA. In the optimum conditions the linear range of detection was 10-1,000 ng, the correlation coefficient was 0.9998, the recovery was 96.5%-99.2% and the detectable limit was 0.53 microgram/g.

  13. OSBP-related protein 8 (ORP8) interacts with Homo sapiens sperm associated antigen 5 (SPAG5) and mediates oxysterol interference of HepG2 cell cycle

    International Nuclear Information System (INIS)

    Zhong, Wenbin; Zhou, You; Li, Jiwei; Mysore, Raghavendra; Luo, Wei; Li, Shiqian; Chang, Mau-Sun; Olkkonen, Vesa M.; Yan, Daoguang

    2014-01-01

    We earlier identified OSBP-related protein 8 (ORP8) as an endoplasmic reticulum/nuclear envelope oxysterol-binding protein implicated in cellular lipid homeostasis, migration, and organization of the microtubule cytoskeleton. Here, a yeast two-hybrid screen identified Homo sapiens sperm associated antigen 5 (SPAG5)/Astrin as interaction partner of ORP8. The putative interaction was further confirmed by pull-down and co-immunoprecipitation assays. ORP8 did not colocalize with kinetochore-associated SPAG5 in mitotic HepG2 or HuH7 cells, but overexpressed ORP8 was capable of recruiting SPAG5 onto endoplasmic reticulum membranes in interphase cells. In our experiments, 25-hydroxycholesterol (25OHC) retarded the HepG2 cell cycle, causing accumulation in G2/M phase; ORP8 overexpression resulted in the same phenotype. Importantly, ORP8 knock-down dramatically inhibited the oxysterol effect on HepG2 cell cycle, suggesting a mediating role of ORP8. Furthermore, knock-down of SPAG5 significantly reduced the effects of both ORP8 overexpression and 25OHC on the cell cycle, placing SPAG5 downstream of the two cell-cycle interfering factors. Taken together, the present results suggest that ORP8 may via SPAG5 mediate oxysterol interference of the HepG2 cell cycle. - Highlights: • The oxysterol-binding protein ORP8 was found to interact with the mitotic regulator SPAG5/Astrin. • Treatment of HepG2 cells with 25-hydroxycholesterol caused cell cycle retardation in G2/M. • ORP8 overexpression caused a similar G2/M accumulation, and ORP8 knock-down reversed the 25-hydroxycholesterol effect. • Reduction of cellular of SPAG5/Astrin reversed the cell cycle effects of both 25-hydroxycholesterol and ORP8 overexpression. • Our results suggest that ORP8 mediates via SPAG5/Astrin the oxysterol interference of HepG2 cell cycle

  14. OSBP-related protein 8 (ORP8) interacts with Homo sapiens sperm associated antigen 5 (SPAG5) and mediates oxysterol interference of HepG2 cell cycle

    Energy Technology Data Exchange (ETDEWEB)

    Zhong, Wenbin [Department of Biotechnology, Jinan University, Guangzhou 510632 (China); Zhou, You [Minerva Foundation Institute for Medical Research, Helsinki (Finland); Li, Jiwei [Department of Biotechnology, Jinan University, Guangzhou 510632 (China); Mysore, Raghavendra [Minerva Foundation Institute for Medical Research, Helsinki (Finland); Luo, Wei; Li, Shiqian [Department of Biotechnology, Jinan University, Guangzhou 510632 (China); Chang, Mau-Sun [Institute of Biochemical Sciences, National Taiwan University, No. 1, Taipei, Taiwan (China); Olkkonen, Vesa M. [Minerva Foundation Institute for Medical Research, Helsinki (Finland); Yan, Daoguang, E-mail: tydg@jnu.edu.cn [Department of Biotechnology, Jinan University, Guangzhou 510632 (China)

    2014-04-01

    We earlier identified OSBP-related protein 8 (ORP8) as an endoplasmic reticulum/nuclear envelope oxysterol-binding protein implicated in cellular lipid homeostasis, migration, and organization of the microtubule cytoskeleton. Here, a yeast two-hybrid screen identified Homo sapiens sperm associated antigen 5 (SPAG5)/Astrin as interaction partner of ORP8. The putative interaction was further confirmed by pull-down and co-immunoprecipitation assays. ORP8 did not colocalize with kinetochore-associated SPAG5 in mitotic HepG2 or HuH7 cells, but overexpressed ORP8 was capable of recruiting SPAG5 onto endoplasmic reticulum membranes in interphase cells. In our experiments, 25-hydroxycholesterol (25OHC) retarded the HepG2 cell cycle, causing accumulation in G2/M phase; ORP8 overexpression resulted in the same phenotype. Importantly, ORP8 knock-down dramatically inhibited the oxysterol effect on HepG2 cell cycle, suggesting a mediating role of ORP8. Furthermore, knock-down of SPAG5 significantly reduced the effects of both ORP8 overexpression and 25OHC on the cell cycle, placing SPAG5 downstream of the two cell-cycle interfering factors. Taken together, the present results suggest that ORP8 may via SPAG5 mediate oxysterol interference of the HepG2 cell cycle. - Highlights: • The oxysterol-binding protein ORP8 was found to interact with the mitotic regulator SPAG5/Astrin. • Treatment of HepG2 cells with 25-hydroxycholesterol caused cell cycle retardation in G2/M. • ORP8 overexpression caused a similar G2/M accumulation, and ORP8 knock-down reversed the 25-hydroxycholesterol effect. • Reduction of cellular of SPAG5/Astrin reversed the cell cycle effects of both 25-hydroxycholesterol and ORP8 overexpression. • Our results suggest that ORP8 mediates via SPAG5/Astrin the oxysterol interference of HepG2 cell cycle.

  15. The G8 global partnership - a survey of the German activities and their legal framework

    International Nuclear Information System (INIS)

    Fillbrandt, M.

    2006-01-01

    At the G8 summit in Kananaskis, Canada, in 2002, the G8 partners established the 'Global Partnership against the Proliferation of Weapons and Materials of Mass Destruction'. The Federal Republic of Germany and the Russian Federation at present cooperate in three areas within the framework of the G8 Global Partnership: (1) Destruction of chemical weapons. (2) Construction of a long-term interim store for the safe storage of irradiated reactor segments of decommissioned nuclear submarines. (3) Modernization of the physical protection of Russian nuclear material. The article mainly covers the 'Modernization of the Physical Protection of Russian Nuclear Material' project. The key part contains an explanation of the legal basis of the project. The main contents and functions of applicable bilateral and multilateral agreements are explained on the basis of the principles and guidelines adopted in connection with the declaration of the G8 Heads of State and Government about global partnership. It is shown that a complex set of rules and contracts are necessary to meet the requirements posed by projects of G8 Global Partnership. (orig.)

  16. A simple micro-batch ion-exchange resin extraction method coupled with reverse-phase HPLC (MBRE-HPLC) to quantify lactoferrin in raw and heat-treated bovine milk.

    Science.gov (United States)

    Pochet, Sylvie; Arnould, Céline; Debournoux, Perrine; Flament, Jocelyne; Rolet-Répécaud, Odile; Beuvier, Eric

    2018-09-01

    Lactoferrin is an iron-binding cationic glycoprotein (pI = 8.7) beneficial for mammal health, especially udder and milk preservation. A new simple two-step method of quantification was developed. Lactoferrin in 1 mL of bovine skim milk was first adsorbed onto 100 mg of macroporous sulfonated-resin at pH 6.8 by rotary stirring for 90 min at 20-25 °C. After washing the resin, lactoferrin was desorbed using 1 mL of 2 M NaCl containing phenylalanine as a dilution marker, then fully resolved and quantified by RP-HPLC at 220 nm using a wide-bore C4 silica column. This robust, inexpensive and flexible method improves selectivity (no protein interference) and sensitivity compared to previous HPLC methods. In-laboratory validation demonstrated its linearity (25 to 514 µg Lf mL -1 ), accuracy (110 to 98% recovery), and precision (<4%), which were comparable to immuno-based methods. The results for individual raw cow's milk were strongly correlated with results using an ELISA test. Copyright © 2018 Elsevier Ltd. All rights reserved.

  17. [IgG4-related lung disease: analysis of 8 cases and literature review].

    Science.gov (United States)

    Han, G J; Hu, H; Mao, D; Bai, X; She, D Y; Zhao, S F; Wen, Z L; Gao, J

    2017-03-12

    Objective: To improve the understanding and treatment of IgG4-related lung disease (IgG4-RLD). Methods: The clinical characteristics, serum IgG4 levels, pathological features, chest CT, therapy and prognosis of 8 patients with IgG4-RLD were retrospectively analyzed. These patients were admitted to the People's Liberation Army General Hospital and the pathological diagnosis was made between December 2005 and March 2016. Relevant literatures were reviewed. Results: The 8 patients with IgG4-RLD included 4 men and 4 women, with an average age of (59±4) years (range, 37-74). The respiratory symptoms included shortness of breath, cough, and expectoration. Extra-pulmonary symptoms included abdominal pain, facial edema, and fever. Extrapulmonary organs were involved in 7 cases. Serum IgG4 levels were elevated in 8 cases, with an average concentration of(17±6)g/L. Chest CT showed solid lung nodules in 6, alveolar-interstitial infiltration in 5, bronchovascular lesions in 3 and ground glass shadows in 2 cases. PET/CT was performed in 2 cases and it showed multiple organ involvement with higher radioactivity uptake(SUVmax2.9-4.2). The pathological examination found lymphocyte and plasma cell infiltration in 7, fibrous tissue hyperplasia in 5, and occlusive vasculitis in 2 cases. On immunohistochemical staining, the ratio of IgG4-positive plasma cells to IgG-positive plasma cells was higher than 40%in 3 cases. The number of IgG4-positive plasma cells was 10-50/HP in 8 cases. The misdiagnosis rate was 100% before the final diagnosis was made. Three cases received glucocorticoids with immunosuppressant therapy, 2 received surgery combined with glucocorticoid therapy, 2 received glucocorticoid therapy alone, and 1 only received surgery. The follow-up time was 4-132 months, with remission in 7 cases, and disease progression in 1 case, but no death. A total of 195 cases of IgG4-RLD were reviewed from the literature, among whom 111 cases were admitted with respiratory symptoms

  18. Methods and applications of HPLC-AMS

    International Nuclear Information System (INIS)

    Buchholz, Bruce A.; Dueker, Stephen R.; Lin, Yumei; Clifford, Andrew J.; Vogel, John S.

    2000-01-01

    Pharmacokinetics of physiologic doses of nutrients, pesticides, and herbicides can easily be traced in humans using a 14 C-labeled compound. Basic kinetics can be monitored in blood or urine by measuring the elevation in the 14 C content above the control predose tissue and converting to equivalents of the parent compound. High performance liquid chromatography (HPLC) is an excellent method for the chemical separation of complex mixtures whose profiles afford estimation of biochemical pathways of metabolism. Compounds elute from the HPLC systems with characteristic retention times and can be collected in fractions that can then be graphitized for AMS measurement. Unknowns are tentatively identified by co-elution with known standards and chemical tests that reveal functional groupings. Metabolites are quantified with the 14 C signal. Thoroughly accounting for the carbon inventory in the LC solvents, ion-pairing agents, samples, and carriers adds some complexity to the analysis. In most cases the total carbon inventory is dominated by carrier. Baseline background and stability need to be carefully monitored. Limits of quantitation near 10 amol of 14 C per HPLC fraction are typically achieved. Baselines are maintained by limiting injected 14 C activity <0.17 Bq (4.5 pCi) on the HPLC column

  19. [Determination of equilibrium solubility and n-octanol/water partition coefficient of pulchinenosiden D by HPLC].

    Science.gov (United States)

    Rao, Xiao-Yong; Yin, Shan; Zhang, Guo-Song; Luo, Xiao-Jian; Jian, Hui; Feng, Yu-Lin; Yang, Shi-Lin

    2014-05-01

    To determine the equilibrium solubility of pulchinenosiden D in different solvents and its n-octanol/water partition coefficients. Combining shaking flask method and high performance liquid chromatography (HPLC) to detect the n-octanol/water partition coefficients of pulchinenosiden D, the equilibrium solubility of pulchinenosiden D in six organic solvents and different pH buffer solution were determined by HPLC analysis. n-Octanol/water partition coefficients of pulchinenosiden D in different pH were greater than zero, the equilibrium solubility of pulchinenosiden D was increased with increase the pH of the buffer solution. The maximum equilibrium solubility of pulchinenosiden D was 255.89 g x L(-1) in methanol, and minimum equilibrium solubility of pulchinenosiden D was 0.20 g x L(-1) in acetonitrile. Under gastrointestinal physiological conditions, pulchinenosiden D exists in molecular state and it has good absorption but poor water-solubility, so increasing the dissolution rate of pulchinenosiden D may enhance its bioavailability.

  20. Nitrofurans residue in broiler chicken meat which analysed by an HPLC

    Directory of Open Access Journals (Sweden)

    Raphaella Widiastuti

    2012-12-01

    Full Text Available Furazolidone (FZD, furaltadone (FTD, nitrofurantoin (NFT and nitrofurazone (NFZ are veterinary drugs that belong to the nitrofurans (NFs group and employed as feed additives for growth promotion and theurapetic treatment of gastrointestinal infections caused by Eschericia coli and Salmonella spp. The occurrence of NFs in animal products will end to cause health problem in human consumed such food. This research conducted to study the analysis of NF residues in chicken meat by a high performance liquid chromatography (HPLC and to study the occurrence of NFs residues in samples collected from traditional markets and supermarkets in Bandung, Bogor and Depok. The results of validation method on several parameters for each NF showed that the average of the relative standard deviation (RSD from the precision study were 2.15 to 2.38%, the R2 values of the linearity study were 0.9964 to 0.9995; recoveries were 75.90 % to 91.50 % and the detection limits were 12.01 to 37.25 ng/g. The residual level of NFs for 42 field samples showed that 2 samples positive for NFZ (9.09 and 10.74 ng/g, 1 positive for NFT (10.46 ng/g, 4 positive for FTD (16.44 up to 27.21 ng/g and none positive for FZD. Present results showed that analysis of NFs in broiler chicken meat can be done using an HPLC and the analysis results from field samples showed that these types of drugs were being used for broiler chicken production both as single and/or combination drugs, therefore it is necessary to raise public awareness to monitor the use of NF in livestock production in Indonesia.

  1. The effect of smoking on the urinary excretion of 8-oxodG and 8-oxoGuo in patients with type 2 diabetes

    DEFF Research Database (Denmark)

    Sørensen, Anne-Sofie; Kjær, Laura Kofoed; Petersen, Kasper Meidahl

    2017-01-01

    as urinary 8-oxo-7, 8-dihydro-2'-deoxyguanosine (8-oxodG) excretion in smokers compared with non-smokers in a healthy population. We aimed to investigate if an increased urinary excretion of 8-oxodG in smokers versus never smokers and former smokers could be verified in a population with type 2 diabetes......Over the past decades, attention has been paid to understanding the impact of oxidative stress and related modifications of DNA and RNA on various human health risks. A recent meta-analysis comprising 1915 smokers and 3462 non-smokers found a significantly higher level of DNA oxidation measured...... to examine the relationship between daily smokers (n = 462) versus former (n = 1341) and never smokers (n = 918) regarding the RNA and DNA oxidation, respectively. We did not find any significant effect of smoking on urinary excretion of 8-oxodG or 8-oxoGuo in our study. Due to a sparse study area...

  2. Discrimination of Black Ball-point Pen Inks by High Performance Liquid Chromatography (HPLC)

    International Nuclear Information System (INIS)

    Mohamed Izzharif Abdul Halim; Norashikin Saim; Rozita Osman; Halila Jasmani; Nurul Nadhirah Zainal Abidin

    2013-01-01

    In this study, thirteen types of black ball-point pen inks of three major brands were analyzed using high performance liquid chromatography (HPLC). Separation of the ink components was achieved using Bondapak C-18 column with gradient elution using water, ethanol and ethyl acetate. The chromatographic data obtained at wavelength 254.8 nm was analyzed using agglomerative hierarchical clustering (AHC) and principle component analysis (PCA). AHC was able to group the inks into three clusters. This result was supported by PCA, whereby distinct separation of the three different brands was achieved. Therefore, HPLC in combination with chemometric methods may be a valuable tool for the analysis of black ball-point pen inks for forensic purposes. (author)

  3. An Efficient Method for the Preparative Isolation and Purification of Flavonoid Glycosides and Caffeoylquinic Acid Derivatives from Leaves of Lonicera japonica Thunb. Using High Speed Counter-Current Chromatography (HSCCC) and Prep-HPLC Guided by DPPH-HPLC Experiments.

    Science.gov (United States)

    Wang, Daijie; Du, Ning; Wen, Lei; Zhu, Heng; Liu, Feng; Wang, Xiao; Du, Jinhua; Li, Shengbo

    2017-02-02

    In this work, the n-butanol extract from leaves of Lonicera japonica Thunb. (L. japonica) was reacted with DPPH and subjected to a HPLC analysis for the guided screening antioxidants (DPPH-HPLC experiments). Then, nine antioxidants, including flavonoid glycosides and caffeoylquinic acid derivatives, were isolated and purified from leaves of L. japonica using high speed counter-current chromatography (HSCCC) and prep-HPLC. The n-butanol extract was firstly isolated by HSCCC using methyl tert-butyl ether/n-butanol/acetonitrile/water (0.5% acetic acid) (2:2:1:5, v/v), yielding five fractions F1, F2 (rhoifolin), F3 (luteoloside), F4 and F5 (collected from the column after the separation). The sub-fractions F1, F4 and F5 were successfully separated by prep-HPLC. Finally, nine compounds, including chlorogenic acid (1), lonicerin (2), rutin (3), rhoifolin (4), luteoloside (5), 3,4-Odicaffeoylquinic acid (6), hyperoside (7), 3,5-O-dicaffeoylquinic acid (8), and 4,5-O-dicaffeoylquinic acid (9) were obtained, respectively, with the purities over 94% as determined by HPLC. The structures were identified by electrospray ionization mass spectrometry (ESI-MS), 1H- and 13C-NMR. Antioxidant activities were tested, and the isolated compounds showed strong antioxidant activities.

  4. Rapid Screening for α-Glucosidase Inhibitors from Gymnema sylvestre by Affinity Ultrafiltration–HPLC-MS

    Directory of Open Access Journals (Sweden)

    Mingquan Guo

    2017-04-01

    Full Text Available Gymnema sylvestre R. Br. (Asclepiadaceae has been known to posses potential anti-diabetic activity, and the gymnemic acids were reported as the main bioactive components in this plant species. However, the specific components responsible for the hypoglycemic effect still remain unknown. In the present study, the in vitro study revealed that the extract of G. sylvestre exhibited significant inhibitory activity against α-glucosidase with IC50 at 68.70 ± 1.22 μg/mL compared to acarbose (positive control at 59.03 ± 2.30 μg/mL, which further indicated the potential anti-diabetic activity. To this end, a method based on affinity ultrafiltration coupled with liquid chromatography mass spectrometry (UF-HPLC-MS was established to rapidly screen and identify the α-glucosidase inhibitors from G. sylvestre. In this way, 9 compounds with higher enrichment factors (EFs were identified according to their MS/MS spectra. Finally, the structure-activity relationships revealed that glycosylation could decrease the potential antisweet activity of sapogenins, and other components except gymnemic acids in G. sylvestre could also be good α-glucosidase inhibitors due to their synergistic effects. Taken together, the proposed method combing α-glucosidase and UF-HPLC-MS presents high efficiency for rapidly screening and identifying potential inhibitors of α-glucosidase from complex natural products, and could be further explored as a valuable high-throughput screening (HTS platform in the early anti-diabetic drug discovery stage.

  5. Fatal Indifference: The G8, Africa, and Global Health | IDRC ...

    International Development Research Centre (IDRC) Digital Library (Canada)

    Book cover Fatal Indifference: The G8, Africa, and Global Health ... It is also the most powerful political force behind the multilateral institutions that are shaping global economic practice ... IDRC joins more than 800 international delegates at the Resilient Cities ... Asian outlook: New growth dependent on new productivity.

  6. Modernizing the G8 Summit Process | CRDI - Centre de recherches ...

    International Development Research Centre (IDRC) Digital Library (Canada)

    Modernizing the G8 Summit Process. This project is based on the premise that emerging countries must be full participants in key agenda-setting bodies if international governance mechanisms are to be realistic and relevant. The project brings together leaders, senior advisors, experts, researchers and opinion leaders to ...

  7. Analysis of alcohol dehydrogenase inhibitors from Desmodium styracifolium using centrifugal ultrafiltration coupled with HPLC-MS

    Directory of Open Access Journals (Sweden)

    Liu Liangliang

    2015-01-01

    Full Text Available Alcohol dehydrogenase (ADH inhibitors play an important role in the treatment of human methanol or ethylene glycol poisoning and the suppression of acetaldehyde accumulation in alcoholics. In this study, centrifugal ultrafiltration coupled with high performance liquid chromatography-mass spectrometry (HPLC-MS was utilized to screen and identify ADH inhibitors from ethyl acetate extract of Desmosium styracifolium (Osb. Merr. The experiment conditions of centrifugal ultrafiltration were optimized. At the optimum conditions (ADH concentration: 37.5 μg mL-1, incubation time: 90 min, pH: 7.0 and temperature: 15°C, formononetin and aromadendrin were successfully screened and identified from ethyl acetate extract of Desmodium styracifolium. The screening result was verified by ADH inhibition assays. The IC50 values of formononetin and aromadendrin were 70.8 and 84.7 μg mL-1, which were accorded with the binding degrees of them. Aromadendrin was first reported to have inhibitory activity on ADH. This method provided an effective way to screen active compounds from natural products.

  8. Analysis of Naturally Occurring Phenolic Compounds in Aromatic Plants by RP-HPLC Coupled to Diode Array Detector (DAD and GC-MS after Silylation

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    Charalampos Proestos

    2013-03-01

    Full Text Available The following aromatic plants of Greek origin, Origanum dictamnus (dictamus, Eucalyptus globulus (eucalyptus, Origanum vulgare L. (oregano, Mellisa officinalis L. (balm mint and Sideritis cretica (mountain tea, were examined for the content of phenolic substances. Reversed phase HPLC coupled to diode array detector (DAD was used for the analysis of the plant extracts. The gas chromatography-mass spectrometry method (GC-MS was also used for identification of phenolic compounds after silylation. The most abundant phenolic acids were: gallic acid (1.5–2.6 mg/100 g dry sample, ferulic acid (0.34–6.9 mg/100 g dry sample and caffeic acid (1.0–13.8 mg/100 g dry sample. (+-Catechin and (−-epicatechin were the main flavonoids identified in oregano and mountain tea. Quercetin was detected only in eucalyptus and mountain tea.

  9. Simultaneous HPLC determination of caffeine, theobromine, and theophylline in food, drinks, and herbal products.

    Science.gov (United States)

    Srdjenovic, Branislava; Djordjevic-Milic, Vukosava; Grujic, Nevena; Injac, Rade; Lepojevic, Zika

    2008-02-01

    A rapid and selective high-performance liquid chromatographic (HPLC) method is developed for the separation and determination of caffeine, theobromine, and theophylline. The chromatography is performed on a Zorbax Eclipse XDB-C8 column (4.6x150 mm i.d., 5-microm particle size) at 25 degrees C, with a mobile phase of water-THF (0.1% THF in water, pH 8)-acetonitrile (90:10, v/v). The flow rate is 0.8 mL/min, and detection is by UV at 273 nm. This method permits the simultaneous determination of caffeine, theobromine, and theophylline in food, drinks, and herbal products with detection limits of 0.07-0.2 mg/L and recoveries of 100.20-100.42%. Correlation coefficients, for the calibration curves in the linear range of 0.2-100 mg/L, are greater than 0.9999 for all compounds. The within- and between-day precision is determined for both retention times and peak area. The data suggests that the proposed HPLC method can be used for routine quality control of food, drinks, and herbal products.

  10. Simultaneous analysis of 17 diuretics in dietary supplements by HPLC and LC-MS/MS.

    Science.gov (United States)

    Woo, H; Kim, J W; Han, K M; Lee, J H; Hwang, I S; Lee, J H; Kim, J; Kweon, S J; Cho, S; Chae, K R; Han, S Y; Kim, J

    2013-01-01

    In order to test health foods for illegally added diuretics for weight loss, we developed simple, rapid, selective, and sensitive methods using HPLC and LC-MS/MS for the simultaneous analysis of 17 diuretics in dietary supplements. HPLC conditions were set with a Capcell-pak C18, using a mobile phase consisting of gradient conditions, UV detection at 254 nm and validated for linearity (r(2)> 0.999), precision (CV ≤ 3%), recoveries (90.4-102.8%) and reproducibility. Identification and quantification of 17 diuretics were accomplished by ion-spray LC-MS/MS using multiple reaction monitoring (MRM). The chromatographic separation was carried out under the reversed-phase mechanism on an HSS-T3 column. The LC-MS/MS method was validated for linearity (r(2)> 0.99) and precision (CV Diuretics were not detected in all samples. Extraction recovery was also investigated and the extraction recoveries in different formulations were from 88% to 110% and from 81% to 116% using HPLC and LC-MS/MS, respectively. There was no significant difference in recoveries in the type of dietary supplements. Based on this result, the developed methods to monitor illegal drug adulterations in dietary supplements using HPLC and LC-MS/MS are simple, fast and reliable. Therefore, it is applicable to routine drug-adulteration screening.

  11. Chemical profiling of anti-hepatocellular carcinoma constituents from Caragana tangutica Maxim. by off-line semi-preparative HPLC-NMR.

    Science.gov (United States)

    Yang, Xinzhou; Huang, Mi; Cai, Jinyan; Lv, Dan; Lv, Jingnan; Zheng, Sijian; Ma, Xinhua; Zhao, Ping; Wang, Qiang

    2017-05-01

    An EtOAc fraction from the roots of Caragana tangutica Maxim. (CTEA) displayed promising anti-hepatocellular carcinoma (HCC) activity during screening of a traditional Chinese ethnic herb library against HepG2 and Hep3B cell lines. HPLC-based activity profiling of CTEA by combination of MS-guided large-scale semi-preparative HPLC and NMR methods led to the identification of a new pterocarpan glycoside, (-)-maackiain 3-O-6'-O-methyl malonyl-β-d-glucopyranoside (1), together with three known pterocarpan glycosides, (-)-maackiain 3-O-β-d-glucopyranoside (2), 3-O-6'-O-acrylyl-β-d-galactopyranoside (3), and (-)-maackiain 3-O-6'-O-acetyl-β-d-glucopyranoside (4). Compound 1 was isolated during a drug discovery programme aimed at identifying new anti-HCC leads from a natural product library. Anti-HCC study showed that all four compounds exhibited cytotoxic activity with IC 50 values range of 29.1-53.5 μg/mL against HepG2 and Hep3B cell lines.

  12. Quality Control of Selected Pesticides with HPLC

    Energy Technology Data Exchange (ETDEWEB)

    Karasali, H. [Benaki Phytopathological Institute Laboratory of Physical and Chemical Analysis of Pesticides, Ekalis (Greece)

    2009-07-15

    Laboratory data obtained on two different HPLC separation columns and detection by UV and DAD under repeatability conditions are presented and discussed. The behaviour of pesticides on different HPLC columns under gradient and isocratic conditions is evaluated concerning the applicability of respective methodologies. Representative chromatograms of real formulations and “empty” formlants are given for illustration. (author)

  13. A simple reversed phase high-performance liquid chromatography (RP-HPLC method for determination of curcumin in aqueous humor of rabbit

    Directory of Open Access Journals (Sweden)

    Akhilesh Mishra

    2014-01-01

    Full Text Available This article describes a simple and rapid method for determination of curcumin (diferuloylmethane in aqueous humor of rabbit using high-performance liquid chromatography (HPLC. Analysis was performed using a C-18 column (250 × 4.6 mm, 5 μ luna by isocratic elution with a mobile phase containing 25 mM potassium dihydrogen orthophosphate (pH 3.5: Acetonitrile (40:60 and detection at 424 nm using a photodiode array (PDA detector for curcumin. The regression data for curcumin showed a good linear relationship with r 2 > 0.998 over the concentration range of 0.1-10 μg ml−1 . Relative standard deviations (RSD for the intraday and interday coefficient of variations for the assay were less than 5.0 and 8.5, respectively. The recovery of the method was between 79.8-83.6%. The quantification limit of the method for curcumin was 0.01 μg ml−1 . This method has good accuracy, precision, and quantitation limit. It is also concluded that the method is useful for measuring very low curcumin concentrations in aqueous humor.

  14. Distinct energetics and closing pathways for DNA polymerase β with 8-oxoG template and different incoming nucleotides

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    Wang Yanli

    2007-02-01

    Full Text Available Abstract Background 8-Oxoguanine (8-oxoG is a common oxidative lesion frequently encountered by DNA polymerases such as the repair enzyme DNA polymerase β (pol β. To interpret in atomic and energetic detail how pol β processes 8-oxoG, we apply transition path sampling to delineate closing pathways of pol β 8-oxoG complexes with dCTP and dATP incoming nucleotides and compare the results to those of the nonlesioned G:dCTP and G:dATPanalogues. Results Our analyses show that the closing pathways of the 8-oxoG complexes are different from one another and from the nonlesioned analogues in terms of the individual transition states along each pathway, associated energies, and the stability of each pathway's closed state relative to the corresponding open state. In particular, the closed-to-open state stability difference in each system establishes a hierarchy of stability (from high to low as G:C > 8-oxoG:C > 8-oxoG:A > G:A, corresponding to -3, -2, 2, 9 kBT, respectively. This hierarchy of closed state stability parallels the experimentally observed processing efficiencies for the four pairs. Network models based on the calculated rate constants in each pathway indicate that the closed species are more populated than the open species for 8-oxoG:dCTP, whereas the opposite is true for 8-oxoG:dATP. Conclusion These results suggest that the lower insertion efficiency (larger Km for dATP compared to dCTP opposite 8-oxoG is caused by a less stable closed-form of pol β, destabilized by unfavorable interactions between Tyr271 and the mispair. This stability of the closed vs. open form can also explain the higher insertion efficiency for 8-oxoG:dATP compared to the nonlesioned G:dATP pair, which also has a higher overall conformational barrier. Our study offers atomic details of the complexes at different states, in addition to helping interpret the different insertion efficiencies of dATP and dCTP opposite 8-oxoG and G.

  15. A rapid and reliable determination of doxycycline hyclate by HPLC with UV detection in pharmaceutical samples

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    SNEZANA S. MITIC

    2008-06-01

    Full Text Available An accurate, sensitive and reproducible high performance liquid chromatographic (HPLC method for the quantification of doxycycline hyclate in pharmaceutical samples has been developed and validated. The drug and the standard were eluted from a Lichrosorb RP-8 (250 mm´4.6 mm, 10 mm particle size at 20 °C with a mobile phase consisting of methanol, acetonitrile and 0.010 M aqueous solution of oxalic acid (2:3:5, v/v/v. The flow rate was 1.25 ml min-1. A UV detector set at 350 nm was used to monitor the effluent. Each analysis required no longer than 4 min. The limits of detection and quantification were 1.15 and 3.84 μg ml-1, respectively. Recoveries for different concentrations ranged from 99.58 to 101.93 %.

  16. Chemical characterization of neonicotinoids in surface waters by high performance liquid chromatography with Tandem Mass Spectrometry (HPLC MS/MS); Caracterização química dos neonicotinóides em águas superficiais via cromatografia liquída de alta eficiência acoplada a Espectrometria de Massas em Tandem (HPLC-MS/MS)

    Energy Technology Data Exchange (ETDEWEB)

    Amaral, Priscila Oliveira

    2017-07-01

    The present study aimed to develop a method for the determination and validation of a method for the identification and quantification of Neonicotinoids in surface waters collected in the Bauru region, in the state of São Paulo. The analytical techniques studied for the development of this method were the high performance liquid chromatography with tandem mass spectrometry (HPLC - MS / MS), gas chromatography with mass spectrometry (GC / MS) and gas chromatography with electron capture detector (GC / ECD). The class of pesticides Neonicotinoids was chosen for this work because it is related to a sudden disappearance of bees in colonies around the world. This phenomenon is known as Colony Collapse Disorder (CCD) and it is characterized by a rapid loss in the population of adult bees. The Neonicotinoids used in this study were the compounds Clothianidin, Imidacloprid and Thiamethoxam which were banned in their use as pesticides in Europe by Implementing Regulation No. 540/2011. The samples were concentrated using solid phase extraction (SPE) and liquid liquid extraction (LLE) techniques and injected into HPLC-MS / MS, GC / MS and GC / ECD. The GC / ECD and GC / MS techniques were not satisfactory for determination in the water matrix because the detection limit (10 mg L{sup -1}) is above the maximum allowed by the US Environmental Protection Agency (0.6 μg L{sup -1}). The HPLC - MS / MS technique using the multiple reaction monitoring (MRM) proved to be adequate for this study because it obtained quantification limits between 5.89 and 8.06 μg L{sup -1} and a linearity between 0.9963 and 0.9999 for the three compounds. (author)

  17. HPLC Separation of Sulforaphane Enantiomers in Broccoli and Its Sprouts by Transformation into Diastereoisomers Using Derivatization with (S)-Leucine.

    Science.gov (United States)

    Okada, Makiko; Yamamoto, Atsushi; Aizawa, Sen-Ichi; Taga, Atsushi; Terashima, Hiroyuki; Kodama, Shuji

    2017-01-11

    Racemic sulforaphane, which was derivatized with (S)-leucine (l-leucine), was resolved by reversed phase HPLC with UV detection. The optimum mobile phase conditions were found to be 10 mM citric acid (pH 2.8) containing 22% methanol at 35 °C using detection at 254 nm. Sulforaphane enantiomers in florets and stems of five brands of broccoli and leaves and stems of three brands of broccoli sprouts were analyzed by the proposed HPLC method. Both sulforaphane enantiomers were detected in all of the samples. The S/R ratios of sulforaphane in broccoli samples were 1.5-2.6/97.4-98.5% for florets and 5.0-12.1/87.9-95.0% for stems. The S/R ratios in broccoli sprout samples were higher than those in broccoli samples and were found to be 8.3-19.7/80.3-91.7% for leaves and 37.0-41.8/58.2-63.0% for stems. (S)-Sulforaphane detected in the broccoli and its sprout samples was positively identified by separately using an HPLC with a chiral column (Chiralpak AD-RH) and mass spectrometry.

  18. [Studies on HPLC-FPS of the saponins from Semen Ziziphi Spinosae].

    Science.gov (United States)

    Wu, He-zhen; Chen, Jing; Liu, Yan-wen

    2006-09-01

    To establish a method of HPLC-fingerprint spectrum (HPLC-FPS) for the active part in Semen Ziziphi Spinosae (SZS) in order to control the quality of SZS from different places. The gradient elution mode was applied in chromatographic separation, and data were analysed by" Similarity Evaluation software" to compare the HPLC-FPS of SZS from different places. The conditions for HPLC analysis of SZS were established and the FPS of samples from different habitats showed some differences. All components in the spectrum were separated well and the HPLC fingerprint method is repeatable. The method can be used in quality assessment of SZS.

  19. Development of the BG-Malaria trap as an alternative to human-landing catches for the capture of Anopheles darlingi

    Directory of Open Access Journals (Sweden)

    Renata Antonaci Gama

    2013-09-01

    Full Text Available Although the human-landing catch (HLC method is the most effective for collecting anthropophilic anophelines, it has been increasingly abandoned, primarily for ethical considerations. The objective of the present study was to develop a new trap for the collection of Anopheles darlingi . The initial trials were conducted using the BG-Sentinel trap as a standard for further trap development based on colour, airflow direction and illumination. The performance of the trap was then compared with those of the CDC, Fay-Prince, counterflow geometry trap (CFG and HLC. All trials were conducted outdoors between 06:00 pm-08:00 pm. Female specimens of An. darlingi were dissected to determine their parity. A total of 8,334 anophelines were captured, of which 4,945 were identified as An. darlingi . The best trap configuration was an all-white version, with an upward airflow and no required light source. This configuration was subsequently named BG-Malaria (BGM. The BGM captured significantly more anophelines than any of the other traps tested and was similar to HLC with respect to the number and parity of anophelines. The BGM trap can be used as an alternative to HLC for collecting anophelines.

  20. Simultaneous detection of water-soluble vitamins using the High Performance Liquid Chromatography (HPLC - a review

    Directory of Open Access Journals (Sweden)

    Rosemond Godbless Dadzie

    2014-01-01

    Full Text Available The water-soluble vitamins (WSV: ascorbic acid (vitamin C, thiamine (B1, riboflavin (B2, niacin (B3, panthothenic acid (B5, pyridoxine, and pyridoxal (B6, folic acid (B9, biotin(B8 , and B12 are very essential in the diet of humankind. As a result of ever increasing pressures from both consumers and legal enforcers, to specify accurately nutritive compositions of WSV that are present in food materials, many researchers have attempted to fill this niche through the provision of highly sensitive and rapid high performance liquid chromatography (HPLC procedures. In view of the health benefits of WSV, a replete of HPLC methods have been developed for simultaneous determination of their contents in nature and fortified food samples, nutritional supplements, as well as blood plasmas. The rate of losses of these vitamins during food processing and analysis, in addition to their transient dynamics, presents complexities in developing a highly sensitive HPLC procedure for their simultaneous separations and assays. This review critically assesses the different HPLC procedures developed by researchers and available in the open literature for simultaneous determination of water-soluble vitamins (WSV in dried tropical fruits materials. The study revealed that not a single chromatographic run developed by researchers can simultaneously elute all the WSV at a time. However, the HPLC procedures that are capable of determining all the WSV were coupled with electrospray ionization mass spectroscopy (ESI-MS, thus making the set-up expensive.

  1. Validation of an HPLC-UV method for the determination of ceftriaxone sodium residues on stainless steel surface of pharmaceutical manufacturing equipments.

    Science.gov (United States)

    Akl, Magda A; Ahmed, Mona A; Ramadan, Ahmed

    2011-05-15

    In pharmaceutical industry, an important step consists in the removal of possible drug residues from the involved equipments and areas. The cleaning procedures must be validated and methods to determine trace amounts of drugs have, therefore, to be considered with special attention. An HPLC-UV method for the determination of ceftriaxone sodium residues on stainless steel surface was developed and validated in order to control a cleaning procedure. Cotton swabs, moistened with extraction solution (50% water and 50% mobile phase), were used to remove any residues of drugs from stainless steel surfaces, and give recoveries of 91.12, 93.8 and 98.7% for three concentration levels. The precision of the results, reported as the relative standard deviation (RSD), were below 1.5%. The method was validated over a concentration range of 1.15-6.92 μg ml(-1). Low quantities of drug residues were determined by HPLC-UV using a Hypersil ODS 5 μm (250×4.6 mm) at 50 °C with an acetonitrile:water:pH 7:pH 5 (39-55-5.5-0.5) mobile phase at flow rate of 1.5 ml min(-1), an injection volume of 20 μl and were detected at 254 nm. A simple, selective and sensitive HPLC-UV assay for the determination of ceftriaxone sodium residues on stainless steel surfaces was developed, validated and applied. Copyright © 2011 Elsevier B.V. All rights reserved.

  2. An in vitro test to screen skin sensitizers using a stable THP-1-derived IL-8 reporter cell line, THP-G8.

    Science.gov (United States)

    Takahashi, Toshiya; Kimura, Yutaka; Saito, Rumiko; Nakajima, Yoshihiro; Ohmiya, Yoshihiro; Yamasaki, Kenshi; Aiba, Setsuya

    2011-12-01

    Several studies have suggested that interleukin (IL)-8 can serve as a biomarker for discrimination of skin sensitizers from nonsensitizers. We established a stable THP-1-derived IL-8 reporter cell line, THP-G8, which harbors SLO and SLR luciferase genes under the control of IL-8 and glyceraldehyde 3-phosphate dehydrogenase promoters, respectively. After 6 h treatment with chemicals, normalized SLO luciferase activity (nSLO-LA) was calculated by dividing SLO-LA by SLR-LA, and the fold induction of nSLO-LA (FInSLO-LA) was calculated by dividing nSLO-LA of chemically treated cells by that of nontreated cells. The nSLO-LA of THP-G8 cells increased in response to lipopolysaccharide (LPS) and several sensitizers. The FInSLO-LA in THP-G8 cells induced by LPS or sensitizers positively correlated with their induction of IL-8 messenger RNA in THP-1 cells. The nSLO-LA value of THP-G8 cells was significantly increased (FInSLO-LA ≥ 1.4) by 13 of the 15 sensitizers as well as by 5 of the 7 nonsensitizers. Interestingly, pretreatment with N-acetylcysteine suppressed the increase in FInSLO-LA induced by all sensitizers (inhibition index (II) ≤ 0.8) but did not suppress that induced by most of the nonsensitizers. We then evaluated the performance of this assay using values of FInSLO-LA ≥ 1.4 and II ≤ 0.8 in at least two of three independent experiments as the criteria of a sensitizer, which resulted in test accuracies of 82% for the 22 chemicals used and of 88% for the chemicals proposed by European Center for the Validation of Alternative Methods. This newly developed assay is a candidate replacement for animal tests of skin sensitization because of its accuracy, convenience, and high throughput performance.

  3. Determination of Dyclonine Hydrochloride by a HPLC Method and Camphor and Menthol by a GC Method in Compound Lotion

    Directory of Open Access Journals (Sweden)

    Suying Ma

    2013-01-01

    Full Text Available A high performance liquid chromatographic (HPLC method with UV detector for the determination of dyclonine hydrochloride and a gas chromatography (GC method with flame ionization detector (FID for the determination of camphor and menthol in lotion were developed. The developed HPLC method involved using a SinoChoom ODS-BP C18 reversed-phase column (5 μm, 4.6 mm × 200 mm and mobile phase consisting of acetonitrile : water : triethylamine in a ratio of 45 : 55 : 1.0; pH was adjusted to 3.5 with glacial acetic acid. The developed GC method for determination of camphor and menthol involved using an Agilent 19091J-413 capillary chromatographic column (30 m × 320 μm × 0.25 μm. The two methods were validated according to official compendia guidelines. The calibration of dyclonine hydrochloride for HPLC method was linear over the range of 20–200 μg/mL. The retention time was found at 6.0 min for dyclonine hydrochloride. The calibration of camphor and menthol of GC method was linear over the range of 10–2000 μg/mL. The retention time was found at 2.9 min for camphor and 3.05 min for menthol. The proposed HPLC and GC methods were proved to be suitable for the determination of dyclonine hydrochloride, camphor, and menthol in lotion.

  4. Two-dimensional fingerprinting approach for comparison of complex substances analysed by HPLC-UV and fluorescence detection.

    Science.gov (United States)

    Ni, Yongnian; Liu, Ying; Kokot, Serge

    2011-02-07

    This work is concerned with the research and development of methodology for analysis of complex mixtures such as pharmaceutical or food samples, which contain many analytes. Variously treated samples (swill washed, fried and scorched) of the Rhizoma atractylodis macrocephalae (RAM) traditional Chinese medicine (TCM) as well as the common substitute, Rhizoma atractylodis (RA) TCM were chosen as examples for analysis. A combined data matrix of chromatographic 2-D HPLC-DAD-FLD (two-dimensional high performance liquid chromatography with diode array and fluorescence detectors) fingerprint profiles was constructed with the use of the HPLC-DAD and HPLC-FLD individual data matrices; the purpose was to collect maximum information and to interpret this complex data with the use of various chemometrics methods e.g. the rank-ordering multi-criteria decision making (MCDM) PROMETHEE and GAIA, K-nearest neighbours (KNN), partial least squares (PLS), back propagation-artificial neural networks (BP-ANN) methods. The chemometrics analysis demonstrated that the combined 2-D HPLC-DAD-FLD data matrix does indeed provide more information and facilitates better performing classification/prediction models for the analysis of such complex samples as the RAM and RA ones noted above. It is suggested that this fingerprint approach is suitable for analysis of other complex, multi-analyte substances.

  5. Metabolite profiling with HPLC-ICP-MS as a tool for in vivo characterization of imaging probes.

    Science.gov (United States)

    Boros, Eszter; Pinkhasov, Omar R; Caravan, Peter

    2018-01-01

    Current analytical methods for characterizing pharmacokinetic and metabolic properties of positron emission tomography (PET) and single photon emission computed tomography (SPECT) probes are limited. Alternative methods to study tracer metabolism are needed. The study objective was to assess the potential of high performance liquid chromatography - inductively coupled plasma - mass spectrometry (HPLC-ICP-MS) for quantification of molecular probe metabolism and pharmacokinetics using stable isotopes. Two known peptide-DOTA conjugates were chelated with nat Ga and nat In. Limit of detection of HPLC-ICP-MS for 69 Ga and 115 In was determined. Rats were administered 50-150 nmol of Ga- and/or In-labeled probes, blood was serially sampled, and plasma analyzed by HPLC-ICP-MS using both reverse phase and size exclusion chromatography. The limits of detection were 0.16 pmol for 115 In and 0.53 pmol for 69 Ga. Metabolites as low as 0.001 %ID/g could be detected and transchelation products identified. Simultaneous administration of Ga- and In-labeled probes allowed the determination of pharmacokinetics and metabolism of both probes in a single animal. HPLC-ICP-MS is a robust, sensitive and radiation-free technique to characterize the pharmacokinetics and metabolism of imaging probes.

  6. A validated HPLC-UV method for the analysis of galloylquinic acid derivatives and flavonoids in Copaifera langsdorffii leaves.

    Science.gov (United States)

    Motta, Erick Vicente da Silva; da Costa, Juliana de Carvalho; Bastos, Jairo Kenupp

    2017-09-01

    Copaifera langsdorffii Desf. (Fabaceae, Caesalpinioideae), popularly known as "copaiba" or "pau d'óleo", is a species of tree that is found throughout Brazil. The leaves of this tree are used in folk medicine to treat kidney stones. Galloylquinic acid derivatives and flavonoids are the main secondary metabolites found in C. langsdorffii leaves and are likely to be responsible for the effectiveness of this treatment. As an attempt to produce a phytotherapic, we have developed a reliable HPLC-UV method for the quality control of C. langsdorffii leaves. Phenolic compounds were extracted from C. langsdorffii leaves using 70% aqueous ethanol as the extraction solvent. HPLC-UV analyses were carried out on a Synergi Polar-RP column (100×3.0mm, 2.5μm), and the mobile phase was made up of formic acid-water (0.1:99.9, solvent A), and isopropanol-methanol-acetonitrile (5:40:60, solvent B). The elution gradient was A:B (90:10 to 85:15) in 8.0min, followed by A:B (85:15 to 64:36) up to 30.0min, using a flow rate of 0.7mL/min, and UV detection at 280nm. This method was used to quantify nine galloylquinic acid derivatives and two flavonoids, which gave a good detection response and linearity in the range of 1.88-110.0μg/mL. Furthermore, the detection and quantification limits ranged from 0.070 to 0.752μg/mL, and 0.211-2.278μg/mL respectively, with a maximum RSD of 4.18%. The method is reliable for the quality control of C. langsdorffii raw material, its hydroethanolic extract, and could potentially be used to quantify these compounds in other Copaifera species. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. The effect of re-dissolution solvents and HPLC columns on the analysis of mycosporine-like amino acids in the eulittoral macroalgae Prasiola crispa and Porphyra umbilicalis

    Science.gov (United States)

    Karsten, Ulf; Escoubeyrou, Karine; Charles, François

    2009-09-01

    Many macroalgal species that are regularly exposed to high solar radiation such as the eulittoral green alga Prasiola crispa and the red alga Porphyra umbilicalis synthesize and accumulate high concentrations of mycosporine-like amino acids (MAAs) as UV-sunscreen compounds. These substances are typically extracted with a widely used standard protocol following quantification by various high performance liquid chromatography (HPLC) techniques. However, further preparation steps prior to HPLC analysis as well as different HPLC column types have not been systematically checked regarding separation quality and reproducibility. Therefore pure methanol, distilled water and HPLC eluent were evaluated as re-dissolution solvent for dried Prasiola and Porphyra extracts, which were subsequently analyzed on three reversed-phase C8 and C18 HPLC columns. The data indicate that distilled water and the HPLC eluent gave almost identical peak patterns and MAA contents on the C8 and C18 columns. In contrast, the application of the widely used methanol led to double peaks or even the loss of specific peaks as well as to a strong decline in total MAA amounts ranging from about 35% of the maximum in P. crispa to 80% of the maximum in P. umbilicalis. Consequently, methanol should be avoided as re-dissolution solvent for the HPLC sample preparation. An improved protocol for the MAA analysis in macroalgae in combination with a reliable C18 column is suggested.

  8. Simultaneous HPLC determination of flavonoids and phenolic acids profile in Pêra-Rio orange juice.

    Science.gov (United States)

    Mesquita, E; Monteiro, M

    2018-04-01

    The aim of this study was to develop and validate an HPLC-DAD method to evaluate the phenolic compounds profile of organic and conventional Pêra-Rio orange juice. The proposed method was validated for 10 flavonoids and 6 phenolic acids. A wide linear range (0.01-223.4μg·g -1 ), good accuracy (79.5-129.2%) and precision (CV≤3.8%), low limits of detection (1-22ng·g -1 ) and quantification (0.7-7.4μg), and overall ruggedness were attained. Good recovery was achieved for all phenolic compounds after extraction and cleanup. The method was applied to organic and conventional Pêra-Rio orange juices from beginning, middle and end of the 2016 harvest. Flavones rutin, nobiletin and tangeretin, and flavanones hesperidin, narirutin and eriocitrin were identified and quantified in all organic and conventional juices. Identity was confirmed by mass spectrometry. Nineteen non-identified phenolic compounds were quantified based on DAD spectra characteristic of the chemical class: 7 cinnamic acid derivatives, 6 flavanones and 6 flavones. The phenolic compounds profile of Pêra-Rio orange juices changed during the harvest; levels increased in organic orange juices, and decreased or were about the same in conventional orange juices. Phenolic compounds levels were higher in organic (0.5-1143.7mg·100g -1 ) than in conventional orange juices (0.5-689.7mg·100g -1 ). PCA differentiated organic from conventional FS and NFC juices, and conventional FCOJ from conventional FS and NFC juices, thus differentiating cultivation and processing. Copyright © 2017. Published by Elsevier Ltd.

  9. Interventional bleeding, hematoma and scar-formation after vacuum-biopsy under stereotactic guidance: Mammotome®-system 11g/8g vs. ATEC®-system 12g/9g

    International Nuclear Information System (INIS)

    Schaefer, F.K.W.; Order, B.M.; Eckmann-Scholz, C.; Strauss, A.; Hilpert, F.; Kroj, K.; Biernath-Wüpping, J.; Heller, M.; Jonat, W.; Schaefer, P.J.

    2012-01-01

    Purpose: To evaluate prospectively the correlation of scar-formations after vacuum-assisted biopsy with different systems and needle-sizes and interventional bleeding/post-interventional hematoma. Methods and materials: Between 01/2008 and 12/2009, 479 patients underwent vacuum-assisted biopsy under stereotactic-guidance, using the Mammotome ® -system with 11/8-gauge and ATEC ® -system with 12/9-gauge, whereas in 178 cases with representative benign histology no surgical-biopsy after vacuum-assisted biopsy was performed and at least a 2-plane-follow-up-mammogram after 6 month post-vacuum-assisted biopsy was available. Bleeding during intervention, hematoma post-intervention and scar-tissue was scored as minimal and moderate/severe. Statistical analysis included Chi-Square-trend-test, p-value ® -system vs. 11-gauge-Mammotome ® -system (41.9% vs. 8.4%, p ® -systems 9-gauge vs. 12-gauge (26.9% vs. 29.7%, p = 0.799/42.3% vs. 43.2%, p = 0.596). 11-gauge-Mammotome ® -system vs. ATEC ® -12-gauge-system revealed significantly less bleedings/hematomas (8.4% vs. 29.7%, p = 0.015/16.7% vs. 43.2%, p = 0.001), no significant differences for the large-systems (p = 0.135/p = 0.352). Follow-up of Mammotome ® -11/8-gauge-system system has shown 13.1/16.1% minimal scar-formation and 1.2/3.2% moderate/severe scars, whereas ATEC ® -12/9-gauge-system has shown 10.8/3.8% minimal scar-formation and 0/11.5% moderate/severe scars, no significant differences. No significant difference was found when comparing Mammotome ® -11/8-g-systems vs. ATEC ® -12/9-g-systems (p = 0.609/p = 0.823). There was also no correlation between risk of scar-formation after occurrence of bleeding or hematoma with any examined VAB-system or any needle size in this study (p = 0.800). Conclusion: Using larger needle-sizes significantly (Mammotome ®) /not significant for ATEC ® ) more interventional bleedings and post-interventional hematomas were detected, only a tendency concerning scar-formation.

  10. MMP-8 C-799T and MMP-8 C+17G polymorphisms in mild and severe preeclampsia: Association between MMP-8 C-799T with susceptibility to severe preeclampsia.

    Science.gov (United States)

    Rahimi, Ziba; Zangeneh, Maryam; Rezaeyan, Arezoo; Shakiba, Ebrahim; Rahimi, Zohreh

    2018-01-01

    The aim of present study was to determine the role of matrix metalloproteinase-8 (MMP-8) C-799T (rs11225395) and C+17 (rs2155052) polymorphisms in susceptibility to preeclampsia. In a case-control study, 256 pregnant women including 152 women with preeclampsia (86 women with mild preeclampsia and 66 women with severe preeclampsia) and 104 women with normal pregnancy from Western Iran with Kurdish ethnic background were investigated for MMP-8 C-799T and C + 17G polymorphisms using polymerase chain reaction-restriction fragment length polymorphism method. Comparing the MMP-8 TT genotype with the combined genotype of CC+CT (recessive model) indicated a significantly higher frequency of the MMP-8 TT genotype (47%) in severe preeclamptic patients than that in healthy pregnant women (30.8%) that was associated with 1.99-fold increased risk of severe preeclampsia (95% CI = 1.05-3.77, p = 0.034). The frequency of MMP-8 G allele was 27.3% in all preeclamptic patients compared to 30.2% in controls (p = 0.56). Also, no significant difference was detected comparing the frequency of G allele in mild (26.6%, p = 0.46) and severe preeclamptic patients (28.4%, p = 0.75) with controls (30.2%). Our study demonstrated that the MMP-8 C-799T is associated with the risk of developing severe preeclampsia during pregnancy. However, the MMP-8 C + 17G polymorphism might not be a risk factor for susceptibility to preeclampsia.

  11. Applications of HPLC/MS in the analysis of traditional Chinese medicines

    Science.gov (United States)

    Li, Miao; Hou, Xiao-Fang; Zhang, Jie; Wang, Si-Cen; Fu, Qiang; He, Lang-Chong

    2012-01-01

    In China, traditional Chinese medicines (TCMs) have been used in clinical applications for thousands of years. The successful hyphenation of high-Performance liquid chromatography (HPLC) and mass spectrometry (MS) has been applied widely in TCMs and biological samples analysis. Undoubtedly, HPLC/MS technique has facilitated the understanding of the treatment mechanism of TCMs. We reviewed more than 350 published papers within the last 5 years on HPLC/MS in the analysis of TCMs. The present review focused on the applications of HPLC/MS in the component analysis, metabolites analysis, and pharmacokinetics of TCMs etc. 50% of the literature is related to the component analysis of TCMs, which show that this field is the most populär type of research. In the metabolites analysis, HPLC coupled with electrospray ionization quadrupole time-of-flight tandem mass spectrometry has been demonstrated to be the powerful tool for the characterization of structural features and fragmentation behavior patterns. This paper presented a brief overview of the applications of HPLC/MS in the analysis of TCMs. HPLC/MS in the fingerprint analysis is reviewed elsewhere. PMID:29403684

  12. Characterization of incompletely typed rotavirus strains from Guinea-Bissau: identification of G8 and G9 types and a high frequency of mixed infections

    DEFF Research Database (Denmark)

    Fischer, T.K.; Page, N.A.; Griffin, D.D.

    2003-01-01

    %, respectively, identical to other African G8 and G9 strains. Multiple G and/or P types were identified at a high frequency (59%), including two previously undescribed mixed infections, P[4]P[6], G2G8 and P[4]P[6], G2G9. These mixed infections most likely represent naturally occurring reassortance of rotavirus......] and P[6] primer binding sites were detected. These findings highlight the need for regular evaluation of the multiplex primer PCR method and typing primers. The high frequency of uncommon as well as reassortant rotavirus strains in countries where rotavirus is an important cause of child mortality...... underscores the need for extensive strain surveillance as a basis to develop appropriate rotavirus vaccine candidates....

  13. [Relationships between smoking and the health locus of control among junior high school students].

    Science.gov (United States)

    Yoshida, Yumi; Takagi, Hirofumi; Inaba, Yutaka

    2007-10-01

    To clarify effects of the Health Locus of Control (HLC) on smoking behavior, relationships between smoking and HLC among junior high school students were examined. The subjects of the initial study, conducted in 1991, were public elementary schoolchildren in their 3rd year (11-12 years old). We then investigated the same children again in 1994 and 1997. We here mainly used data for 265 students (136 males and 129 females) obtained in 1997 when they were public junior high school students in their 3rd year (14-15 years old). Questionnaires included items on smoking experience, smoking intention and the Parcel & Meyer's Children's HLC scales. 1. Smoking experience was not associated with the HLC. 2. Concerning smoking intention among boys, the neutral group expressed stronger beliefs in the powerful others HLC in 1994 and 1997 than the positive group. In addition, the positive group expressed weaker beliefs in the powerful others HLC in 1994 than the negative group. 3. Concerning smoking intention among girls, the neutral group expressed stronger belifs in the powerful others HLC in 1997 than the negative group. Smoking experience was not associated with the HLC. However, smoking intention was significantly associated with beliefs in the powerful others HLC. In this regard, the neutral group tended to have strong beliefs in the powerful others HLC suggesting that students in this group might be easily affected by other people in both positive and negative ways. In other words, they must be guided in a good fashion through appropriate health education.

  14. Human rotavirus strains circulating in Venezuela after vaccine introduction: predominance of G2P[4] and reemergence of G1P[8].

    Science.gov (United States)

    Vizzi, Esmeralda; Piñeros, Oscar A; Oropeza, M Daniela; Naranjo, Laura; Suárez, José A; Fernández, Rixio; Zambrano, José L; Celis, Argelia; Liprandi, Ferdinando

    2017-03-21

    Rotavirus (RV) is the most common cause of severe childhood diarrhea worldwide. Despite Venezuela was among the first developing countries to introduce RV vaccines into their national immunization schedules, RV is still contributing to the burden of diarrhea. Concerns exist about the selective pressure that RV vaccines could exert on the predominant types and/or emergence of new strains. To assess the impact of RV vaccines on the genotype distribution 1 year after the vaccination was implemented, a total of 912 fecal specimens, collected from children with acute gastroenteritis in Caracas from February 2007 to April 2008, were screened, of which 169 (18.5%) were confirmed to be RV positive by PAGE. Rotavirus-associated diarrhea occurred all year-round, although prevailed during the coolest and driest months among unvaccinated children under 24 months old. Of 165 RV strains genotyped for G (VP7) and P (VP4) by seminested multiplex RT-PCR, 77 (46.7%) were G2P[4] and 63 (38.2%) G1P[8]. G9P[8], G3P[8] and G2P[6] were found in a lower proportion (7.3%). Remarkable was also the detection of rotaviruses, but they were rather distant from Rotarix ® vaccine and pre-vaccine strains. Unique amino acid substitutions observed on neutralization domains of the VP7 sequence from Venezuelan post-vaccine G1P[8] could have conditioned their re-emergence and a more efficient dissemination into susceptible population. The results suggest that natural fluctuations of genotypes in combination with forces driving the genetic evolution could determine the spread of novel strains, whose long-term effect on the efficacy of available vaccines should be determined.

  15. G8 global partnership. France's contribution; Partenariat mondial du G8. L'action de la France

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2005-09-15

    During the G8 summit at Kananaskis (Canada) in June 2002, G8 Leaders decided to launch the Global Partnership against the Spread of Weapons and Materials of Mass Destruction. Under this initiative, partners support specific cooperation projects to address non-proliferation, disarmament, counter-terrorism and nuclear safety issues. Since then, thirteen other donor countries have joined the initiative from which the Ukraine may also now benefit. France intends to make an effective contribution, up to 750 million euros, to the implementation of this initiative, giving priority to a genuine partnership between France and Russia covering projects in the nuclear, chemical and biological fields. France intends to be involved in the various fields identified at Kananaskis: in the nuclear field, it is participating in nuclear submarine dismantling actions and contributes to the improvement of nuclear safety and security. It also supports the program for the disposition of Russian weapons-grade plutonium designated as no longer required for defence purposes. France is also involved in the destruction of chemical weapons and intends to develop responses to bio-terrorist threats, while promoting reemployment of scientists. To optimise its action, France has committed itself to both multilateral and bilateral programs. In the multilateral framework, France contributes to: - the NDEP fund (Northern Dimension Environment Partnership) which will finance projects related to the dismantling of nuclear submarines and remediation of the sites concerned; - the MPDG (Multilateral Plutonium Disposition Group), whose objective is to enable the disposition of Russian weapons-grade plutonium designated as no longer required for defence purposes; - the construction of the new Chernobyl shelter in the Ukraine. France is also developing bilateral cooperation, primarily with Russia: - in the nuclear field, the implementing agreement negotiated in the framework of the Multilateral Environmental

  16. Vergelijking van HPLC-methoden voor de bepaling van pentachloorfenol in houtmonsters

    NARCIS (Netherlands)

    Goewie; C.E.; Berkhoff; C.J.

    1986-01-01

    Een vergelijkend onderzoek is verricht naar de bruikbaarheid van verschillende detectiemethoden in combinatie met HPLC voor de analyse van pentachloorfenol in hout. In het onderzoek wordt RP-HPLC met UK en amperometrische detectie beschreven, evenals NP-HPLC met elektroneninvangdetectie. In

  17. Analysis of sesquiterpene lactones, lignans, and flavonoids in wormwood (Artemisia absinthium L.) using high-performance liquid chromatography (HPLC)-mass spectrometry, reversed phase HPLC, and HPLC-solid phase extraction-nuclear magnetic resonance.

    Science.gov (United States)

    Aberham, Anita; Cicek, Serhat Sezai; Schneider, Peter; Stuppner, Hermann

    2010-10-27

    Today, the medicinal use of wormwood (Artemisia absinthium) is enjoying a resurgence of popularity. This study presents a specific and validated high-performance liquid chromatography (HPLC)-diode array detection method for the simultaneous determination and quantification of bioactive compounds in wormwood and commercial preparations thereof. Five sesquiterpene lactones, two lignans, and a polymethoxylated flavonoid were baseline separated on RP-18 material, using a solvent gradient consisting of 0.085% (v/v) o-phosphoric acid and acetonitrile. The flow rate was 1.0 mL/min, and chromatograms were recorded at 205 nm. The stability of absinthin was tested exposing samples to light, moisture, and different temperatures. Methanolic and aqueous solutions of absinthin were found to be stable for up to 6 months. This was also the case when the solid compound was kept in the refrigerator at -35 °C. In contrast, the colorless needles, when stored at room temperature, turned yellow. Three degradation compounds (anabsin, anabsinthin, and the new dimer 3'-hydroxyanabsinthin) were identified by HPLC-mass spectrometry and HPLC-solid-phase extraction-nuclear magnetic resonance and quantified by the established HPLC method.

  18. On-line radioactivity detector for HPLC

    International Nuclear Information System (INIS)

    Kessler, M.J.

    1986-01-01

    Over the last ten years the technique of high performance liquid chromotography (HPLC) has become extensively employed for the separation and quantitation of various biological, organic, and inorganic substances. The use of HPLC for the separation of various metabolic compounds has become routine. The major problem of analyzing the metabolism process is that the quantitation is accomplished by the use of radioactive substrates. Until recently the only method to quantitate these radioactive compounds eluting from the HPLC was by collecting fractions at preset times, removing aliquots and quantitating in a liquid scintillation counter. Once the radioactivity present in each fraction was determined, the results were plotted on a graph and the area of each of the radioactive peaks was determined. This entire process required from 3-20 hours. The introduction of the flow through radioactivity detector enable the investigator to directly quantitate the radioactive peaks as they elute from the HPLC in real time and at about one-tenth the original cost of the previous methods. The detection limits of this technique are dependent on the residence time of the sample in the flow cell and the type of flow cell used for the analysis. Using a 2.5 ml liquid flow cell, (mixing with liquid scintillation solution), base line resolution can be obtained for peaks 1.5 minutes apart, and a sensitivity of 70 dpm for tritium and 30 dpm for carbon-14 can be achieved

  19. Encapsulation of probiotic Bifidobacterium longum BIOMA 5920 with alginate-human-like collagen and evaluation of survival in simulated gastrointestinal conditions.

    Science.gov (United States)

    Su, Ran; Zhu, Xiao-Li; Fan, Dai-Di; Mi, Yu; Yang, Chan-Yuan; Jia, Xin

    2011-12-01

    Alginate (ALg)-human-like collagen (HLC) microspheres were prepared by the technology of electrostatic droplet generation in order to develop a biocompatible vehicle for probiotic bacteria. Microparticles were spherical with mean particle size of 400μm. The encapsulation efficiency (EE) of ALg-HLC microspheres could reach 92-99.2%. Water-soluble and fibrous human-like collagen is combined with sodium alginate through intermolecular hydrogen bonding and electrostatic force which were investigated by Fourier transform infrared spectroscopy (FTIR) and differential scanning calorimetry (DSC), thus the matrix of ALg-HLC was very stable. Bifidobacterium longum BIOMA 5920, as a kind of probiotic bacteria, was encapsulated with alginate-human-like collagen to survive and function in simulated gastrointestinal juice. Microparticles were very easy to degradation in simulated intestinal juices. After incubation in simulated gastric (pH 2.0, 2h), the encapsulated B. longum BIOMA 5920 numbers were 4.81 ± 0.38 log cfu/g. Copyright © 2011 Elsevier B.V. All rights reserved.

  20. Development of an Ultrasonication-Assisted Extraction Based HPLC With a Fluorescence Method for Sensitive Determination of Aflatoxins in Highly Acidic Hibiscus sabdariffa.

    Science.gov (United States)

    Liu, Xiaofei; Ying, Guangyao; Sun, Chaonan; Yang, Meihua; Zhang, Lei; Zhang, Shanshan; Xing, Xiaoyan; Li, Qian; Kong, Weijun

    2018-01-01

    The high acidity and complex components of Hibiscus sabdariffa have provided major challenges for sensitive determination of trace aflatoxins. In this study, sample pretreatment of H. sabdariffa was systematically developed for sensitive high performance liquid chromatography-fluorescence detection (HPLC-FLD) after ultrasonication-assisted extraction, immunoaffinity column (IAC) clean-up and on-line post-column photochemical derivatization (PCD). Aflatoxins B 1 , B 2 , G 1 , G 2 were extracted from samples by using methanol/water (70:30, v/v ) with the addition of NaCl. The solutions were diluted 1:8 with 0.1 M phosphate buffer (pH 8.0) to negate the issues of high acidity and matrix interferences. The established method was validated with satisfactory linearity ( R > 0.999), sensitivity (limits of detection (LODs) and limits of quantitation (LOQs) of 0.15-0.65 and 0.53-2.18 μg/kg, respectively), precision (RSD sabdariffa samples indicated that one sample incubated with Aspergillus flavus was positive with aflatoxin B 1 (AFB 1 ) at 3.11 μg/kg. The strategy developed in this study also has the potential to reliably extract and sensitively detect more mycotoxins in other complex acidic matrices, such as traditional Chinese medicines, foodstuffs, etc.

  1. Novel magnetic hollow zein nanoparticles for preconcentration of chlorpyrifos from water and soil samples prior to analysis via high-performance liquid chromatography (HPLC).

    Science.gov (United States)

    Rahimi Moghadam, Mojtaba; Zargar, Behrooz; Rastegarzadeh, Saadat

    2018-04-30

    Herein, magnetically hollow zein nanoparticles were synthesized and used as a magnetic sorbent for the preconcentration of chlorpyrifos and its analysis by high-performance liquid chromatography (HPLC). Morphology of the sorbent was characterized by transmission electron microscopy (TEM). In this study, the effects of important parameters such as pH of the solution, adsorption and desorption time, type and volume of desorption solvent, and salt addition were investigated. Under optimized experimental conditions, the linear range was from 50 to 2000 μg mL-1, and an LOD of 25 μg L-1 was calculated. The relative standard deviations (RSD) varied from 3.8 to 5.1% (n = 5). The enrichment factors for 50 and 100 μg L-1 samples were calculated as 187 and 210, respectively. The developed method was successfully applied in soil and water samples and showed good extraction recoveries.

  2. HPLC-based quantification of bacterial housekeeping nucleotides and alarmone messengers ppGpp and pppGpp.

    Science.gov (United States)

    Varik, Vallo; Oliveira, Sofia Raquel Alves; Hauryliuk, Vasili; Tenson, Tanel

    2017-09-08

    Here we describe an HPLC-based method to quantify bacterial housekeeping nucleotides and the signaling messengers ppGpp and pppGpp. We have replicated and tested several previously reported HPLC-based approaches and assembled a method that can process 50 samples in three days, thus making kinetically resolved experiments feasible. The method combines cell harvesting by rapid filtration, followed by acid extraction, freeze-drying with chromatographic separation. We use a combination of C18 IPRP-HPLC (GMP unresolved and co-migrating with IMP; GDP and GTP; AMP, ADP and ATP; CTP; UTP) and SAX-HPLC in isocratic mode (ppGpp and pppGpp) with UV detection. The approach is applicable to bacteria without the requirement of metabolic labelling with 32P-labelled radioactive precursors. We applied our method to quantify nucleotide pools in Escherichia coli BW25113 K12-strain both throughout the growth curve and during acute stringent response induced by mupirocin. While ppGpp and pppGpp levels vary drastically (40- and ≥8-fold, respectively) these changes are decoupled from the quotients of the housekeeping pool and guanosine and adenosine housekeeping nucleotides: NTP/NDP/NMP ratio remains stable at 6/1/0.3 during both normal batch culture growth and upon acute amino acid starvation.

  3. G 126.1-0.8-14: A molecular shell related to Sh2-187

    Science.gov (United States)

    Cichowolski, S.; Pineault, S.; Gamen, R.; Ortega, M. E.; Arnal, E. M.; Suad, L. A.

    2014-10-01

    We present a multi-wavelength study of a region where a well defined molecular shell, named G 126.1-0.8-14, is observed. The distance of G 126.1-0.8-14 is about 1 kpc. Based on HI and CO data we analyze the atomic and molecular gas related to the structure and estimate its main physical properties. From the radio continuum and infrared data we analyze whether the emission associated with G 126.1-0.8-14 has a thermal origin. To disentangle the possible origin of the shell, and given the lack of catalogued O-type stars in the area, we observed with GEMINI the spectra of four OB stars located in projection inside the shell, to get their accurate spectral types and distances. The young HII region Sh2-187 is located onto the densest part of this molecular shell. A search for young stellar object candidates (cYSOs) was made using infrared point source catalogs. Several cYSOs are found spread out onto the shell. Based on all the available data, we discuss the possible origin of G 126.1-0.8-14 as well as its role in the formation of a new generation of stars.

  4. DISCOVERY OF X-RAY EMISSION FROM AND DISTANCE TO THE SUPERNOVA REMNANT G84.2-0.8

    Energy Technology Data Exchange (ETDEWEB)

    Leahy, Denis A.; Green, Kaylie S., E-mail: leahy@ucalgary.ca, E-mail: ksgreen@ucalgary.ca [Department of Physics and Astronomy, University of Calgary, Calgary, Alberta, T2N 1N4 (Canada)

    2012-11-20

    We analyze X-ray and radio observations of the supernova remnant G84.2-0.8. 1420 MHz atomic hydrogen (H I) line and radio continuum data yield H I absorption spectra and a new H I absorption distance of 5.8-6.2 kpc. Archival X-ray observations from ROSAT and Chandra which cover the area including G84.2-0.8 are analyzed to show extended X-ray emission from G84.2-0.8. Fits to X-ray spectra from Chandra, with the new H I distance of 5.8-6.2 kpc, are used to determine the Sedov parameters of the supernova remnant. G84.2-0.8 is large (16-18 pc radius), middle aged ({approx}9000 yr), expanding in low-density interstellar medium (0.02 cm{sup -3}), and consistent with a low explosion energy (0.8-6.5 Multiplication-Sign 10{sup 50} erg).

  5. Ramalina capitata (Ach.) Nyl. acetone extract: HPLC analysis, genotoxicity, cholinesterase, antioxidant and antibacterial activity.

    Science.gov (United States)

    Zrnzevic, Ivana; Stankovic, Miroslava; Stankov Jovanovic, Vesna; Mitic, Violeta; Dordevic, Aleksandra; Zlatanovic, Ivana; Stojanovic, Gordana

    2017-01-01

    In the present investigation, effects of Ramalina capitata acetone extract on micronucleus distribution on human lymphocytes, on cholinesterase activity and antioxidant activity (by the CUPRAC method) were examined, for the first time as well as its HPLC profile. Additionally, total phenolic compounds (TPC), antioxidant properties (estimated via DPPH, ABTS and TRP assays) and antibacterial activity were determined. The predominant phenolic compounds in this extract were evernic, everninic and obtusatic acids. Acetone extract of R. capitata at concentration of 2 μg mL -1 decreased a frequency of micronuclei (MN) for 14.8 %. The extract reduces the concentration of DPPH and ABTS radicals for 21.2 and 36.1 % (respectively). Values for total reducing power (TRP) and cupric reducing capacity (CUPRAC) were 0.4624 ± 0.1064 μg ascorbic acid equivalents (AAE) per mg of dry extract, and 6.1176 ± 0.2964 μg Trolox equivalents (TE) per mg of dry extract, respectively. The total phenol content was 670.6376 ± 66.554 μg galic acid equivalents (GAE) per mg of dry extract. Tested extract at concentration of 2 mg mL -1 exhibited inhibition effect (5.2 %) on pooled human serum cholinesterase. The antimicrobial assay showed that acetone extract had inhibition effect towards Gram-positive strains. The results of manifested antioxidant activity, reducing the number of micronuclei in human lymphocytes, and antibacterial activity recommends R. capitata extract for further in vivo studies.

  6. G8 Global Partnership: Germany's contribution to strengthening international security

    International Nuclear Information System (INIS)

    Pfaffernoschke, A.

    2013-01-01

    This series of slides presents the German contribution to the G8 Global partnership whose aim is to support specific cooperation projects to address non-proliferation, disarmament, counter-terrorism and nuclear safety issues. 4 priorities have been identified: -) destruction of chemical weapons, -) dismantlement of decommissioned nuclear submarines, -) disposition of fissile materials, and -) employment of former weapon scientists. Today there are 23 donor countries and 2 official recipient countries (Russian Federation and Ukraine). Since the beginning Germany's activities in the G8 Global partnership have focused on chemical weapon destruction (340 million euros), dismantlement of nuclear submarines (600 million euros) and physical protection of nuclear materials (170 million euros). In the Gorny project (1995-2005) German provided the incinerator for the thermal treatment of liquid and solid residues and the equipment for destruction by hydrolysis. Germany's contribution to the following projects: -) the Kambarka project (2003-2007) for the destruction of lewisite, -) the Pochep project (2007-2010) for the destruction of munition containing nerve agents, and -) the Sajda-Bay project for the construction of a long-term storage site for reactor sections of decommissioned submarines, are detailed

  7. Implementation of the G8GP program on physical protection - experiences and results

    International Nuclear Information System (INIS)

    Hagemann, A.

    2006-01-01

    At the Kananaskis Summit in June 2002, G8 Leaders launched the Global Partnership against the Spread of Weapons and Materials of Mass Destruction committing to support projects to issues of non-proliferation, disarmament, counter terrorism and nuclear safety in Russia. Since then progress has been made in implementing projects. The German Federal Foreign Office contracted GRS to implement a program for improving the physical protection of nuclear or highly radioactive materials of relevance at facilities in the Russian Federation. This paper reports about this G8GP Program on physical protection, its implementation, gained experiences, current achievements and results. (author)

  8. Comparative analysis of pentavalent rotavirus vaccine strains and G8 rotaviruses identified during vaccine trial in Africa.

    Science.gov (United States)

    Heylen, Elisabeth; Zeller, Mark; Ciarlet, Max; Lawrence, Jody; Steele, Duncan; Van Ranst, Marc; Matthijnssens, Jelle

    2015-10-06

    RotaTeqTM is a pentavalent rotavirus vaccine based on a bovine rotavirus genetic backbone in vitro reassorted with human outer capsid genes. During clinical trials of RotaTeqTM in Sub-Saharan Africa, the vaccine efficacy over a 2-year follow-up was lower against the genotypes contained in the vaccine than against the heterotypic G8P[6] and G8P[1] rotavirus strains of which the former is highly prevalent in Africa. Complete genome analyses of 43 complete rotavirus genomes collected during phase III clinical trials of RotaTeqTM in Sub-Saharan Africa, were conducted to gain insight into the high level of cross-protection afforded by RotaTeqTM against these G8 strains. Phylogenetic analysis revealed the presence of a high number of bovine rotavirus gene segments in these human G8 strains. In addition, we performed an in depth analysis on the individual amino acid level which showed that G8 rotaviruses were more similar to the RotaTeqTM vaccine than non-G8 strains. Because RotaTeqTM possesses a bovine genetic backbone, the high vaccine efficacy against G8 strains might be partially explained by the fact that all these strains contain a complete or partial bovine-like backbone. Altogether, this study supports the hypothesis that gene segments other than VP7 and VP4 play a role in vaccine-induced immunity.

  9. Fermi Large Area Telescope Observations of the Supernova Remnant G8.7-0.1

    Energy Technology Data Exchange (ETDEWEB)

    Ajello, M.; Allafort, A.; /Stanford U., HEPL /KIPAC, Menlo Park /SLAC; Baldini, L.; /INFN, Pisa; Ballet, J.; /AIM, Saclay; Barbiellini, G.; /INFN, Trieste /Trieste U.; Bastieri, D.; /INFN, Padua /Padua U.; Bechtol, K.; /Stanford U., HEPL /KIPAC, Menlo Park /SLAC; Bellazzini, R.; /INFN, Pisa; Berenji, B.; Blandford, R.D.; Bloom, E.D.; /Stanford U., HEPL /KIPAC, Menlo Park /SLAC; Bonamente, E.; /INFN, Perugia /Perugia U.; Borgland, A.W.; /Stanford U., HEPL /KIPAC, Menlo Park /SLAC; Bregeon, J.; /INFN, Pisa; Brigida, M.; /Bari Polytechnic /INFN, Bari; Bruel, P.; /Ecole Polytechnique; Buehler, R.; /Stanford U., HEPL /KIPAC, Menlo Park /SLAC; Buson, S.; /INFN, Padua /Padua U.; Caliandro, G.A.; /CSIC, Catalunya; Cameron, R.A.; /Stanford U., HEPL /KIPAC, Menlo Park /SLAC; Caraveo, P.A.; /IASF, Milan /AIM, Saclay /INFN, Perugia /Perugia U. /Stanford U., HEPL /KIPAC, Menlo Park /SLAC /Unlisted, US /Naval Research Lab, Wash., D.C. /Perugia U. /ASDC, Frascati /Stanford U., HEPL /KIPAC, Menlo Park /SLAC /Montpellier U. /ASDC, Frascati /Udine U. /INFN, Trieste /Bari Polytechnic /INFN, Bari /Naval Research Lab, Wash., D.C. /Stanford U., HEPL /KIPAC, Menlo Park /SLAC /Bari Polytechnic /INFN, Bari /Ecole Polytechnique /NASA, Goddard /Stanford U., HEPL /KIPAC, Menlo Park /SLAC /Udine U. /INFN, Trieste /Trieste Observ. /Hiroshima U. /Nagoya U. /Bari Polytechnic /INFN, Bari /INFN, Bari /ASDC, Frascati /INFN, Perugia /Perugia U. /Bari Polytechnic /INFN, Bari /ASDC, Frascati /Bari Polytechnic /INFN, Bari /Bologna Observ. /Stanford U., HEPL /KIPAC, Menlo Park /SLAC /Naval Research Lab, Wash., D.C. /Alabama U., Huntsville /CSIC, Catalunya /Hiroshima U. /NASA, Goddard /Hiroshima U.; /more authors..

    2012-09-14

    We present a detailed analysis of the GeV gamma-ray emission toward the supernova remnant (SNR) G8.7-0.1 with the Large Area Telescope (LAT) on board the Fermi Gamma-ray Space Telescope. An investigation of the relationship between G8.7-0.1 and the TeV unidentified source HESS J1804-216 provides us with an important clue on diffusion process of cosmic rays if particle acceleration operates in the SNR. The GeV gamma-ray emission is extended with most of the emission in positional coincidence with the SNR G8.7-0.1 and a lesser part located outside the western boundary of G8.7-0.1. The region of the gamma-ray emission overlaps spatially connected molecular clouds, implying a physical connection for the gamma-ray structure. The total gamma-ray spectrum measured with LAT from 200 MeV-100 GeV can be described by a broken power-law function with a break of 2.4 {+-} 0.6 (stat) {+-} 1.2 (sys) GeV, and photon indices of 2.10 {+-} 0.06 (stat) {+-} 0.10 (sys) below the break and 2.70 {+-} 0.12 (stat) {+-} 0.14 (sys) above the break. Given the spatial association among the gamma rays, the radio emission of G8.7-0.1, and the molecular clouds, the decay of p0s produced by particles accelerated in the SNR and hitting the molecular clouds naturally explains the GeV gamma-ray spectrum. We also find that the GeV morphology is not well represented by the TeV emission from HESS J1804-216 and that the spectrum in the GeV band is not consistent with the extrapolation of the TeV gamma-ray spectrum. The spectral index of the TeV emission is consistent with the particle spectral index predicted by a theory that assumes energy-dependent diffusion of particles accelerated in an SNR. We discuss the possibility that the TeV spectrum originates from the interaction of particles accelerated in G8.7-0.1 with molecular clouds, and we constrain the diffusion coefficient of the particles.

  10. Fermi Large Area Telescope Observations of the Supernova Remnant G8.7-0.1

    International Nuclear Information System (INIS)

    2012-01-01

    We present a detailed analysis of the GeV gamma-ray emission toward the supernova remnant (SNR) G8.7-0.1 with the Large Area Telescope (LAT) on board the Fermi Gamma-ray Space Telescope. An investigation of the relationship between G8.7-0.1 and the TeV unidentified source HESS J1804-216 provides us with an important clue on diffusion process of cosmic rays if particle acceleration operates in the SNR. The GeV gamma-ray emission is extended with most of the emission in positional coincidence with the SNR G8.7-0.1 and a lesser part located outside the western boundary of G8.7-0.1. The region of the gamma-ray emission overlaps spatially connected molecular clouds, implying a physical connection for the gamma-ray structure. The total gamma-ray spectrum measured with LAT from 200 MeV-100 GeV can be described by a broken power-law function with a break of 2.4 ± 0.6 (stat) ± 1.2 (sys) GeV, and photon indices of 2.10 ± 0.06 (stat) ± 0.10 (sys) below the break and 2.70 ± 0.12 (stat) ± 0.14 (sys) above the break. Given the spatial association among the gamma rays, the radio emission of G8.7-0.1, and the molecular clouds, the decay of p0s produced by particles accelerated in the SNR and hitting the molecular clouds naturally explains the GeV gamma-ray spectrum. We also find that the GeV morphology is not well represented by the TeV emission from HESS J1804-216 and that the spectrum in the GeV band is not consistent with the extrapolation of the TeV gamma-ray spectrum. The spectral index of the TeV emission is consistent with the particle spectral index predicted by a theory that assumes energy-dependent diffusion of particles accelerated in an SNR. We discuss the possibility that the TeV spectrum originates from the interaction of particles accelerated in G8.7-0.1 with molecular clouds, and we constrain the diffusion coefficient of the particles.

  11. Development and Validation of a Precise, Single HPLC Method for the Determination of Tolperisone Impurities in API and Pharmaceutical Dosage Forms.

    Science.gov (United States)

    Raju, Thummala Veera Raghava; Seshadri, Raja Kumar; Arutla, Srinivas; Mohan, Tharlapu Satya Sankarsana Jagan; Rao, Ivaturi Mrutyunjaya; Nittala, Someswara Rao

    2013-01-01

    A novel, sensitive, stability-indicating HPLC method has been developed for the quantitative estimation of Tolperisone-related impurities in both bulk drugs and pharmaceutical dosage forms. Effective chromatographic separation was achieved on a C18 stationary phase with a simple mobile phase combination delivered in a simple gradient programme, and quantitation was by ultraviolet detection at 254 nm. The mobile phase consisted of a buffer and acetonitrile delivered at a flow rate 1.0 ml/min. The buffer consisted of 0.01 M potassium dihydrogen phosphate with the pH adjusted to 8.0 by using diethylamine. In the developed HPLC method, the resolution between Tolperisone and its four potential impurities was found to be greater than 2.0. Regression analysis showed an R value (correlation coefficient) of greater than 0.999 for the Tolperisone impurities. This method was capable of detecting all four impurities of Tolperisone at a level of 0.19 μg/mL with respect to the test concentration of 1000 μg/mL for a 10 µl injection volume. The tablets were subjected to the stress conditions of hydrolysis, oxidation, photolysis, and thermal degradation. Considerable degradation was found to occur in base hydrolysis, water hydrolysis, and oxidation. The stress samples were assayed against a qualified reference standard and the mass balance was found to be close to 100%. The established method was validated and found to be linear, accurate, precise, specific, robust, and rugged.

  12. EPR imaging and HPLC characterization of the pigment-based organic free radical in black soybean seeds.

    Science.gov (United States)

    Nakagawa, Kouichi; Maeda, Hayato

    2017-02-01

    We investigated the location and distribution of paramagnetic species in dry black, brown, and yellow (normal) soybean seeds using electron paramagnetic resonance (EPR), X-band (9 GHz) EPR imaging (EPRI), and HPLC. EPR primarily detected two paramagnetic species in black soybean. These two different radical species were assigned as stable organic radical and Mn 2+  species based on the g values and hyperfine structures. The signal from the stable radical was noted at g ≈ 2.00 and was relatively strong and stable. Subsequent noninvasive two-dimensional (2D) EPRI of the radical present in black soybean revealed that the stable radical was primarily located in the pigmented region of the soybean coat, with very few radicals observed in the soybean cotyledon (interior). Pigments extracted from black soybean were analyzed using HPLC. The major compound was found to be cyanidin-3-glucoside. Multi-EPR and HPLC results indicate that the stable radical was only found within the pigmented region of the soybean coat, and it could be cyanidin-3-glucoside or an oxidative decomposition product.

  13. Direct 13C NMR Detection in HPLC Hyphenation Mode

    DEFF Research Database (Denmark)

    Wubshet, Sileshi Gizachew; Johansen, Kenneth; Nyberg, Nils

    2012-01-01

    Solid phase extraction (SPE) was introduced as a crucial step in the HPLC-SPE-NMR technique to enable online analyte enrichment from which proton-detected NMR experiments on submicrogram amounts from complex mixtures were possible. However, the significance of direct-detected (13)C NMR experiments...... application of HPLC-SPE-NMR analysis using direct-detected (13)C NMR spectra. HPLC column loading, accumulative SPE trappings, and the effect of different elution solvents were evaluated and optimized. A column loading of approximately 600 mug of a prefractionated triterpenoid mixture, six trappings...

  14. HPLC-RID-DAD-MS analysis of 18F-Fluorodeoxyglucose

    International Nuclear Information System (INIS)

    Macasek, F.; Buriova, E.; Bruder, P.

    2001-01-01

    Objective of new method of FDG analysis development is to replace existing tests by more complex assay. In this work, a liquid chromatography/refractive index detector/diode array detector/mass spectrometric detector combination (HPLC/RID/DAD/MSD) was used for development of a complex routine technique. Optimization of the HPLC/MS analysis was performed investigating MSD analytical signal as a function of various eluent composition. HPLC-RID-DAD-MSD analysis has potentiality of a complex quality control of radiopharmaceuticals, FDG in particular, providing information about: isotope composition; chemical composition; biochemical composition; radiation stability; pharmacodynamics. (author)

  15. A convenient method for the quantitative determination of elemental sulfur in coal by HPLC analysis of perchloroethylene extracts

    Science.gov (United States)

    Buchanan, D.H.; Coombs, K.J.; Murphy, P.M.; Chaven, C.

    1993-01-01

    A convenient method for the quantitative determination of elemental sulfur in coal is described. Elemental sulfur is extracted from the coal with hot perchloroethylene (PCE) (tetrachloroethene, C2Cl4) and quantitatively determined by HPLC analysis on a C18 reverse-phase column using UV detection. Calibration solutions were prepared from sublimed sulfur. Results of quantitative HPLC analyses agreed with those of a chemical/spectroscopic analysis. The HPLC method was found to be linear over the concentration range of 6 ?? 10-4 to 2 ?? 10-2 g/L. The lower detection limit was 4 ?? 10-4 g/L, which for a coal sample of 20 g is equivalent to 0.0006% by weight of coal. Since elemental sulfur is known to react slowly with hydrocarbons at the temperature of boiling PCE, standard solutions of sulfur in PCE were heated with coals from the Argonne Premium Coal Sample program. Pseudo-first-order uptake of sulfur by the coals was observed over several weeks of heating. For the Illinois No. 6 premium coal, the rate constant for sulfur uptake was 9.7 ?? 10-7 s-1, too small for retrograde reactions between solubilized sulfur and coal to cause a significant loss in elemental sulfur isolated during the analytical extraction. No elemental sulfur was produced when the following pure compounds were heated to reflux in PCE for up to 1 week: benzyl sulfide, octyl sulfide, thiane, thiophene, benzothiophene, dibenzothiophene, sulfuric acid, or ferrous sulfate. A sluury of mineral pyrite in PCE contained elemental sulfur which increased in concentration with heating time. ?? 1993 American Chemical Society.

  16. Characterization of incompletely typed rotavirus strains from Guinea-Bissau: identification of G8 and G9 types and a high frequency of mixed infections

    DEFF Research Database (Denmark)

    Fischer, TK; Page, NA; Griffin, DD

    2003-01-01

    Among 167 rotavirus specimens collected from young children in a suburban area of Bissau, Guinea-Bissau, from 1996 to 1998, most identifiable strains belonged to the uncommon P[6], G2 type and approximately 50% remained incompletely typed. In the present study, 76 such strains were further......%, respectively, identical to other African G8 and G9 strains. Multiple G and/or P types were identified at a high frequency (59%), including two previously undescribed mixed infections, P[4]P[6], G2G8 and P[4]P[6], G2G9. These mixed infections most likely represent naturally occurring reassortance of rotavirus......] and P[6] primer binding sites were detected. These findings highlight the need for regular evaluation of the multiplex primer PCR method and typing primers. The high frequency of uncommon as well as reassortant rotavirus strains in countries where rotavirus is an important cause of child mortality...

  17. Analysis of brominated and phosphate-based flame retardants in polymer samples by HPLC-UV/MS and online-GPC-HPLC-UV

    Energy Technology Data Exchange (ETDEWEB)

    Schlummer, M.; Brandl, F. [Fraunhofer-Institut fuer Verfahrenstechnik und Verpackung (IVV), Freising (Germany); Maeurer, A.

    2004-09-15

    Here we present two analytical approaches for the identification and quantification of brominated and phosphate-based flame retardants. The first is an HPLC-UV/MS approach, which allows the separation and unequivocal identification and quantification of at least 15 different technical flame retardants. The second approach was set-up as a screening tool, consisting of a GPC separation coupled to an HPLC-UV device.

  18. Chiral chromatography studies of chemical behavior of cinacalcet on polysaccharide chiral reversed-phase HPLC stationary phases.

    Science.gov (United States)

    Dousa, Michal; Brichác, Jirí

    2012-01-01

    A rapid HPLC method for the analytical resolution of cinacalcet enantiomers was developed. Four chiral columns (two amylose and two cellulose type) were evaluated in RP systems. Excellent enantioseparation with a resolution of more than 6 was achieved on Chiralpak AY (amylose 5-chloro-2-methylphenylcarbamate chiral stationary phase) using 10 mM triethylamine (pH 8.0)-acetonitrile (40 + 60, v/v) mobile phase. Validation of the HPLC method, including linearity, LOD, LOQ, precision, accuracy, and selectivity, was performed according to the International Conference on Harmonization guidelines. The method was successfully applied for the determination of (S)-cinacalcet in enantiopure active pharmaceutical ingredient (R)-cinacalcet.

  19. 72 - 80_Aminu_HPLC1

    African Journals Online (AJOL)

    pc

    HPLC, Gymnema sylvestre, carbohydrate hydrolyzing enzymes, lipid a chronic .... Method. Test for Tannins and Flavonoids was by. Trease and Evans (2002). Soluble Starch ... Fenton reaction was quantified using 2- deoxyribose oxidative ...

  20. Chemometrics-Assisted UV Spectrophotometric and RP-HPLC Methods for the Simultaneous Determination of Tolperisone Hydrochloride and Diclofenac Sodium in their Combined Pharmaceutical Formulation.

    Science.gov (United States)

    Gohel, Nikunj Rameshbhai; Patel, Bhavin Kiritbhai; Parmar, Vijaykumar Kunvarji

    2013-01-01

    Chemometrics-assisted UV spectrophotometric and RP-HPLC methods are presented for the simultaneous determination of tolperisone hydrochloride (TOL) and diclofenac sodium (DIC) from their combined pharmaceutical dosage form. Chemometric methods are based on principal component regression and partial least-square regression models. Two sets of standard mixtures, calibration sets, and validation sets were prepared. Both models were optimized to quantify each drug in the mixture using the information included in the UV absorption spectra of the appropriate solution in the range 241-290 nm with the intervals λ = 1 nm at 50 wavelengths. The optimized models were successfully applied to the simultaneous determination of these drugs in synthetic mixture and pharmaceutical formulation. In addition, an HPLC method was developed using a reversed-phase C18 column at ambient temperature with a mobile phase consisting of methanol:acetonitrile:water (60:30:10 v/v/v), pH-adjusted to 3.0, with UV detection at 275 nm. The methods were validated in terms of linearity, accuracy, precision, sensitivity, specificity, and robustness in the range of 3-30 μg/mL for TOL and 1-10 μg/mL for DIC. The robustness of the HPLC method was tested using an experimental design approach. The developed HPLC method, and the PCR and PLS models were used to determine the amount of TOL and DIC in tablets. The data obtained from the PCR and PLS models were not significantly different from those obtained from the HPLC method at 95% confidence limit.

  1. Determination of the Trans-resveratrol content of Champagne wines by reversed-phase HPLC

    Directory of Open Access Journals (Sweden)

    Philippe Jeandet

    2006-06-01

    Full Text Available Levels of trans-resveratrol in Champagne wines were determined by the use of reversed-phase HPLC with UV and fluorometric detection after liquid-liquid extraction with ethyl acetate. Resveratrol concentrations in Champagne wines range from 20 to 77 μg/L except for the Champagne rosé in which resveratrol reaches several hundred micrograms per litre. The resveratrol content of Champagne wines was also shown to decrease with aging on lees.

  2. Synthesis and mechanical properties of bulk Al{sub 76}Ni{sub 8}Ti{sub 8}Zr{sub 4}Y{sub 4} alloy fabricated by consolidation of mechanically alloyed amorphous powders

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Xinfu; Wang, Kun; Li, Zhendong; Wang, Xingfu; Wang, Dan; Han, Fusheng, E-mail: fshan@issp.ac.cn

    2015-05-25

    Graphical abstract: Different regions indentation morphologies under 50 g load consolidated at 723 K (left), nanohardness of the Al{sub 76}Ni{sub 8}Ti{sub 8}Zr{sub 4}Y{sub 4} alloy as a function consolidation temperature (right). It can be seen from the above figures that the consolidated sample presents white regions, and the microhardness in the white regions is a little lower than the matrix, which could be caused by the difference of the chemical composition and chemical bonding forces between them. Interestingly, the cracks were formed around the indentation periphery in the white regions, which are not shown in the matrix. The nanohardness of the bulk composites increased from 11.16 to 13.27 GPa with the consolidation temperature increasing, mechanical softening was also found in the present alloys. - Highlights: • Bulk amorphous–nanocrystalline Al-based alloys were prepared by HPS process. • The Vickers microhardness of bulk samples is in the range of 945–1177HV0.1. • The nanohardness agrees well with the Vickers hardness testing results. - Abstract: Mechanically alloyed amorphous Al{sub 76}Ni{sub 8}Ti{sub 8}Zr{sub 4}Y{sub 4} (at.%) alloy powder was consolidated by high-pressure sintering process. The influence of the consolidation temperature on the structure and mechanical properties of the consolidated bulk alloys was examined by X-ray diffraction (XRD), Optical microscopy (OM), Scanning electron microscopy (SEM), Vickers Hardness Tester and Nano Indenter. Structural investigations of the bulk materials revealed that most of the amorphous structure was retained after consolidation at 623 K, however, compaction at 723 K and 823 K caused crystallization of the amorphous phase with the appearance of white regions. The results also indicate that application of high pressure affected the crystallization products of the present alloy. Micro mechanical analysis showed that the microhardness of the bulk composites increased from 945HV{sub 0.1} to 1177HV

  3. Solvent optimization on Taxol extraction from Taxus baccata L., using HPLC and LC-MS

    Directory of Open Access Journals (Sweden)

    H Sadeghi-aliabadi

    2009-10-01

    Full Text Available "nBackground and the purpose of the study: Taxol, a natural antitumor agent, was first isolated from the extract of the bark of Taxus brevifolia Nutt., which is potentially a limited source for Taxol. In the search of an alternative source, optimum and cost benefit extracting solvents, various solvents with different percentage were utilized to extract Taxol from needles of Taxus baccata. "nMethods: One g of the dried needles of Taxus baccata, collected from Torkaman and Noor cities of Iran, was extracted with pure ethanol or acetone and 50% and 20% of ethanol or acetone in water. Solvents were evaporated to dryness and the residues were dissolved in 5 ml of methanol and filtered. To one ml of the filtrate was added 50 μl of cinamyl acetate as the internal standard and 20 μl of the resulting solution was subjected to the HPLC to determine the extraction efficiencies of tested solvents. Five μl of filtrate was also subjected to the LC-MS using water/acetonitrile (10/90 as mobile phase and applying positive electrospray ionization (ESI to identify the authenticity of Taxol. "nResults: Results of this study indicated that Taxol extraction efficiency was enhanced as the percentage of ethanol or acetone was increased. HPLC analysis showed that Taxol could be quantified by UV detection using standard curve. The standard curve covering the concentration ranges of 7.8 - 500 μg/ml was linear (r2= 0.9992 and CV% ranged from 0.52 to 15.36. LC-MS analysis using ESI in positive-ion mode confirmed the authenticity of Taxol (m/z 854; M+H, as well as some adduct ions such as M+Na (m/z 876, M+K (m/z 892 and M+CH3CN+H2O (m/z 913. "nConclusions: The results suggest that 100% acetone is the best solvent for the extraction of Taxol from Taxus baccata needles.

  4. Determination of ursolic acid and ursolic acid lactone in the leaves of Eucalyptus tereticornis by HPLC

    International Nuclear Information System (INIS)

    Maurya, Anupam; Srivastava, Santosh Kumar

    2012-01-01

    A simple isocratic HPLC method has been developed for the simultaneous quantification of two bioactive triterpenes, ursolic acid and ursolic acid lactone in E. tereticornis leaves. Samples were analyzed on RP-18 (4.6 x 250 mm, 5 m u m ) column with methanol and water acidified to pH 3.5 with TFA (88:12) at 210 nm. The method was validated and applied for the simultaneous quantification of the individual triterpenes in E. tereticornis extract. The calibration curves were linear over a concentration range of 0.05-0.3 mg mL -1 (r = 0.999 and 0.998, respectively). The limits of detection and quantification were 0.190 and 0.644 μg for ursolic acid, and 0.176 and 0.587 μg for ursolic acid lactone, while the percentage recoveries were 97.32 and 96.23% for ursolic acid and ursolic acid lactone, respectively. This is the first report on the HPLC method of ursolic acid lactone with high precision and accuracy. (author)

  5. Determination of ursolic acid and ursolic acid lactone in the leaves of Eucalyptus tereticornis by HPLC

    Energy Technology Data Exchange (ETDEWEB)

    Maurya, Anupam; Srivastava, Santosh Kumar [Analytical Chemistry Division, Central Institute of Medicinal and Aromatic Plants, Lucknow (India)

    2012-03-15

    A simple isocratic HPLC method has been developed for the simultaneous quantification of two bioactive triterpenes, ursolic acid and ursolic acid lactone in E. tereticornis leaves. Samples were analyzed on RP-18 (4.6 x 250 mm, 5 {sup m}u{sup m}) column with methanol and water acidified to pH 3.5 with TFA (88:12) at 210 nm. The method was validated and applied for the simultaneous quantification of the individual triterpenes in E. tereticornis extract. The calibration curves were linear over a concentration range of 0.05-0.3 mg mL{sup -1} (r = 0.999 and 0.998, respectively). The limits of detection and quantification were 0.190 and 0.644 {mu}g for ursolic acid, and 0.176 and 0.587 {mu}g for ursolic acid lactone, while the percentage recoveries were 97.32 and 96.23% for ursolic acid and ursolic acid lactone, respectively. This is the first report on the HPLC method of ursolic acid lactone with high precision and accuracy. (author)

  6. Breaking bad news: patients' preferences and health locus of control.

    Science.gov (United States)

    Martins, Raquel Gomes; Carvalho, Irene Palmares

    2013-07-01

    To identify patients' preferences for models of communicating bad news and to explore how such preferences, and the reasons for the preferences, relate with personality characteristics, specifically patients' health locus of control (HLC): internal/external and 'powerful others' (PO). Seventy-two patients from an oncology clinic watched videotaped scenarios of a breaking bad news moment, selected the model they preferred, filled an HLC scale and were interviewed about their choices. Data were analyzed with Chi-square, Kruskal-Wallis and Mann-Whitney tests. Interviews were content-analyzed. 77.8% preferred an "empathic professional", 12.5% a "distanced expert" and 9.7% an "emotionally burdened expert". Preferences varied significantly with HLC scores (patients with higher internal locus of control (ILC) and lower PO preferred the empathic model), presence of cancer, age and education. Patients explained their preferences through aspects of Caring, Professionalism, Wording, Time and Hope. ILC registered significant differences in regards to Wording and Time, whereas PO was associated with Hope and Time. HLC is an important dimension that can help doctors to better know their patients. Knowing whether patients attribute their health to their own behaviors or to chance/others can help tailor the disclosure of bad news to their specific preferences. Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

  7. Retinoid quantification by HPLC/MS(n)

    Science.gov (United States)

    McCaffery, Peter; Evans, James; Koul, Omanand; Volpert, Amy; Reid, Kevin; Ullman, M. David

    2002-01-01

    Retinoic acid (RA) mediates most of the biological effects of vitamin A that are essential for vertebrate survival. It acts through binding to receptors that belong to the nuclear receptor transcription factor superfamily (Mangelsdorf et al. 1994). It is also a highly potent vertebrate teratogen. To determine the function and effects of endogenous and exogenous RA, it is important to have a highly specific, sensitive, accurate, and precise analytical procedure. Current analyses of RA and other retinoids are labor intensive, of poor sensitivity, have limited specificity, or require compatibility with RA reporter cell lines (Chen et al. 1995. BIOCHEM: Pharmacol. 50: 1257-1264; Creech Kraft et al. 1994. BIOCHEM: J. 301: 111-119; Lanvers et al. 1996. J. Chromatogr. B Biomed. Appl. 685: 233-240; Maden et al. 1998. DEVELOPMENT: 125: 4133-4144; Wagner et al. 1992. DEVELOPMENT: 116: 55-66). This paper describes an HPLC/mass spectrometry/mass spectrometry product ion scan (HPLC/MS(n)) procedure for the analysis of retinoids that employs atmospheric pressure chemical ionization MS. The retinoids are separated by normal-phase column chromatography with a linear hexane-isopropanol-dioxane gradient. Each retinoid is detected by a unique series of MS(n) functions set at optimal collision-induced dissociation energy (30% to 32%) for all MS(n) steps. The scan events are divided into three segments, based on HPLC elution order, to maximize the mass spectrometer duty cycle. The all-trans, 9-cis, and 13-cis RA isomers are separated, if desired, by an isocratic hexane-dioxane-isopropanol mobile phase. This paper describes an HPLC/MS(n) procedure possessing high sensitivity and specificity for retinoids.

  8. Characterization of bioactive compounds of Annona cherimola L. leaves using a combined approach based on HPLC-ESI-TOF-MS and NMR.

    Science.gov (United States)

    Díaz-de-Cerio, Elixabet; Aguilera-Saez, Luis Manuel; Gómez-Caravaca, Ana María; Verardo, Vito; Fernández-Gutiérrez, Alberto; Fernández, Ignacio; Arráez-Román, David

    2018-06-01

    Annona cherimola Mill. (cherimoya) has widely been used as food crop. The leaves of this tree possess several health benefits, which are, in general, attributed mainly to its bioactive composition. However, literature concerning a comprehensive characterization based on a combined approach, which consists of nuclear magnetic resonance (NMR) and high-performance liquid chromatography coupled with time-of-flight mass spectrometry (HPLC-TOF-MS), from these leaves is scarce. Thus, the aim of this work was to study the polar profile of full extracts of cherimoya leaves by using these tools. Thus, a total of 77 compounds have been characterized, 12 of which were identified by both techniques. Briefly, 23 compounds were classified as amino acids, organic acids, carbohydrates, cholines, phenolic acid derivatives, and flavonoids by NMR, while 66 metabolites were divided into sugars, amino acids, phenolic acids and derivatives, flavonoids, phenylpropanoids, and other polar compounds by HPLC-TOF-MS. It is worth mentioning that different solvent mixtures were tested and the total phenolic content in the extracts quantified (TPC via HPLC-TOF-MS). The tendency observed was EtOH/water 80/20 (v/v) (17.0 ± 0.2 mg TPC/g leaf dry weight (d.w.)) ≥ acetone/water 70/30 (v/v) (16.1 ± 0.7 mg TPC/g leaf d.w.) > EtOH/water 70/30 (v/v) (14.0 ± 0.3 mg TPC/g leaf d.w.) > acetone/water 80/20 (v/v) (13.5 ± 0.4 mg TPC/g leaf d.w.). Importantly, flavonoids derivatives were between 63 and 76% of the TPC in those extracts. Major compounds were sucrose, glucose (α and β), and proline, and chlorogenic acid and rutin for NMR and HPLC-TOF-MS, respectively. Graphical abstract The combined use of LC-HRMS and NMR is a potential synergic combination for a comprehensive metabolite composition of cherimoya leaves.

  9. HPLC/MS analysis of glucose and fluorodeoxyglucose

    International Nuclear Information System (INIS)

    Bruder, P.; Macasek, F.; Patakyova, A.; Buriova, E.

    2001-01-01

    Objective of a new method of FDG analysis development is to replace existing tests by a more complex assay. In this work, a liquid chromatography/refractive index detector/ radiometric detector/mass spectrometric detector combination (HPLC/RID/RAD/MSD) was used for development of a complex routine technique. Optimization of HPLC/MS analysis was performed investigating the MSD analytical signal as a function of various eluent composition. Solutions of glucose in methanol/water and acetonitrile/water solutions of various semi-volatile electrolytes (ammonium chloride, formic acid, ammonium formate) were analyzed on the Agilent 1100 HPLC/RID/DAD/MSD system either in the flow injection (FIA) mode of analysis, and after passing the samples through Zorbax C-18 column. The most intensive signals of the ions were obtained in the acetonitrile : 0.25% ammonium formate = 80:20 solutions. This eluent would be also used for the radioactive FDG analysis on the Asahipak NH2P columns. (authors)

  10. HPLC/MS analysis of glucose and fluorodeoxyglucose

    Energy Technology Data Exchange (ETDEWEB)

    Bruder, P; Macasek, F; Patakyova, A; Buriova, E [Department of Nuclear Chemistry, Faculty of Natural Sciences, Comenius University, 84215 Bratislava (Slovakia)

    2001-05-31

    Objective of a new method of FDG analysis development is to replace existing tests by a more complex assay. In this work, a liquid chromatography/refractive index detector/ radiometric detector/mass spectrometric detector combination (HPLC/RID/RAD/MSD) was used for development of a complex routine technique. Optimization of HPLC/MS analysis was performed investigating the MSD analytical signal as a function of various eluent composition. Solutions of glucose in methanol/water and acetonitrile/water solutions of various semi-volatile electrolytes (ammonium chloride, formic acid, ammonium formate) were analyzed on the Agilent 1100 HPLC/RID/DAD/MSD system either in the flow injection (FIA) mode of analysis, and after passing the samples through Zorbax C-18 column. The most intensive signals of the ions were obtained in the acetonitrile : 0.25% ammonium formate = 80:20 solutions. This eluent would be also used for the radioactive FDG analysis on the Asahipak NH2P columns. (authors)

  11. Pharmacological Targeting Of Neuronal Kv7.2/3 Channels: A Focus On Chemotypes And Receptor Sites.

    Science.gov (United States)

    Miceli, Francesco; Soldovieri, Maria Virginia; Ambrosino, Paolo; Manocchio, Laura; Medoro, Alessandro; Mosca, Ilaria; Taglialatela, Maurizio

    2017-10-12

    The Kv7 (KCNQ) subfamily of voltage-gated potassium channels consists of 5 members (Kv7.1-5) each showing a characteristic tissue distribution and physiological roles. Given their functional heterogeneity, Kv7 channels represent important pharmacological targets for development of new drugs for neuronal, cardiac and metabolic diseases. In the present manuscript, we focus on describing the pharmacological relevance and the potential therapeutic applications of drugs acting on neuronally-expressed Kv7.2/3 channels, placing particular emphasis on the different modulator chemotypes, and highlighting their pharmacodynamic and, whenever possible, pharmacokinetic peculiarities. The present work is based on an in-depth search of the currently available scientific literature, and on our own experience and knowledge in the field of neuronal Kv7 channel pharmacology. Space limitations impeded to describe the full pharmacological potential of Kv7 channels; thus, we have chosen to focus on neuronal channels composed of Kv7.2 and Kv7.3 subunits, and to mainly concentrate on their involvement in epilepsy. An astonishing heterogeneity in the molecular scaffolds exploitable to develop Kv7.2/3 modulators is evident, with important structural/functional peculiarities of distinct compound classes. In the present work we have attempted to show the current status and growing potential of the Kv7 pharmacology field. We anticipate a bright future for the field, and we express our hopes that the efforts herein reviewed will result in an improved treatment of hyperexcitability (or any other) diseases. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

  12. The cytology, isozyme, HPLC fingerprint, and interspecific hybridization studies of genus epimedium (berberidaceae).

    Science.gov (United States)

    Wang, Lin-Jiao; Sheng, Mao-Yin

    2013-01-01

    104 samples from 27 accessions belonging to 12 species of genus Epimedium were studied on the basis of cytology observation, POD (i.e., peroxide) isozyme, high performance liquid chromatography (i.e., HPLC) fingerprint, and interspecific hybridization. The cytology observation showed karyotypes of twelve species studied; all are 2A symmetry type of Stebbins standard and similar to each other, and except for karyotype of E. leptorrhizum which is 2n = 2x = 8m (2SAT) + 4sm, the rest are 2n = 2x = 6m (2SAT) + 6sm. Chromosomes C-banding of barrenwort species varies, with 15 to 22 bands, consisting of centromeric bands, intercalary bands, terminal bands, and middle satellite bands. Results of POD isozyme showed that the zymographs vary greatly and sixteen bands were detected in the eleven species, and each species has its own characteristic bands different from the others. Studies on the HPLC fingerprint showed that the HPLC fingerprint of different species has characteristic peaks, divided into two regions (retention time 10 min). Results of interspecific hybridization showed that crosses of any combination among seven species studied are successful and the rates of grain set vary greatly. Based on these results, the system and phylogeny of this genus were inferred.

  13. Reverse-phase HPLC analysis of human alpha crystallin.

    Science.gov (United States)

    Swamy, M S; Abraham, E C

    1991-03-01

    A rapid and highly sensitive reverse-phase HPLC (RP-HPLC) method was used to separate crystallin subunits from human alpha crystallin. Three distinct peaks were separated; by electrophoretic and immunological analyses the first and second peaks were identified as alpha B and alpha A respectively. On the other hand, peak 3 appeared to be a modified form of alpha crystallin. The ratio of alpha A and alpha B proteins was 3:1 in 1 day old lenses which gradually changed to 2:1 in 17 year old lenses and to 1:1 in the 50 and 82 year old whole lenses and 82 year old lens cortex, with a concomitant increase in the modified alpha, suggesting that alpha A subunits are relatively more involved in aggregation. Analysis of the 82 year old lens nucleus also supported this conclusion. The RP-HPLC analysis of the HMW aggregate fraction showed substantial enrichment of the modified alpha. The alpha A and alpha B subunits independently reassociated to form polymeric alpha crystallin whereas the modified alpha reassociated to form HMW aggregates as shown by molecular sieve HPLC. Hence it appears that the HMW aggregate peak was constituted by modified alpha crystallin. Only in the peak 3 material the 280 nm absorbance was about 2-fold higher than what was expected from the actual protein content. The data suggest that the changes induced by post-translational modifications may have some role in the formation of modified alpha. The present RP-HPLC method is useful in separating these modified alpha from the unmodified alpha A and alpha B subunits.

  14. Enrichment of steroid hormones in water with porous and hydrophobic polymer-based SPE followed by HPLC-UV determination.

    Science.gov (United States)

    Hu, Yinfen; Zhang, Man; Tong, Changlun; Wu, Jianmin; Liu, Weiping

    2013-10-01

    There have been great concerns about the persistence of steroid hormones in surface water. Since the concentrations of these compounds in water samples are usually at a trace level, the efficient enrichment of steroid hormones is vital for further analysis. In this work, a porous and hydrophobic polymer was synthesized and characterized. The composition of solvent used as porogen in the synthetic process was shown to have an effect on the morphology of the polymer, which was successfully used as an SPE sorbent for simultaneously enriching steroid hormones in surface water samples. The recoveries of the steroid hormones on the custom-made polymer ranged from 93.4 to 106.2%, whereas those on commercialized ENVI-18, LC-18, and Oasis HLB ranged from 54.8 to 104.9, 66 to 93.6, and 77.2 to 106%, respectively. Five types of steroid hormones were simultaneously measured using HPLC-UV after they were enriched by the custom-made sorbent. Based on these findings, the SPE-HPLC method was developed. The LODs of this method for estriol, estradiol, estrone, androstenedione, progesterone were 0.07, 0.43, 0.61, 0.27, and 0.42 μg/L, respectively, while precision and reproducibility RSDs were <6.40 and 7.49%, respectively. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Optimizing Chromatographic Separation: An Experiment Using an HPLC Simulator

    Science.gov (United States)

    Shalliker, R. A.; Kayillo, S.; Dennis, G. R.

    2008-01-01

    Optimization of a chromatographic separation within the time constraints of a laboratory session is practically impossible. However, by employing a HPLC simulator, experiments can be designed that allow students to develop an appreciation of the complexities involved in optimization procedures. In the present exercise, a HPLC simulator from "JCE…

  16. Extreme Anemia (Hemoglobin 1.8g/dL Secondary to Abnormal Uterine Bleeding

    Directory of Open Access Journals (Sweden)

    Ketaki Panse

    2017-01-01

    Full Text Available We present the case of a 39-year-old G5P5 woman who presented to the emergency department with complaints of shortness of breath, lightheadedness, and excessive uterine bleeding for 14 days, with a heart rate of 123 and a blood pressure of 137/65. Menses had been heavy for several months. A hemoglobin of 1.8g/dL was discovered. An ultrasound revealed an 11.8 cm fibroid uterus, and the patient was transfused with 6 units of blood and placed on oral contraceptive pills.

  17. A new affinity-HPLC packing for protein separation: Cibacron blue attached uniform porous poly(HEMA-co-EDM) beads.

    Science.gov (United States)

    Unsal, Ender; Durdu, Aysun; Elmas, Begum; Tuncel, Murvet; Tuncel, Ali

    2005-11-01

    In this study, a new affinity high-performance liquid chromatography (HPLC) stationary phase suitable for protein separation was synthesized. In the first stage of the synthesis, uniform porous poly(2-hydroxyethyl methacrylate-co-ethylene dimethacrylate), poly(HEMA-co-EDM), beads 6.2 mum in size were obtained. Homogeneous distribution of hydroxyl groups in the bead interior was confirmed by confocal laser scanning microscopy. The plain poly(HEMA-co-EDM) particles gave very low non-specific protein adsorption with albumin. The selected dye ligand Cibacron blue F3G-A (CB F3G-A) was covalently linked onto the beads via hydroxyl groups. In the batch experiments, albumin adsorption up to 60 mg BSA/g particles was obtained with the CB F3G-A carrying poly(HEMA-co-EDM) beads. The affinity-HPLC of selected proteins (albumin and lysozyme) was investigated in a 25 mm x 4.0-mm inner diameter column packed with CB F3G-A carrying beads and both proteins were successfully resolved. By a single injection, 200 mug of protein was loaded and quantitatively eluted from the column. The protein recovery increased with increasing flow rate and salt concentration of the elution buffer and decreased with the increasing protein feed concentration. During the albumin elution, theoretical plate numbers up to 30,000 plates/m were achieved by increasing the salt concentration.

  18. Carbon dioxide baited trap catches do not correlate with human landing collections of Anopheles aquasalis in Suriname

    Directory of Open Access Journals (Sweden)

    Hélène Hiwat

    2011-05-01

    Full Text Available Three types of carbon dioxide-baited traps, i.e., the Centers for Disease Control Miniature Light Trap without light, the BioGents (BG Sentinel Mosquito Trap (BG-Sentinel and the Mosquito Magnet® Liberty Plus were compared with human landing collections in their efficiency in collecting Anopheles (Nyssorhynchus aquasalis mosquitoes. Of 13,549 total mosquitoes collected, 1,019 (7.52% were An. aquasalis. Large numbers of Culex spp were also collected, in particular with the (BG-Sentinel. The majority of An. aquasalis (83.8% were collected by the human landing collection (HLC. None of the trap catches correlated with HLC in the number of An. aquasalis captured over time. The high efficiency of the HLC method indicates that this malaria vector was anthropophilic at this site, especially as carbon dioxide was insufficiently attractive as stand-alone bait. Traps using carbon dioxide in combination with human odorants may provide better results.

  19. Development of a new rapid HPLC method for the fractionation of histones

    International Nuclear Information System (INIS)

    Gurley, L.R.; Valdez, J.G.; Prentice, D.A.; Spall, W.D.

    1983-01-01

    To study histone functions, it is necessary to fractionate the histones into their five classes (H1, H2A, H2B, H3 and H4) and then to subfractionate these classes into variants having slightly different primary structures and into different phosphorylated and acetylated forms. With the advent of high-performance liquid chromatography (HPLC), it was hoped that laborious and time-consuming conventional methods could be replaced by a simple, rapid, high-resolving HPLC method for fractionating histones. However, problems of irreversible adsorption of the histones to HPLC column packings discouraged this development. Our laboratory has now determined that the strong adsorption of histones to HPLC columns results from two different forces: (1) polar interactions between the histones and the silanol groups of silica-based HPLC column packing, and (2) hydrophobic interactions between the histones and the bound organic phase of the column packings. By minimizing these forces, we have succeeded in developing an HPLC method suitable for histone studies

  20. Determination of Two Sulfonylurea Herbicides Residues in Soil Environment Using HPLC and Phytotoxicity of These Herbicides by Lentil Bioassay.

    Science.gov (United States)

    Mehdizadeh, Mohammad; Alebrahim, Mohammad Taghi; Roushani, Mahmoud

    2017-07-01

    A HPLC-UV detection system was used for determination of sulfosulfuron and tribenuron methyl residues from soils. The soils were fortified with sulfosulfuron and tribenuron methyl at rates of 26 and 15 g a.i. ha -1 respectively and samples were taken randomly on 0 (2 h), 1, 2, 4, 10, 20, 40, 60, 90 and 120 days after treatment. The final extracts were prepared for analysis by HPLC. The results showed that degradation of both herbicides in the silty loam soil was faster than sandy loam soil. Half-life of sulfosulfuron was ranged from 5.37 to 10.82 days however this value for tribenuron methyl was ranged from 3.23 to 5.72 days on different soils. The residue of both herbicides at 120 days after application in wheat field had no toxicitic effect on lentil. It was concluded that HPLC analysis procedure was an appropriate method for determination of these herbicides from soils.

  1. Determination of fructooligosaccharides in burdock using HPLC and microwave-assisted extraction.

    Science.gov (United States)

    Li, Jing; Liu, Xiaomei; Zhou, Bin; Zhao, Jing; Li, Shaoping

    2013-06-19

    The root of burdock ( Arctium lappa L.) is a commonly used vegetable in Asia. Fructooligosaccharides (FOS) are usually considered as its main bioactive components. Thus, quantitative analysis of these components is very important for the quality control of burdock. In this study, an HPLC-ELSD and microwave-assisted extraction method was developed for the simultaneous determination of seven FOS with degrees of polymerization (DP) between 3 and 9, as well as fructose, glucose, and sucrose in burdock from different regions. The separation was performed on a Waters XBridge Amide column (4.6 × 250 mm i.d., 3.5 μm) with gradient elution. All calibration curves for investigated analytes showed good linear regression (r > 0.9990). Their LODs and LOQs were lower than 3.63 and 24.82 μg/mL, respectively. The recoveries ranged from 99.2 to 102.6%. The developed method was successfully applied to determination of ten sugars in burdock from different locations of Asia. The results showed that the contents of FOS in different samples of burdock collected at appropriate times were similar, and the developed HPLC-ELSD with microwave-assisted extraction method is helpful to control the quality of burdock.

  2. Moskva ja Lääs enne Peterburi G-8 tippkohtumist / Urmas Kiil

    Index Scriptorium Estoniae

    Kiil, Urmas

    2006-01-01

    Hiljuti avalikustatud ettekannet Engaging with Russia - the Next Phase (Koostöö Venemaaga - järgmine etapp) võib pidada Venemaa ja lääneriikide suhete külmenemise mastaapseks kroonikaks ja see teeb problemaatiliseks Venemaa edaspidise osalemise G-8 seltskonnas

  3. Chromatographic Analysis of a Multicomponent Mixture of B1, B6, B12, Benfotiamine, and Diclofenac; Part I: HPLC and UPLC Methods for the Simultaneous Quantification of These Five Components in Tablets and Capsules.

    Science.gov (United States)

    Fayed, Ahmed Salah; Hegazy, Maha Abdel-Monem; Wahab, Nada Sayed Abdel

    2016-11-01

    New, simple, highly sensitive, precise, and accurate gradient reversed-phase chromatographic methods were developed using HPLC and ultra-HPLC (UPLC) systems for the determination of five components, namely thiamine, pyridoxine, cyanocobalamin, benfotiamine, and diclofenac in tablets and capsules. The methods were compared for their efficiency in the separation and determination of these five compounds using two different C18 columns (250 × 4.6 mm, 5 μm; and 100 × 4.6 mm, 2.6 μm) for HPLC and UPLC, respectively. Chromatographic separation was performed with a mobile phase containing acetonitrile and 0.025 M phosphate buffer (pH 3.5), with a gradient program and a flow rate of 1.5 and 1.0 mL/min for both methods, respectively. The methods were validated according to International Conference on Harmonization guidelines. Linearity was achieved in the range of 5.00 to 150.00 μg/mL for each of the five compounds. Ruggedness and intermediate precision were confirmed by different analysts on different columns on different days. Moreover, the components were subjected to an accelerated stability study under acidic, alkaline, and oxidative stress conditions and no interfering peaks were observed. The five compounds were efficiently separated in <20 min by HPLC, whereas for UPLC, separation was achieved in <8 min, which dramatically decreased the consumption of organic solvents.

  4. Magnetic molecularly imprinted polymer nanoparticles for the solid-phase extraction of paracetamole from plasma samples, followed its determination by HPLC

    International Nuclear Information System (INIS)

    Azodi-Deilami, Saman; Najafabadi, Alireza Hassani; Asadi, Ebadullah; Abdouss, Majid; Kordestani, Davood

    2014-01-01

    We are presenting magnetic molecularly imprinted polymer nanoparticles (m-MIPs) for solid-phase extraction and sample clean-up of paracetamole. The m-MIPs were prepared from magnetite (Fe 3 O 4 ) as the magnetic component, paracetamole as the template, methacrylic acid as a functional monomer, and 2-(methacrylamido) ethyl methacrylate as a cross-linker. The m-MIPs were then characterized by transmission electron microscopy, FT-IR spectroscopy, X-ray diffraction and vibrating sample magnetometry. The m-MIPs were applied to the extraction of paracetamole from human blood plasma samples. Following its elution from the column loaded with the m-MIPs with an acetonitrile-buffer (9:1) mixture, it was submitted to HPLC analysis. Paracetamole can be quantified by this method in the 1 μg L −1 to 300 μg L −1 concentration range. The limit of detection and limit of quantification in plasma samples are 0.17 and 0.4 μg L −1 . The preconcentration factor of the m-MIPs is 40. The HPLC method shows good precision (4.5 % at 50 μg L −1 levels) and recoveries (between 83 and 91 %) from spiked plasma samples. (author)

  5. Methods and applications of HPLC-AMS (WBio 5)

    International Nuclear Information System (INIS)

    Bucholz, B A; Clifford, A J; Duecker, S R; Lin, Y; Vogel, J S

    1999-01-01

    Pharmacokinetics of physiologic doses of nutrients, pesticides, and herbicides can easily be traced in humans using a(sup 14)C-labelled compound. Basic kinetics can be monitored in blood or urine by measuring the elevation in the(sup 14)C content above the control predose tissue and converting to equivalents of the parent compound. High Performance Liquid Chromatography (HPLC) is an excellent method for the chemical separation of complex mixtures whose profiles afford estimation of biochemical pathways of metabolism. Compounds elute from the HPLC systems with characteristic retention times and can be collected in fractions that can then be graphitized for AMS measurement. Unknowns are identified by coelution with known standards and chemical tests that reveal functional groupings. Metabolites are quantified with the(sup 14)C signal. Thoroughly accounting for the carbon inventory in the LC solvents, ion-pairing agents, samples, and carriers adds some complexity to the analysis. In most cases the total carbon inventory is dominated by carrier. Baseline background and stability need to be carefully monitored. Limits of quantitation near 10 amol of(sup 14)C per HPLC fraction are typically achieved. Baselines are maintained by limiting injected(sup 14)C activity and lt;0.17 Bq (4.5 pCi) on the HPLC column

  6. FERMI LARGE AREA TELESCOPE OBSERVATIONS OF THE SUPERNOVA REMNANT G8.7–0.1

    International Nuclear Information System (INIS)

    Ajello, M.; Allafort, A.; Bechtol, K.; Berenji, B.; Blandford, R. D.; Bloom, E. D.; Borgland, A. W.; Buehler, R.; Cameron, R. A.; Baldini, L.; Bellazzini, R.; Bregeon, J.; Ballet, J.; Barbiellini, G.; Bastieri, D.; Buson, S.; Bonamente, E.; Brigida, M.; Bruel, P.; Caliandro, G. A.

    2012-01-01

    We present a detailed analysis of the GeV gamma-ray emission toward the supernova remnant (SNR) G8.7–0.1 with the Large Area Telescope (LAT) on board the Fermi Gamma-ray Space Telescope. An investigation of the relationship between G8.7–0.1 and the TeV unidentified source HESS J1804–216 provides us with an important clue on diffusion process of cosmic rays if particle acceleration operates in the SNR. The GeV gamma-ray emission is extended with most of the emission in positional coincidence with the SNR G8.7–0.1 and a lesser part located outside the western boundary of G8.7–0.1. The region of the gamma-ray emission overlaps spatially connected molecular clouds, implying a physical connection for the gamma-ray structure. The total gamma-ray spectrum measured with LAT from 200 MeV-100 GeV can be described by a broken power-law function with a break of 2.4 ± 0.6 (stat) ± 1.2 (sys) GeV, and photon indices of 2.10 ± 0.06 (stat) ± 0.10 (sys) below the break and 2.70 ± 0.12 (stat) ± 0.14 (sys) above the break. Given the spatial association among the gamma rays, the radio emission of G8.7–0.1, and the molecular clouds, the decay of π 0 s produced by particles accelerated in the SNR and hitting the molecular clouds naturally explains the GeV gamma-ray spectrum. We also find that the GeV morphology is not well represented by the TeV emission from HESS J1804–216 and that the spectrum in the GeV band is not consistent with the extrapolation of the TeV gamma-ray spectrum. The spectral index of the TeV emission is consistent with the particle spectral index predicted by a theory that assumes energy-dependent diffusion of particles accelerated in an SNR. We discuss the possibility that the TeV spectrum originates from the interaction of particles accelerated in G8.7–0.1 with molecular clouds, and we constrain the diffusion coefficient of the particles.

  7. Assessment of radiochemical purity of [18F]fludeoxyglucose by high pressure liquid chromatography (HPLC)

    International Nuclear Information System (INIS)

    Lacerda, Aline E.; Silva, Juliana B.; Silveira, Marina B.; Ferreira, Soraya Z.

    2011-01-01

    The quality control of [ 18 F]fludeoxyglucose ( 18 FDG) has received attention due to its increasing clinical use. Although the quality requirements of 18 FDG are established in various pharmacopoeia, the suitability of all testing methods used should be verified under actual conditions of use and documented. The aim of this study was to develop a high pressure liquid chromatography (HPLC) method for radiochemical purity evaluation of 18 FDG, based on pharmacopoeia references, and to verify its suitability for routine quality control in our centre. HPLC analysis was performed with an Agilent HPLC. 18 FDG and impurities were separated on an anion-exchange column by isocratic elution with 0.1 M NaOH as the mobile phase. Detection was accomplished with refractive index and NaI (Tl) scintillation detectors. The flow rate of the mobile phase was set at 0.8 mL/min and the column temperature was kept at 35 deg C. Specificity, linearity, precision and robustness were assessed to verify if the method was adequate for its intended purpose. Retention time of 18 FDG was not affected by the presence of other components of the formulation and a good peak resolution was achieved. The analytical curve of 18 FDG was linear, with a correlation coefficient value of 0.9995. Intraday repeatable precision, reported as the relative standard deviation, was 0.11%. Analytical procedure remained unaffected by small variations in mobile phase flow rate. Results evidenced that HPLC is suitable for radiochemical purity evaluation of 18 FDG, considering operational conditions of our laboratory. (author)

  8. Thermal Performance Characterization using Time Series Data - IEA EBC Annex 58 Guidelines

    DEFF Research Database (Denmark)

    Madsen, Henrik; Bacher, Peder; Bauwens, Geert

    -dynamical) steady state models where the parameters are found using classical methods for linear regression. Such steady state techniques provide sub-optimal use of the information embedded in the data and provides information only about the HLC and gA-values. Next the guidelines consider dynamical models. Firstly......, linear input-output models are considered. More specifically we will consider the class of AutoRegressive with eXogenous input (ARX) (p) models. These models provides information about the HLC and gA-values, and information about the dynamics (most frequently described as time-constants for the system......This document presents guidelines for using time series analysis methods, models and tools for estimating the thermal performance of buildings and building components. The thermal performance is measured as estimated parameters of a model, or parameters derived from estimated parameters of a model...

  9. Identification and evaluation of radiolysis products of irradiated chloramphenicol by HPLC-MS and HPLC-DAD

    Energy Technology Data Exchange (ETDEWEB)

    Hong, L; Altorfer, H R [Institute of Pharmaceutical Science, Swiss Federal Institute of Technology (ETH), Zurich (Switzerland); Horni, A; Hesse, M [Institute of Organic Chemistry, University of Zurich, Zurich (Switzerland)

    2005-07-01

    The radiolysis products of chloramphenicol under {gamma}-radiation sterilization were investigated systematically in the present study. Eight main radiolysis products were identified and quantified by HPLC-MS and HPLC-DAD, including two compounds that have never been reported. The minor radiolysis products were quantified, which shows that they are at the concentration levels below the threshold for identification. Carbon-carbon rupture reaction and oxidation reaction were proposed as the main radiolysis reactions of chloramphenicol powder. The applicability of {gamma}-sterilization for chloramphenicol products was quantitatively evaluated with qualitative and quantitative data and the data were compared to the threshold requirements of international regulations for identification. It was concluded that toxicities of the radiolysis products of chloramphenicol produced by {gamma}-radiation sterilization can be neglected, the radiolysis products are safe for human health from chemical view. (author)

  10. Identification and evaluation of radiolysis products of irradiated chloramphenicol by HPLC-MS and HPLC-DAD

    International Nuclear Information System (INIS)

    Hong, L.; Altorfer, H.R.; Horni, A.; Hesse, M.

    2005-01-01

    The radiolysis products of chloramphenicol under γ-radiation sterilization were investigated systematically in the present study. Eight main radiolysis products were identified and quantified by HPLC-MS and HPLC-DAD, including two compounds that have never been reported. The minor radiolysis products were quantified, which shows that they are at the concentration levels below the threshold for identification. Carbon-carbon rupture reaction and oxidation reaction were proposed as the main radiolysis reactions of chloramphenicol powder. The applicability of γ-sterilization for chloramphenicol products was quantitatively evaluated with qualitative and quantitative data and the data were compared to the threshold requirements of international regulations for identification. It was concluded that toxicities of the radiolysis products of chloramphenicol produced by γ-radiation sterilization can be neglected, the radiolysis products are safe for human health from chemical view. (author)

  11. Line-Shape Code Comparison through Modeling and Fitting of Experimental Spectra of the C ii 723-nm Line Emitted by the Ablation Cloud of a Carbon Pellet

    Directory of Open Access Journals (Sweden)

    Mohammed Koubiti

    2014-07-01

    Full Text Available Various codes of line-shape modeling are compared to each other through the profile of the C ii 723-nm line for typical plasma conditions encountered in the ablation clouds of carbon pellets, injected in magnetic fusion devices. Calculations were performed for a single electron density of 1017 cm−3 and two plasma temperatures (T = 2 and 4 eV. Ion and electron temperatures were assumed to be equal (Te = Ti = T. The magnetic field, B, was set equal to either to zero or 4 T. Comparisons between the line-shape modeling codes and two experimental spectra of the C ii 723-nm line, measured perpendicularly to the B-field in the Large Helical Device (LHD using linear polarizers, are also discussed.

  12. [Study on the fingerprint of Morus alba from different habitats by HPLC].

    Science.gov (United States)

    Chen, Cheng; Li, Hong-Bo; Wang, Liu-Ping; Li, Yun-Rong; Xin, Ning

    2012-12-01

    To establish HPLC fingerprint of Morus alba from different habitats by HPLC and provide basis for its quality control. HPLC analysis was performed on an Agilent XDB C18 Column (4.6 mm x 250 mm, 5 microm), gradient eluted composed of acetonitrile and 0.3% phosphate acid. The column temperature was set at 35 degrees C and the flow rate was 0.5 mL/min. The detective wavelength was 290 nm. The HPLC fingerprint for 10 batches of Morus alba was studied on their similarity. There were twelve common peaks in the fingerprint. The similarity of 7 batches was above 0.9 and the other batches had low similarity. The HPLC fingerprint can be used for quality control of Morus alba with high characteristics and specificity.

  13. Relevance of G8 scale in referring elderly patients with aortic stenosis requiring a TAVI for a geriatric consultation.

    Science.gov (United States)

    de Thézy, Albane; Lafargue, Aurélie; d'Arailh, Lydie; Dijos, Marina; Leroux, Lionel; Salles, Nathalie; Rainfray, Muriel

    2017-12-01

    Aortic stenosis (AS) may soon become a significant public health issue. Referring elderly suffering from aortic stenosis for a transcatheter aortic valve implantation (TAVI) versus surgical valve replacement might be difficult and requires a multidisciplinary staff. G8 is a geriatric screening scale for frailty, validated in oncogeriatry. We study sensibility and specificity of G8 used by cardiologists in comparison to a comprehensive geriatric assessment (CGA) performed by geriatrician. Prospective study, from February to July 2015, in Bordeaux university Hospital, France. Every elderly admitted for a TAVI had a G8 scale performed by cardiologist and CGA by a geriatrician in blind. Comorbidities were assessed using Cumulative Illness Rating Scale in his geriatric version (CIRS-G). CGA was abnormal if: MMSE value in comparison to gold-standard CGA. 49 patients were included (55.1% women, mean age 84.8 years old). Nearly half of the patients (48.96%) had multiple comorbidities (CIRS G score >3 for at least three items excluding the cardiology item). 38 CGA were abnormal (77.55%) and 41 G8 (83.67%). G8 had a sensibility of 100% (IC 95% [0.9-1]), a specificity of 72.7% (IC 95% [0.43-0.9]), a positive predictive value of 92.6% and a negative prospective value of 100% (IC: 95%). G8 scale seems to be an efficient geriatric screening tool for frailty in elderly undergoing TAVI in comparison to CGA. Simple and useful, G8 scale could be performed by cardiologists in older patients with AS for identifying patients with a geriatric risk profile in consultation before surgery. Further studies with bigger samples are needed to confirm these results.

  14. Development and Validation of a HPLC Method for the Determination of Lacidipine in Pure Form and in Pharmaceutical Dosage Form

    International Nuclear Information System (INIS)

    Vinodh, M.; Vinayak, M.; Rahul, K.; Pankaj, P.

    2012-01-01

    A simple and reliable high-performance liquid chromatography (HPLC) method was developed and validated for Lacidipine in pure form and pharmaceutical dosage form. The method was developed on X bridge C-18 column (150 mm x 4.6 mm, 5 μm) with a mobile phase gradient system of ammonium acetate and acetonitrile. The effluent was monitored by PDA detector at 240 nm. Calibration curve was linear over the concentration range of 50-250 μg/ml. For Intra-day and inter-day precision % RSD values were found to be 0.83 % and 0.41 % respectively. Recovery of Lacidipine was found to be in the range of 99.78-101.76 %. The limits of detection (LOD) and quantification (LOQ) were 1.0 and 7.3 μg/ml respectively. The developed RP-HPLC method was successfully applied for the quantitative determination of lacidipine in pharmaceutical dosage. (author)

  15. Xanthophylls in commercial egg yolks: quantification and identification by HPLC and LC-(APCI)MS using a C30 phase.

    Science.gov (United States)

    Schlatterer, Jörg; Breithaupt, Dietmar E

    2006-03-22

    The xanthophylls lutein and zeaxanthin have attracted a lot of interest since it was presumed that an increased nutritional uptake may prevent adult macula degeneration (AMD). Although egg yolks serve as an important dietary source of lutein and zeaxanthin, data on xanthophyll concentrations in commercial egg yolks are not available. Thus, an high-performance liquid chromatography-diode array detector (HPLC-DAD) method was developed allowing for simultaneous separation of eight xanthophylls used to fortify poultry feed. Peak identification was carried out by liquid chromatography-atmospheric pressure chemical ionization mass spectrometry [LC-(APCI)MS]. Egg yolks of four types of husbandry (seven batches each) were examined. Lutein and zeaxanthin were the predominant xanthophylls in egg yolks produced in accordance with ecological husbandry (class 0) because the concentrations of these xanthophylls ranged from 1274 to 2478 microg/100 g and from 775 to 1288 microg/100 g, respectively. Analysis of variance (ANOVA) proved that both mean lutein and mean zeaxanthin concentrations of eggs from class 0 were statistically discriminable from mean lutein and zeaxanthin concentrations from eggs of all other classes (P xanthophylls in eggs of classes 1 (free range), 2 (barn), and 3 (cage) were as follows: canthaxanthin, 707 +/- 284 microg/100 g; beta-apo-8'-carotenoic acid ethyl ester, 639 +/- 391 microg/100 g; and citranaxanthin, 560 +/- 231 microg/100 g. Experiments with boiled eggs proved that beta-apo-8'-carotenoic acid ethyl ester was the xanthophyll with the highest stability, whereas lutein was degraded to the largest extent (loss of 19%). Detailed knowledge about the xanthophyll amounts in eggs is indispensable to calculate the human uptake.

  16. HPLC-MS technique in radiopharmaceutical research (the quality control of 18F-2-fluorodeoxyglucose as an example)

    International Nuclear Information System (INIS)

    Macasek, F.

    2001-01-01

    Application of radiopharmaceuticals puts increasing demands on their quality control, considering the short half-times, high specific activities (auto-radiolytic effects), and general quality (chemical purity, apyrogenity and sterility) of pharmacy. Mostly, the radioanalytical control consists of application of several separation and instrumental analytical techniques. In this paper, perspective of the hyphenated HPLC and MS techniques is demonstrated on the example of one of the most spread radiopharmaceutical, 2-[ 18 F]fluoro-2-deoxy-D-glucose (further as FDG). In this work, a liquid chromatography/refractive index detector/radiometric detector/mass spectrometric detector combination (HPLC/RID/RAD/MSD) was used for development of a complex routine technique. Optimization of HPLC/MS analysis was performed investigating the electrospray ionization (ESI) analytical signal of mass spectrometer as a function of various eluent composition (see this book, p. 39). Some results, illustrating the glucose and FDG ESI-MS, and also composition of FDG after autoradiolysis, which were obtained either by a TOF Mariner (Perkin Elmer) mass-spectrometer and Agilent 1100 HPLC-MS equipment with quadrupole MS detector are discussed. They give evidence of admixtures and radiolytic formation of deoxyglucose, deoxychloroglucose, erythrose, erytritol, gluconic acid, lactose, raffinose, saccharic acid, sorbitol/[ 19 F]FDG, xylitol, and also univalent ions of C 6 H 10 O 7 F.H 2 O and C 6 H 12 O 8 compounds. The results indicate that the emerging demands on radiopharmaceuticals quality control can be fulfilled in-time only by the radio-HPLC technique developed by the help of a tandem mass-spectrometric detector. (authors)

  17. Separation and identification of beta-carotene and its cis isomers by high pressure liquid chromatography (HPLC); Separacion e identificacion del beta-caroteno y sus isomeros cis por cromatografia liquida de alta resolucion (HPLC)

    Energy Technology Data Exchange (ETDEWEB)

    Carrillo de Padilla, F [Universidad Central de Venezuela (UCV), Facultad de Farmacia, Catedra de Analisis de Alimentos, Caracas (Venezuela)

    1996-07-01

    The separation and identification by HPLC of the cis isomers of beta-carotene was studied. A 1.26 mg/ml beta-carotene solution previously isomerized with iodine as a catalyst, was eluted with 2% acetone in hexane, from a Ca(OH)2 chromatographic column in three bands. The fractions were identified by spectrophotometry and the retention times of 2.05, 2.4 and 2.8 min for the 13 cis, all-trans, and 9 cis beta-carotene isomers, determined by HPLC, with 1% acetone in hexane as Mobil phase. 22.13 mg % of all-trans beta-carotene were found in a sample of canned carrots. It is recommended the analyses of a greater number of samples, the determination of the method's sensitivity, reproducibility, and the use of a standard of reference of a response factor for calculations.

  18. Hb Tianshui (HBB: C.119A > G) in Compound Heterozygosity with Hb S (HBB: C.20A > T) from Odisha, India.

    Science.gov (United States)

    Meher, Satyabrata; Dehury, Snehadhini; Mohanty, Pradeep Kumar; Patel, Siris; Pattanayak, Chinmayee; Bhattacharya, Subhra; Das, Kishalaya; Sarkar, Biswanath

    2016-08-01

    We describe here a rare β-globin gene variant, Hb Tianshui [β39(C5)Glu→Arg; HBB: c.119A > G], detected during routine screening in Odisha, India. This is the second report of Hb Tianshui and the first to describe the cation exchange high performance liquid chromatography (HPLC) and DNA studies of two cases of this variant. Both cases had coinherited Hb S (HBB: c.20A > T) but none presented with typical symptoms of sickle cell disease. One of the cases was heterozygous for a common α-thalassemia (α-thal) allele (-α(3.7)) (rightward) (NG_000006.1: g.34164_37967del3804) and marginally raised Hb F percentage, while the other Hb S/Hb Tianshui case was completely benign and healthy. An atypical Asian Indian haplotype [+ - + - +] could be assigned to the Hb Tianshui variant. Hb Tianshui seems to mimic a few other Hb variants in cation exchange HPLC. However, we report two specific patterns in the chromatograms that are characteristic to Hb Tianshui. Combining an alkaline electrophoresis result with cation exchange HPLC at screening would be preferred to detect this rare variant, especially in regions with considerable frequency of Hb E [β26(B8)Glu→Lys; HBB: c.79G > A] or Hb S.

  19. Analysis of the radiochemical purity of 18F-FDG by HPLC

    International Nuclear Information System (INIS)

    Chen Liguang; Tang Anwu; He Shanzhen; Chen Yulong

    2001-01-01

    The radiochemical purity (RCP) of 18 F-FDG is analyzed by HPLC. Eighty-five percent acetonitrile is used as the eluting solution. Carbon hydrate column is used as separation column. The t R of 18 F - is 6.50 min and 18 F-FDG is 9.00 min. HPLC take less time and has higher sensitivity than TLC for the same sample at the same time. So HPLC excels TLC in analyzing RCP of 18 F-FDG

  20. DETERMINATION AND VALIDATION OF MEBHYDROLINE NAPADISYLATE IN TABLETS BY HPLC

    Directory of Open Access Journals (Sweden)

    Lestyo Wulandari

    2010-06-01

    Full Text Available An accurate and sensitive HPLC method has been developed for the determination of mebhydroline napadisylate in the tablet. The Chromatography was performed on a reversed phase C-18 column, using a mobile phase of acetonitrile : ammonia 25% (80 : 20 v/v at ambient temperature 25±5 °C and UV detection operates at 320 nm in an overall analysis time of about 15 min, based on peak area. This HPLC method is selective, precise, and accurate and can be used for routine analysis of pharmaceutical preparation in industrial quality-control laboratories.   Keywords : HPLC, mebhydroline napadisylate, validation

  1. Authentication and Quantitation of Fraud in Extra Virgin Olive Oils Based on HPLC-UV Fingerprinting and Multivariate Calibration

    Science.gov (United States)

    Carranco, Núria; Farrés-Cebrián, Mireia; Saurina, Javier

    2018-01-01

    High performance liquid chromatography method with ultra-violet detection (HPLC-UV) fingerprinting was applied for the analysis and characterization of olive oils, and was performed using a Zorbax Eclipse XDB-C8 reversed-phase column under gradient elution, employing 0.1% formic acid aqueous solution and methanol as mobile phase. More than 130 edible oils, including monovarietal extra-virgin olive oils (EVOOs) and other vegetable oils, were analyzed. Principal component analysis results showed a noticeable discrimination between olive oils and other vegetable oils using raw HPLC-UV chromatographic profiles as data descriptors. However, selected HPLC-UV chromatographic time-window segments were necessary to achieve discrimination among monovarietal EVOOs. Partial least square (PLS) regression was employed to tackle olive oil authentication of Arbequina EVOO adulterated with Picual EVOO, a refined olive oil, and sunflower oil. Highly satisfactory results were obtained after PLS analysis, with overall errors in the quantitation of adulteration in the Arbequina EVOO (minimum 2.5% adulterant) below 2.9%. PMID:29561820

  2. Complex Interaction of Hb Q-Thailand (HBA1: c.223G>C) with β-Thalassemia/Hb E (HBB: c.79G>A) Disease.

    Science.gov (United States)

    Panyasai, Sitthichai; Satthakarn, Surada; Pornprasert, Sakorn

    2018-01-01

    Hb Q-Thailand [α74(EF3)Asp→His (α1), GAC>CAC, HBA1: c.223G>C] is an abnormal hemoglobin (Hb) frequently found in Thailand and Southeast Asian countries. The association of the α Q-Thailand allele with other globin gene disorders has important implications in diagnosis. Here, we report how to diagnose the coinheritance of Hb Q-Thailand with β-thalassemia (β-thal)/Hb E disease in four Thai samples from high performance liquid chromatography (HPLC) and capillary electrophoresis (CE) testing results. Understanding of the HPLC chromatogram and CE electropherogram patterns of this complex mutation is important for interpretation of testing results and providing genetic counseling.

  3. Quantitation of radiolabeled compounds eluting from the HPLC system

    International Nuclear Information System (INIS)

    Kessler, M.J.

    1982-01-01

    Three techniques are compared for the quantitation of various radiolabeled compounds eluting in the high performance liquid chromatography system. The first technique requires fraction-collecting the effluent from the HPLC, removing an aliquot to scintillation vials, and counting each fraction in a liquid scintillation counter. The second uses direct interface of the HPLC effluent to a flow-through radioactivity detector. The third involves quantitation of various radiolabeled compounds (proteins, steroids, and nucleotides) by splitting the effluent from the HPLC with an electronic steam splitter, thus diverting a present portion to the fraction collector for further chemical characterization and the remainder to the radioactivity flow detector for direct quantitation. A direct comparison of the chromatograms and the radioactivity counting efficiencies of these three techniques is presented

  4. Application of Hplc-Pda Method Using Two Different Extraction Procedures for the Determination of Alkylresorcinols in Cereals

    Directory of Open Access Journals (Sweden)

    Gailāne Natālija

    2015-09-01

    Full Text Available Cereals, especially barley, are an important source of vitamins, minerals, dietary fibre and various phytochemicals, such as alkylresorcinols (ARs. Cereal ARs are a group of phenolic lipids located in the outer parts of grain, particularly in rye and wheat, but not found in refined flour or in refined products from cereals. This study focuses on the comparison of different extraction procedures applied for the determination of the content of ARs (C15:0 - C23:0 in grain of Latvian barley genotypes. The content of ARs in 1 rye and 16 barley samples grown with different amounts of fertilier was determined by High Performance Liquid Chromatography method with Photodiode Array detection (HPLC-PDA developed by us. Two different extraction methods were compared: accelerated Soxhlet extraction and 24-hour extraction. Aside from validation of the extraction procedures, validation parameters for the HPLC-PDA based quantitation method were provided. The coefficients of variation for repeatability and intermediate precision were < 9% and < 3%, respectively. The content of ARs determined with the HPLC-PDA method in conjunction with accelerated Soxhlet extraction was up to 1.5 times higher than using 24-hour extraction. AR content varied from 2.11 ± 0.04 to 3.80 ± 0.10 mg·100 g-1 for 24-hour extraction and from 2.66 ± 0.06 to 5.70 ± 0.20 mg·100 g-1 for accelerated Soxhlet extraction, indicating the increased efficiency of this procedure in analysis of ARs.

  5. HPLC-ED Analysis of Phenolic Compounds in Three Bosnian Crataegus Species

    Directory of Open Access Journals (Sweden)

    Dušan Čulum

    2018-04-01

    Full Text Available The aim of this work was the qualitative and quantitative determination of selected phenolic compounds in three Crataegus species grown in Bosnia. Crataegus plants are consumed for medicinal purposes and as foodstuff in the form of canned fruit, jam, jelly, tea, and wine. Two samples of plant material, dry leaves with flowers, and berries of three Crataegus species—Crataegus rhipidophylla Gand., Crataegus x subsphaericea Gand., and Crataegus x macrocarpa Hegetschw.—were analyzed. Twelve ethanolic extracts were isolated from the selected plant material using Soxhlet and ultrasound extraction, respectively. Soxhlet extraction proved to be more effective than ultrasound extraction. A simple and sensitive method, high-performance liquid chromatography with electrochemical detection, HPLC-ED, was used for the simultaneous determination of phenolic acids and flavonoids in Crataegus species. The content of gallic acid in the extracts ranged from 0.001 to 0.082 mg/g dry weight (DW, chlorogenic acid from 0.19 to 8.70 mg/g DW, and rutin from 0.03 to 13.49 mg/g DW. Two flavonoids, vitexin and hyperoside, commonly found in chemotaxonomic investigations of Crataegus species, were not detected in the examined extracts. In general, leaves with flowers samples are richer in gallic acid and rutin, whereas the berries samples are richer in chlorogenic acid. Distinct similarities were found in the relative distribution of gallic acid among the three species. Extracts of C. x macrocarpa had the highest content of all detected compounds, while significant differences were found in rutin content, depending on the plant organ. To the best of our knowledge, this is the first study reporting content of phenolic compounds in Crataegus rhipidophylla Gand., Crataegus x subsphaericea, and Crataegus x macrocarpa from Bosnia.

  6. Isolation and identification of phytochemicals and biological activities of Hericium ernaceus and their contents in Hericium strains using HPLC/UV analysis.

    Science.gov (United States)

    Lee, Dong Gu; Kang, Hee-Wan; Park, Chun-Geon; Ahn, Young-Sup; Shin, Yusu

    2016-05-26

    Hericium ernaceus has been traditionally used for the treatment of dyspepsia, gastric ulcer and enervation in traditional Chinese medicine for a long time. To examine the effect of Hericium strains on their ability to inhibit LPS and interferon-γ induced NO production in cell culture and the bioassay correlation of hericenone C, D, F, isolated from H. ernaceus. Hericenone C, D, F were isolated from H. ernaceus by open column chromatography and identified on the basis of spectroscopic analyses including (1)H NMR, (13)C NMR and MS. The amounts of hericenone C, D, and F in Hericium strains were determined by HPLC/UV analysis. In order to investigate the anti-inflammatory effect of Hericium strains extracts, RAW 264.7 cells were treated with 200μg/mL of Hericium strains extracts for 48h. Cell growth was assessed by MTT assay. Phytochemical constituents were isolated from H. ernaceus by open column chromatography. Their structures were elucidated as hericenones C, D, and F on the basis of spectroscopic analyses including (1)H NMR, (13)C NMR and MS. The amounts of hericenones C, D, and F in Hericium strains were determined by HPLC/UV analysis. Hericenones C, D, and F contents were highest in Norugungdenglee-2 (8.289±0.593mg/g), KFRI-1453 (4.657±0.462mg/g), and KFRI-1093 (5.408±0.420mg/g) strains, respectively. All Hericium strains extracts tested inhibited the lipopolysaccharide- and interferon-γ-induced inflammatory activity of RAW264.7 cells. The strain KFRI-1093 about 39.6% reduced NO generation with compared to control. We believe that the anti-inflammatory effect of KFRI-1093 was due to hericenone F content. Our results contribute towards validation of the traditional use, natural drugs and health supplements. And also, the developed simple, accurate and rapid LC method can be used determinate the content of hericenones from other Hericium strains. Copyright © 2016. Published by Elsevier Ireland Ltd.

  7. Theoretische en practische aspecten van het gebruik van micro-HPLC

    NARCIS (Netherlands)

    de Fluiter P; Jansen EHJM

    1992-01-01

    A practical and theoretical approach for the implementation of micro high performance liquid chromatography (HPLC) is described. A new simple and rapid test procedure was developed in wich a HPLC system can be validated for its suitability for micro-bore columns. It appeared that the detector

  8. [HPLC characteristic fingerprints of sedi linearis herba and sedi herba].

    Science.gov (United States)

    Lu, Lan-Qing; Mei, Qing; Wan, Ding-Rong; Yang, Xin-Zhou; Qiao, Shu; Zhao, Yu-Dan

    2014-04-01

    To study HPLC characteristic fingerprint of Sedum lineare from different harvest periods, and to compare with its related species Sedum sarmentosum. The HPLC fingerprints of Sedum lineare from different collecting periods were established and compared with Sedum sarmentosum by the same detection method. Hyperin, isoquercitrin and astragaloside were identified from the HPLC fingerprint of Sedum lineare. The fingerprint of Sedum lineare growing in the same area but different environment were basically identical; while there were remarkable differences of Sedum lineare growing in the same place but from different harvest periods, with the area of most common peaks changing from little to great, and slightly different peak number. The HPLC fingerprint of the two Sedum species had four common peaks, but could be distinguished from each other. The optimal harvest period of these two species should be full-bloom stage. The established method can provide reference for identification and quality analysis of Sedum lineare.

  9. Stability-Indicating TLC-Densitometric and HPLC Methods for the Simultaneous Determination of Piracetam and Vincamine in the Presence of Their Degradation Products.

    Science.gov (United States)

    Ahmed, Amal B; Abdelrahman, Maha M; Abdelwahab, Nada S; Salama, Fathy M

    2016-11-01

    Newly established TLC-densitometric and RP-HPLC methods were developed and validated for the simultaneous determination of Piracetam (PIR) and Vincamine (VINC) in their pharmaceutical formulation and in the presence of PIR and VINC degradation products, PD and VD, respectively. The proposed TLC-densitometric method is based on the separation and quantitation of the studied components using a developing system that consists of chloroform-methanol-glacial acetic acid-triethylamine (8 + 2 + 0.1 + 0.1, v/v/v/v) on TLC silica gel 60 F254 plates, followed by densitometric scanning at 230 nm. On the other hand, the developed RP-HPLC method is based on the separation of the studied components using an isocratic elution of 0.05 M KH2PO4 (containing 0.1% triethylamine adjusted to pH 3 with orthophosphoric acid)-methanol (95 + 5, v/v) on a C8 column at a flow rate of 1 mL/min with diode-array detection at 230 nm. The developed methods were validated according to International Conference on Harmonization guidelines and demonstrated good accuracy and precision. Moreover, the developed TLC-densitometric and RP-HPLC methods are suitable as stability-indicating assay methods for the simultaneous determination of PD and VD either in bulk powder or pharmaceutical formulation. The results were statistically compared with those obtained by the reported RP-HPLC method using t- and F-tests.

  10. Characterization of Jamaican agro-industrial wastes. Part II, fatty acid profiling using HPLC: precolumn derivatization with phenacyl bromide.

    Science.gov (United States)

    Bailey-Shaw, Y A; Golden, K D; Pearson, A G M; Porter, R B R

    2012-09-01

    This paper describes the determination of fatty acid composition of coffee, citrus and rum distillery wastes using reversed-phase high-performance liquid chromatography (RP-HPLC). Lipid extracts of the waste samples are derivatized with phenacyl bromide and their phenacyl esters are separated on a C8 reversed-phase column by using continuous gradient elution with water and acetonitrile. The presence of saturated and unsaturated fatty acids in quantifiable amounts in the examined wastes, as well as the high percentage recoveries, are clear indications that these wastes have potential value as inexpensive sources of lipids. The HPLC procedures described here could be adopted for further analysis of materials of this nature.

  11. [HPLC fingerprint analysis of flavonoids of phyllanthi fructus from different habitats].

    Science.gov (United States)

    Wang, Fei; Wang, Shuai; Meng, Xian-sheng; Bao, Yong-rui; Zhu, Ying-huan

    2014-11-01

    To establish the HPLC fingerprint of flavonoids of Phyllanthi Fructus from different habitats. HPLC method was adopted. The flavonoids composition of Phyllanthi Fructus from 10 different habitats was determined on an Agilent C, chromatographic column with 0. 5% formic acid water (A)-acetonitrile (B) as the mobile phase in gradient elution under the wavelength of 254 nm. The HPLC fingerprints of flavonoids composition of Phyllanthi Fructus were established to evaluate the qualitiy of them. The HPLC fingerprints of flavonoids composition of Phyllanthi Fructus from 10 different habitats were established. 18 common peaks were found and the similarities of them were more than 0. 90 except the ones from Guangxi and Guangdong. The method is simple, accurate and repeatable. It can be used for research and quality control of the effective components in Phyllanthi Fructus.

  12. 8×8 Planar Phased Array Antenna with High Efficiency and Insensitivity Properties for 5G Mobile Base Stations

    DEFF Research Database (Denmark)

    Ojaroudiparchin, Naser; Shen, Ming; Pedersen, Gert F.

    2016-01-01

    An insensitive planar phased array antenna with high efficiency function for 5G applications is introduced in this study. 64-elements of compact slot-loop antenna elements have been used to form the 8×8 planar array. The antenna is designed on a low cost FR4 substrate and has good performance in ...... at both sides of the substrate and could be used for mobile base station (MBS) applications. The proposed planar array could be integrated with the transceivers on the low-cost printed circuit boards (PCBs) to reduce the manufacturing cost....

  13. Electrochemically Pretreated Carbon Microfiber Electrodes as Sensitive HPLC-EC Detectors

    Directory of Open Access Journals (Sweden)

    Zdenka Bartosova

    2012-01-01

    Full Text Available The paper focuses on the analysis and detection of electroactive compounds using high-performance liquid chromatography (HPLC combined with electrochemical detection (EC. The fabrication and utilization of electrochemically treated carbon fiber microelectrodes (CFMs as highly sensitive amperometric detectors in HPLC are described. The applied pretreatment procedure is beneficial for analytical characteristics of the sensor as demonstrated by analysis of the model set of phenolic acids. The combination of CFM with separation power of HPLC technique allows for improved detection limits due to unique electrochemical properties of carbon fibers. The CFM proved to be a promising tool for amperometric detection in liquid chromatography.

  14. Extraction and Determination of Cyproheptadine in Human Urine by DLLME-HPLC Method.

    Science.gov (United States)

    Maham, Mehdi; Kiarostami, Vahid; Waqif-Husain, Syed; Abroomand-Azar, Parviz; Tehrani, Mohammad Saber; Khoeini Sharifabadi, Malihe; Afrouzi, Hossein; Shapouri, Mahmoudreza; Karami-Osboo, Rouhollah

    2013-01-01

    Novel dispersive liquid-liquid microextraction (DLLME), coupled with high performance liquid chromatography with photodiode array detection (HPLC-DAD) has been applied for the extraction and determination of cyproheptadine (CPH), an antihistamine, in human urine samples. In this method, 0.6 mL of acetonitrile (disperser solvent) containing 30 μL of carbon tetrachloride (extraction solvent) was rapidly injected by a syringe into 5 mL urine sample. After centrifugation, the sedimented phase containing enriched analyte was dissolved in acetonitrile and an aliquot of this solution injected into the HPLC system for analysis. Development of DLLME procedure includes optimization of some important parameters such as kind and volume of extraction and disperser solvent, pH and salt addition. The proposed method has good linearity in the range of 0.02-4.5 μg mL(-1) and low detection limit (13.1 ng mL(-1)). The repeatability of the method, expressed as relative standard deviation was 4.9% (n = 3). This method has also been applied to the analysis of real urine samples with satisfactory relative recoveries in the range of 91.6-101.0%.

  15. Development of an Ultrasonication-Assisted Extraction Based HPLC With a Fluorescence Method for Sensitive Determination of Aflatoxins in Highly Acidic Hibiscus sabdariffa

    Directory of Open Access Journals (Sweden)

    Xiaofei Liu

    2018-04-01

    Full Text Available The high acidity and complex components of Hibiscus sabdariffa have provided major challenges for sensitive determination of trace aflatoxins. In this study, sample pretreatment of H. sabdariffa was systematically developed for sensitive high performance liquid chromatography-fluorescence detection (HPLC-FLD after ultrasonication-assisted extraction, immunoaffinity column (IAC clean-up and on-line post-column photochemical derivatization (PCD. Aflatoxins B1, B2, G1, G2 were extracted from samples by using methanol/water (70:30, v/v with the addition of NaCl. The solutions were diluted 1:8 with 0.1 M phosphate buffer (pH 8.0 to negate the issues of high acidity and matrix interferences. The established method was validated with satisfactory linearity (R > 0.999, sensitivity (limits of detection (LODs and limits of quantitation (LOQs of 0.15–0.65 and 0.53–2.18 μg/kg, respectively, precision (RSD <11%, stability (RSD of 0.2–3.6%, and accuracy (recovery rates of 86.0–102.3%, which all met the stipulated analytical requirements. Analysis of 28 H. sabdariffa samples indicated that one sample incubated with Aspergillus flavus was positive with aflatoxin B1 (AFB1 at 3.11 μg/kg. The strategy developed in this study also has the potential to reliably extract and sensitively detect more mycotoxins in other complex acidic matrices, such as traditional Chinese medicines, foodstuffs, etc.

  16. A validated solid-liquid extraction method for the HPLC determination of polyphenols in apple tissues Comparison with pressurised liquid extraction.

    Science.gov (United States)

    Alonso-Salces, Rosa M; Barranco, Alejandro; Corta, Edurne; Berrueta, Luis A; Gallo, Blanca; Vicente, Francisca

    2005-02-15

    A solid-liquid extraction procedure followed by reversed-phase high-performance liquid chromatography (RP-HPLC) coupled with a photodiode array detector (DAD) for the determination of polyphenols in freeze-dried apple peel and pulp is reported. The extraction step consists in sonicating 0.5g of freeze-dried apple tissue with 30mL of methanol-water-acetic acid (30:69:1, v/v/v) containing 2g of ascorbic acid/L, for 10min in an ultrasonic bath. The whole method was validated, concluding that it is a robust method that presents high extraction efficiencies (peel: >91%, pulp: >95%) and appropriate precisions (within day: R.S.D. (n = 5) <5%, and between days: R.S.D. (n = 5) <7%) at the different concentration levels of polyphenols that can be found in apple samples. The method was compared with one previously published, consisting in a pressurized liquid extraction (PLE) followed by RP-HPLC-DAD determination. The advantages and disadvantages of both methods are discussed.

  17. Development and validation of methodology for technetium-99m radiopharmaceuticals using high performance liquid chromatography (HPLC)

    International Nuclear Information System (INIS)

    Almeida, Erika Vieira de

    2009-01-01

    Radiopharmaceuticals are compounds, with no pharmacological action, which have a radioisotope in their composition and are used in Nuclear Medicine for diagnosis and therapy of several diseases. In this work, the development and validation of an analytical method for 99 mTc-HSA, 99 mTc-EC, 99 mTc-ECD and 99 mTc-Sestamibi radiopharmaceuticals and for some raw materials were carried out by high performance liquid chromatography (HPLC). The analyses were performed in a Shimadzu HPLC equipment, LC-20AT Prominence model. Some impurities were identified by the addition of a reference standard substance. Validation of the method was carried out according to the criteria defined in RE n. 899/2003 of the National Sanitary Agency (ANVISA). The results for robustness of the method showed that it is necessary to control flow rate conditions, sample volume, pH of the mobile phase and temperature of the oven. The analytical curves were linear in the concentration ranges, with linear correlation coefficients (r 2 ) above 0.9995. The results for precision, accuracy and recovery showed values in the range of 0.07-4.78%, 95.38-106.50% and 94.40-100.95%, respectively. The detection limits and quantification limits varied from 0.27 to 5.77 μg mL -1 and 0.90 to 19.23 μg mL -1 , respectively. The values for HAS, EC, ECD and MIBI in the lyophilized reagents were 8.95; 0.485; 0.986 and 0.974 mg L-1, respectively. The mean radiochemical purity for 99 mTc-HSA, 99 mTc-EC, 99 mTc-ECD and 99 mTc-Sestamibi was (97.28 ± 0.09)%, (98.96 ± 0.03)%, (98.96 ± 0.03)% and (98.07 ± 0.01)%, respectively. All the parameters recommended by ANVISA were evaluated and the results are below the established limits. (author)

  18. Comparative determination of sibutramine as an adulterant in natural slimming products by HPLC and HPTLC densitometry.

    Science.gov (United States)

    Ariburnu, Etil; Uludag, Mehmet Fazli; Yalcinkaya, Huseyin; Yesilada, Erdem

    2012-05-01

    A new validated method for the identification and quantification of the sibutramine was developed by HPTLC-densitometry at 225 nm and advantages and disadvantages compared with HPLC-FLD at 225 nm emission and 316 nm excitation. Both methods were applied to the analysis of three natural slimming products in the market for the quantitative analysis of illegally added sibutramine. HPTLC separations were performed on (20 cm × 10 cm) glass HPTLC plates coated with silica gel 60 F(254) using a mobile phase, n-hexane-acetone-ammonia (10:1:0.1, v/v/v). For HPLC analysis, a phenyl column (5.0 μm, 150 mm × 4.6 mm, i.d.) and an isocratic mobile phase of acetonitrile-water-formic acid (pH 3.0; 0.19M) (45:55:0.78, v/v/v) was used. The calibration curve area versus concentration was found to be linear in the range of 250-2000 ng/spot(-1) and 5-200 μg/ml for HPTLC and HPLC, respectively. Both methods were validated for accuracy, precision, linearity, selectivity, recovery and short term stability. As a conclusion, these methods were found to be useful for the routine analysis of illegally added sibutramine in the marketed products. Copyright © 2012 Elsevier B.V. All rights reserved.

  19. [Determination of rhynchophylline and isorhynchophylline in Uncaria rhynchophylla by HPLC].

    Science.gov (United States)

    Yang, Xiu-Juan; Hong, Yan-Long; Wu, Fei; Ruan, Ke-Feng; Feng, Yi

    2013-03-01

    To explore an HPLC method for determination of rhnchophylline and isorhnchophylline in Uncaria rhnchophylla. An HPLC method has been developed for determination of rhnchophylline and isorhnchophylline. The transformation of rhnchophylline and isorhnchophylline after heating was also studied by HPLC-ESI-MS. Good linearities of rhynchophylline and isorhynchophylline were 0.064-5.100, 0.064-5.110 mg, respectively. The average recoveries were from 87.51% to 88.83% for rhynchophylline and from 107.9% to 113.9% for isorhynchophylline. The recoveries of rhynchophylline and isorhnchophylline reference solutions after extraction were 12.60% and 40.00% in the reflux extraction procedure, respectively. While in the ultrasonic extraction procedure, the average recoveries of rhynchophylline and isorhynchophylline was from 99.48% to 103.2% and from 97.00% to 99.59%, resepectively. The recoveries of rhynchophylline and isorhnchophylline reference solutions after extraction were 47.08% and 51.03%, respectively. The unqualified recovery could be elucidated by HPLC-ESI-MS analysis, indicating that trhynchophylline could be transformed mostly into isorhynchophylline and a little amount of unkown composition, while isorhynchophylline could be transformed into rhynchophylline isocorynoxeine, corynoxeine and 22-O-beta-D-glucopyranosyl isocorynoxeinic acid during the extraction procedure. Ultrasonic extraction procedure was more sutble for HPLC determination of the content of rhynchophylline and isorhynchophylline in U. rhnchophylla, however, the recovery problems should be paid attention to when it comes to the determination.

  20. Validation of a dissolution method with RP-HPLC analysis for Perindopril erbumine and Indapamide combination tablet

    Directory of Open Access Journals (Sweden)

    Jain P.S.

    2012-01-01

    Full Text Available A Dissolution method with high performance liquid chromatography (HPLC analysis was validated for perindopril erbumine and indapamide in combination tablet formulation. The method was validated to meet requirements for a global regulatory filing and this validation included specificity, linearity, accuracy, precision, range, robustness and solution stability studies. The dissolution method, which uses USP apparatus 1 with basket rotating at 100 rpm, 1000 ml of phosphate buffer pH 6.8 as the dissolution medium, and reversed-phased HPLC was carried out at 50⁰C on a 4.6mm×250mm 5μm cyano column that contained USP packing L1 with acetonitrile: buffer pH 2.8::40:60 (v/v, as mobile phase. UV detector was set at 225 nm. A method was found to be selective, linear, accurate and precise in the specified ranges. Intra-day and inter-day variability for method was <2% RSD. This method was successfully used for quantification of perindopril erbumine and indapamide combination tablet formulations.

  1. INFORMATION AND RECOMMENDATIONS CONCERNING THE ENLARGED G8 SUMMIT MEETING AT EVIAN

    CERN Multimedia

    2003-01-01

    Despite the difficulties that CERN might encounter, the Organization will pursue its activities for the duration of the G8 Summit Meeting. The Management and Division leaders will take the necessary steps to ensure the proper functioning of the Organization, while taking account of the aforementioned difficulties. The Swiss and French authorities have informed CERN of the following general security and traffic arrangements associated with the enlarged G8 summit: a) Road traffic Between 22 May and 6 June traffic on certain roads in the Canton of Geneva (notably on the left bank) and in neighbouring France (mainly Haute-Savoie) will be disrupted and, in some cases, roads closed. As far as border crossings between 22 May and 4 June are concerned, the frontier posts will be divided into three categories (see map): - posts closed to all traffic (diversion signs will be in place), - posts open at certain times, - posts open at all times. N.B. : the road from Prévessin to Mategnin will be closed and traffic div...

  2. Simultaneous Determination and Pharmacokinetic Study of Quercetin, Luteolin, and Apigenin in Rat Plasma after Oral Administration of Matricaria chamomilla L. Extract by HPLC-UV

    Directory of Open Access Journals (Sweden)

    Xiaoxv Dong

    2017-01-01

    Full Text Available A simple and sensitive HPLC-UV method has been developed for the simultaneous determination of quercetin, luteolin, and apigenin in rat plasma after oral administration of Matricaria chamomilla L. extract. The flow rate was set at 1.0 ml/min and the detection wavelength was kept at 350 nm. The calibration curves were linear in the range of 0.11–11.36 μg/ml for quercetin, 0.11–11.20 μg/ml for luteolin, and 0.11–10.60 μg/ml for apigenin, respectively. The intraday and interday precisions (RSD were less than 8.32 and 8.81%, respectively. The lower limits of quantification (LLOQ of the three compounds were 0.11 μg/ml. The mean recoveries for quercetin, luteolin, and apigenin were 99.11, 95.62, and 95.21%, respectively. Stability studies demonstrated that the three compounds were stable in the preparation and analytical process. The maximum plasma concentration (Cmax was 0.29 ± 0.06, 3.04 ± 0.60, and 0.42 ± 0.10 μg/ml, respectively. The time to reach the maximum plasma concentration (Tmax was 0.79 ± 0.25, 0.42 ± 0.09, and 0.51 ± 0.13 h, respectively. The validated method was successfully applied to investigate the pharmacokinetics study of quercetin, luteolin, and apigenin in rat plasma after oral administration of M. chamomilla extract.

  3. Selenium speciation analysis of Misgurnus anguillicaudatus selenoprotein by HPLC-ICP-MS and HPLC-ESI-MS/MS

    Science.gov (United States)

    Analytical methods for selenium (Se) speciation were developed using high performance liquid chromatography (HPLC) coupled to either inductively coupled plasma mass spectrometry (ICP-MS) or electrospray ionization tandem mass spectrometry (ESI-MS/MS). Separations of selenomethionine (Se-Met) and sel...

  4. Transfusion Associated Peak in Hb HPLC Chromatogram – a Case Report

    Science.gov (United States)

    Jain, Sonal; Dass, Jasmita; Pati, Hara Prasad

    2012-01-01

    High performance liquid chromatography (HPLC) and electrophoresis are commonly used to diagnose various hemoglobinopathies. However, insufficient information about the transfusion history can lead to unexpected and confusing results. We are reporting a case of Juvenile myelomonocytic leukemia (JMML) in which HbHPLC was done to quantify fetal hemoglobin (HbF). The chromatogram showed elevated HbF along with a peak in the HbD window. A transfusion acquired peak was suspected based on the unexpectedly low percentage of HbD and was subsequently confirmed using parental HbHPLC. PMID:22348188

  5. RP-HPLC/MS-APCI Analysis of Branched Chain TAG Prepared by Precursor-Directed Biosynthesis with Rhodococcus erythropolis

    Czech Academy of Sciences Publication Activity Database

    Schreiberová, O.; Krulikovská, T.; Sigler, Karel; Čejková, A.; Řezanka, Tomáš

    2010-01-01

    Roč. 45, č. 8 (2010), s. 743-756 ISSN 0024-4201 R&D Projects: GA MŠk 2B08062 Institutional research plan: CEZ:AV0Z50200510 Keywords : Rhodococcus erythropolis * RP-HPLC/MS-APCI * Branched chain triacylglycerols Subject RIV: EE - Microbiology, Virology Impact factor: 2.151, year: 2010

  6. Quantitative analysis of PMR-15 polyimide resin by HPLC

    Science.gov (United States)

    Roberts, Gary D.; Lauver, Richard W.

    1987-01-01

    The concentration of individual components and of total solids of 50 wt pct PMR-15 resin solutions was determined using reverse-phase HPLC to within + or - 8 percent accuracy. Acid impurities, the major source of impurities in 3,3', 4,4'-benzophenonetetracarboxylic acid (BTDE), were eliminated by recrystallizing the BTDE prior to esterification. Triester formation was not a problem because of the high rate of esterification of the anhydride relative to that of the carboxylic acid. Aging of PMR-15 resin solutions resulted in gradual formation of the mononadimide and bisnadimide of 4,4'-methylenedianiline, with the BTDE concentration remaining constant. Similar chemical reactions occurred at a reduced rate in dried films of PMR-15 resin.

  7. SAJCH 723.indd

    African Journals Online (AJOL)

    Hypoglycaemia in children aged 1 month to 10 years admitted to the ... 3 Department of Paediatrics, Lagos State University Teaching Hospital, Ikeja, Lagos, Nigeria. Corresponding ... Database on Child Growth and Malnutrition.[8]. Results.

  8. [HPLC-ELSD for determining contents of three triterpenoidal saponins in fruits of Buddleja lindleyana from different habitats].

    Science.gov (United States)

    Wu, Pei-Yun; Ren, Ya-Shuo; Wu, De-Ling; Qiao, Jin-Wei

    2016-04-01

    To establish an HPLC-ELSD method for the quantification of triterpenoids in the fruits of Buddleja lindleyana. The RP-HPLC-ELSD method was used for the determination of triterpenoids in B. lindleyana fruits, which were collected from different habitats. The column used was a packed with 5 μm stationary phase Waters SunFireTM C₁₈ (4.6 mm×150 mm, 5 μm). The mobile phase consisted of Methanol-water(82∶18) at a flow rate of 1 mL•min⁻¹. Column temperature: 30 ℃. ELSD conditions: drift tube temperature: 106 ℃; carrier gas (nitrogen) flow rate: 1.5 L•min⁻¹; amplification factor: 1. The calibration curves showed good linear relationship on a range from 0.702 to 28.08 μg(r=0.999 2) for Clinoposaponin III, 0.390 to 15.60 μg(r=0.998 9) for Desrhamnoverbascosaponin and 0.192 to 7.68μg(r=0.999 0) for Mimengoside I. The average recovery rate(n=6) were 99.41%, 99.08% and 98.67% and it's RSD were 0.86%, 1.56% and 1.80%. This method can be used to determine the contents of triterpenoids in the fruits of Buddleja lindleyana for its simplicity, accurateness and reliability. Copyright© by the Chinese Pharmaceutical Association.

  9. Antioxidant Properties and Hyphenated HPLC-PDA-MS Profiling of Chilean Pica Mango Fruits (Mangifera indica L. Cv. piqueño

    Directory of Open Access Journals (Sweden)

    Javier E. Ramirez

    2013-12-01

    Full Text Available Antioxidant capacities and polyphenolic contents of two mango cultivars from northern Chile, one of them endemic of an oasis in the Atacama Desert, were compared for the first time. Twenty one phenolic compounds were detected in peel and pulp of mango fruits varieties Pica and Tommy Atkins by HPLC-PDA-MS and tentatively characterized. Eighteen compounds were present in Pica pulp (ppu, 13 in Pica peel (ppe 11 in Tommy Atkins pulp (tpu and 12 in Tommy Atkins peel (tpe. Three procyanidin dimers (peaks 6, 9 and 10, seven acid derivatives (peaks 1–4, 11, 20 and 21 and four xanthones were identified, mainly mangiferin (peak 12 and mangiferin gallate, (peak 7, which were present in both peel and pulp of the two studied species from northern Chile. Homomangiferin (peak 13 was also present in both fruit pulps and dimethylmangiferin (peak 14 was present only in Tommy pulp. Pica fruits showed better antioxidant capacities and higher polyphenolic content (73.76/32.23 µg/mL in the DPPH assay and 32.49/72.01 mg GAE/100 g fresh material in the TPC assay, for edible pulp and peel, respectively than Tommy Atkins fruits (127.22/46.39 µg/mL in the DPPH assay and 25.03/72.01 mg GAE/100 g fresh material in the TPC assay for pulp and peel, respectively. The peel of Pica mangoes showed also the highest content of phenolics (66.02 mg/100 g FW measured by HPLC-PDA. The HPLC generated fingerprint can be used to authenticate Pica mango fruits and Pica mango food products.

  10. Antioxidant properties and hyphenated HPLC-PDA-MS profiling of Chilean Pica mango fruits (Mangifera indica L. Cv. piqueño).

    Science.gov (United States)

    Ramirez, Javier E; Zambrano, Ricardo; Sepúlveda, Beatriz; Simirgiotis, Mario J

    2013-12-31

    Antioxidant capacities and polyphenolic contents of two mango cultivars from northern Chile, one of them endemic of an oasis in the Atacama Desert, were compared for the first time. Twenty one phenolic compounds were detected in peel and pulp of mango fruits varieties Pica and Tommy Atkins by HPLC-PDA-MS and tentatively characterized. Eighteen compounds were present in Pica pulp (ppu), 13 in Pica peel (ppe) 11 in Tommy Atkins pulp (tpu) and 12 in Tommy Atkins peel (tpe). Three procyanidin dimers (peaks 6, 9 and 10), seven acid derivatives (peaks 1-4, 11, 20 and 21) and four xanthones were identified, mainly mangiferin (peak 12) and mangiferin gallate, (peak 7), which were present in both peel and pulp of the two studied species from northern Chile. Homomangiferin (peak 13) was also present in both fruit pulps and dimethylmangiferin (peak 14) was present only in Tommy pulp. Pica fruits showed better antioxidant capacities and higher polyphenolic content (73.76/32.23 µg/mL in the DPPH assay and 32.49/72.01 mg GAE/100 g fresh material in the TPC assay, for edible pulp and peel, respectively) than Tommy Atkins fruits (127.22/46.39 µg/mL in the DPPH assay and 25.03/72.01 mg GAE/100 g fresh material in the TPC assay for pulp and peel, respectively). The peel of Pica mangoes showed also the highest content of phenolics (66.02 mg/100 g FW) measured by HPLC-PDA. The HPLC generated fingerprint can be used to authenticate Pica mango fruits and Pica mango food products.

  11. Measurement of isotopic composition of lanthanides in reprocessing process solutions by high-performance liquid chromatography with inductively coupled plasma mass spectrometry (HPLC/ICP-MS)

    International Nuclear Information System (INIS)

    Okano, Masanori; Jitsukata, Shu; Kuno, Takehiko; Yamada, Keiji

    2011-01-01

    Isotopic compositions of fission products in process solutions and wastes in a reprocessing plant are valuable to proceed safety study of the solutions and research/development concerning treatment/disposal of the wastes. The amount of neodymium-148 is a reliable indication to evaluate irradiation history. The isotopic compositions of samarium and gadolinium in high radioactive wastes are referred to as essential data to evaluate environmental impact in geological repositories. However, pretreatment of analysis must be done with complicated chemical separation such as solvent extraction and ion exchange. The actual measurement data of isotopic compositions of lanthanides comparable to the one of actinides in spent fuel reprocessing process has not been obtained enough. Rapid and high sensitive analytical technique based on high-performance liquid chromatography (HPLC) with an inductively coupled plasma mass spectrometry (ICP-MS) has been developed for the measurement of isotopic compositions of lanthanides in spent fuel reprocessing solutions. HPLC/ICP-MS measurement system was customized for a glove-box to be applied to the radioactive solutions. The cation exchange chromatographic columns (Shim-pack IC-C1) and injection valve (20μL) were located inside of the glove-box except the chromatographic pump. The elements of lanthanide group were separated by a gradient program of HPLC with α-hydroxyisobutyric acid. Isotopic compositions of lanthanides in eluate was sequentially analyzed by a quadruple ICP-MS. Optimization of parameter of HPLC and ICP-MS measurement system was examined with standard solutions containing 14 lanthanide elements. The elements of lanthanides were separated by HPLC and detected by ICP-MS within 25 minutes. The detection limits of Nd-146, Sm-147 and Gd-157 were 0.37 μg L -1 , 0.69 μg L -1 and 0.47 μg L -1 , respectively. The analytical precision of the above three isotopes was better than 10% for standard solutions of 100 μg L -1 with

  12. Optimization of supercritical fluid extraction and HPLC identification of wedelolactone from Wedelia calendulacea by orthogonal array design.

    Science.gov (United States)

    Patil, Ajit A; Sachin, Bhusari S; Wakte, Pravin S; Shinde, Devanand B

    2014-11-01

    The purpose of this work is to provide a complete study of the influence of operational parameters of the supercritical carbon dioxide assisted extraction (SC CO2E) on yield of wedelolactone from Wedelia calendulacea Less., and to find an optimal combination of factors that maximize the wedelolactone yield. In order to determine the optimal combination of the four factors viz. operating pressure, temperature, modifier concentration and extraction time, a Taguchi experimental design approach was used: four variables (three levels) in L9 orthogonal array. Wedelolactone content was determined using validated HPLC methodology. Optimum extraction conditions were found to be as follows: extraction pressure, 25 MPa; temperature, 40 °C; modifier concentration, 10% and extraction time, 90 min. Optimum extraction conditions demonstrated wedelolactone yield of 8.01 ± 0.34 mg/100 g W. calendulacea Less. Pressure, temperature and time showed significant (p yield. The supercritical carbon dioxide extraction showed higher selectivity than the conventional Soxhlet assisted extraction method.

  13. Comparison of the BioRad Variant and Primus Ultra2 high-pressure liquid chromatography (HPLC) instruments for the detection of variant hemoglobins.

    Science.gov (United States)

    Gosselin, R C; Carlin, A C; Dwyre, D M

    2011-04-01

    Hemoglobin variants are a result of genetic changes resulting in abnormal or dys-synchronous hemoglobin chain production (thalassemia) or the generation of hemoglobin chain variants such as hemoglobin S. Automated high-pressure liquid chromatography (HPLC) systems have become the method of choice for the evaluation of patients suspected with hemoglobinopathies. In this study, we evaluated the performance of two HPLC methods used in the detection of common hemoglobin variants: Variant and Ultra2. There were 377 samples tested, 26% (99/377) with HbS, 8.5% (32/377) with HbC, 20.7% (78/377) with other hemoglobin variant or thalassemia, and 2.9% with increased hemoglobin A(1) c. The interpretations of each chromatograph were compared. There were no differences noted for hemoglobins A(0), S, or C. There were significant differences between HPLC methods for hemoglobins F, A(2), and A(1) c. However, there was good concordance between normal and abnormal interpretations (97.9% and 96.2%, respectively). Both Variant and Ultra2 HPLC methods were able to detect most common hemoglobin variants. There was better discrimination for fast hemoglobins, between hemoglobins E and A(2), and between hemoglobins S and F using the Ultra2 HPLC method. © 2010 Blackwell Publishing Ltd.

  14. Separation, purification and identification of flavonoid glycosides using reversed phase hplc

    International Nuclear Information System (INIS)

    Hasan, A.; Khan, M.A.

    2002-01-01

    Optimal high performance liquid chromatography (HPLC) separation conditions and semi-preparative scale isolation of flavonoid glycosides from three plant species namely Vitex nagunda, Rubus ulmifolious and Malotus philipensis is reported. Identification of purified flavonoid glycoside was achieved using spiking technique in HPLC. (author)

  15. Prognostic value of serum heavy/light chain ratios in patients with POEMS syndrome.

    Science.gov (United States)

    Wang, Chen; Su, Wei; Cai, Qian-Qian; Cai, Hao; Ji, Wei; Di, Qian; Duan, Ming-Hui; Cao, Xin-Xin; Zhou, Dao-Bin; Li, Jian

    2016-07-01

    POEMS syndrome is a rare plasma cell dyscrasia. Serum concentrations of the monoclonal protein in this disorder are typically low, and inapplicable to monitor disease activity in most cases, resulting in limited practical and prognostic values. Novel immunoassays measuring isotype-specific heavy/light chain (HLC) pairs showed its utility in disease monitoring and outcome prediction in several plasma cell dyscrasias. We report results of HLC measurements in 90 patients with POEMS syndrome. Sixty-six patients (73%; 95% confidence interval, 63-82%) had an abnormal HLC ratio at baseline. It could stratify the risk of disease relapse and was strongly associated with worse progression-free survival in a multivariate analysis (P = 0.021; hazard ratio [HR] 6.89, 95% CI 1.34-35.43). After therapy, HLC ratios improved, with 43 patients (48%) remaining abnormal. The post-therapeutic HLC ratio, if abnormal, also remained as an independent prognostic factor associated with worse progression-free survival (P = 0.019; HR 4.30, 95% CI 1.27-14.56). These results suggest the prognostic utility of HLC ratios in clinical management of POEMS patients. © 2015 John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.

  16. Comparison of the effects of Mylabris and Acanthopanax senticosus on promising cancer marker polyamines in plasma of a Hepatoma-22 mouse model using HPLC-ESI-MS.

    Science.gov (United States)

    Wang, Qian; Wang, Yixiang; Liu, Ran; Yan, Xu; Li, Yujiao; Fu, Hui; Bi, Kaishun; Li, Qing

    2013-02-01

    A simple and sensitive method for the simultaneous determination of plasma concentrations of five polyamines in normal and Hepatoma-22 mice, and mice treated with Mylabris and Acanthopanax senticosus was developed by HPLC-ESI-MS. Male Kunming mice were divided into nine groups, a control group (inoculation without treatment), a positive group (Cyclophosphamide), treatment groups [Mylabris (4, 8, 16 mg/kg), Acanthopanax senticosus (6, 12, 24 g/kg)] and a normal group (without inoculation). Twenty-four hours after the last administration, plasma samples were collected. The derived polyamines were separated on a C(18) column by a gradient elution using methanol-water with excellent linearity within the range from 2.5 to 1000 ng/mL. Polyamines were confirmed as useful biochemical markers of hepatoma. The differences in anti-cancer therapeutic efficacy between Mylabris and Acanthopanax senticosus might contribute to the variability of polyamine levels in vivo. This HPLC-ESI-MS method was successfully applied to investigate the relationship between polyamines and cancer in mice and might be a useful method to test the activity of potential anti-tumor drugs. Copyright © 2012 John Wiley & Sons, Ltd.

  17. RP-HPLC Method Development and Validation for the Determination and Stability Indicative Studies of Montelukast in Bulk and its Pharmaceutical Formulations

    Directory of Open Access Journals (Sweden)

    A. Patnaik

    2012-01-01

    Full Text Available A simple, precise, accurate, economical and reproducible HPLC method for estimation of montelukast in tablet dosage form has been developed. Quantitative HPLC was performed with Shimadzu LC2010c HT with Winchrom Software with UV-Visible detector (SPD-IOA, PUMP (LC-IOAT and (LC-IOATvp. Phenomenex C8, 5 μm, 25 cm × 4.6 mm i.d. column was used in the study. The mobile phase of ACN: Acetate buffer= 6.5:3.5 of pH 3 were used in this study. The conditions optimized were: flow rate (1 mL/minute, wavelength (222 nm and run time was 20 min. Retention time was found to be 3.08 min. The linearity was found to be in the concentration range of 10-100 μg/mL. The developed method was evaluated in the assay of commercially available tablet moni containing 10 mg of montelukast. The amount of drug in tablet was found to be 10.34 mg/tab for the brand. Results of analysis were validated statistically and by recovery studies. The recovery studies 99.67% was indicative of the accuracy of proposed method. The precision was calculated as repeatability, inter and intraday variation (%RSD for the drug. By using the method, stability of the drug has been studied.

  18. In vitro antimicrobial and antimycobacterial activity and HPLC-DAD screening of phenolics from Chenopodium ambrosioides L.

    Directory of Open Access Journals (Sweden)

    Roberta S. Jesus

    Full Text Available Abstract The main objective of this study was to demonstrate the antimicrobial potential of the crude extract and fractions of Chenopodium ambrosioides L., popularly known as Santa-Maria herb, against microorganisms of clinical interest by the microdilution technique, and also to show the chromatographic profile of the phenolic compounds in the species. The Phytochemical screening revealed the presence of cardiotonic, anthraquinone, alkaloids, tannins and flavonoids. The analysis by HPLC-DAD revealed the presence of rutin in the crude extract (12.5 ± 0.20 mg/g, ethyl acetate (16.5 ± 0.37 mg/g and n-butanol (8.85 ± 0.11 mg/g, whereas quercetin and chrysin were quantified in chloroform fraction (1.95 ± 0.04 and 1.04 ± 0.01 mg/g, respectively. The most promising results were obtained with the ethyl acetate fraction, which inhibited a greater number of microorganisms and presented the lowest values of MIC against Staphylococcus aureus and Enterococcus faecalis (MIC = 0.42 mg/mL, Pseudomonas aeruginosa (MIC = 34.37 mg/mL, Paenibacillus apiarus (MIC = 4.29 mg/mL and Paenibacillus thiaminolyticus (MIC = 4.29 mg/mL. Considering mycobacterial inhibition, the best results were obtained by chloroform fraction against M. tuberculosis, M. smegmatis, and M. avium (MIC ranging from 156.25 to 625 µg/mL. This study proves, in part, that the popular use of C. ambrosioides L. can be an effective and sustainable alternative for the prevention and treatment of diseases caused by various infectious agents.

  19. Análise, por CLAE, de carotenóides de cinco linhagens de Rhodotorula HPLC analysis of carotenoids from five Rhodotorula strains

    Directory of Open Access Journals (Sweden)

    Fabio M. Squina

    2003-09-01

    Full Text Available Um método por cromatografia líquida de alta eficiência (CLAE foi otimizado para a análise da composição de carotenóides de cinco linhagens de Rhodotorula.A extração com ruptura mecânica da parede celular da levedura com areia tratada mostrou ser mais eficiente que a ruptura química com dimetilsulfóxido. Os carotenóides foram separados e quantificados por CLAE em coluna de C18 utilizando como fase móvel acetonitrila/metanol (0,1% trietilamina/acetato de etila (75:15:10 e 100% metanol (0,1% trietilamina entre as injeções, com vazão de 1 mL/min. Em todas as linhagens, os carotenóides majoritários encontrados foram torularrodina, toruleno, ³-caroteno e ²-caroteno. Os teores totais de carotenóides, em µg/g, foram de 251,7 em R. glutinis,123,5 em R. rubra,113,2 em R. araucariae,105,8 em R. lactosa ede 103,7 em R. minuta.A method for extraction and HPLC separation of carotenoids from fiveRhodotorula strains was optimized. The extraction by mechanical disruption of the yeast cell wall with fine treated sand was shown to be more efficient than chemical disruption with dimethylsulfoxide. The carotenoids were separated and quantified by HPLC on a C18 column using as mobile phase acetonitrile/methanol (0.1% triethylamina/ethyl acetate (75:15:10 with 100% methanol (0.1% triethylamine between the injections, at a flow rate of 1.0 mL/min. In all strains, the major carotenoids found were torularhodin, torulene, ³-carotene and ²-carotene. The total carotenoid contents, in µg/g, obtained were 251.7 for R. glutinis,123.5 for R. rubra,113.2 for R. araucariae,105.8 for R. lactosaand 103.7 for R. minuta.

  20. A Validated Stability-Indicating HPLC Method for Simultaneous Determination of Amoxicillin and Enrofloxacin Combination in an Injectable Suspension

    Directory of Open Access Journals (Sweden)

    Nidal Batrawi

    2017-02-01

    Full Text Available The combination of amoxicillin and enrofloxacin is a well-known mixture of veterinary drugs; it is used for the treatment of Gram-positive and Gram-negative bacteria. In the scientific literature, there is no high-performance liquid chromatography (HPLC-UV method for the simultaneous determination of this combination. The objective of this work is to develop and validate an HPLC method for the determination of this combination. In this regard, a new, simple and efficient reversed-phase HPLC method for simultaneous qualitative and quantitative determination of amoxicillin and enrofloxacin, in an injectable preparation with a mixture of inactive excipients, has been developed and validated. The HPLC separation method was performed using a reversed-phase (RP-C18e (250 mm × 4.0 mm, 5 μm column at room temperature, with a gradient mobile phase of acetonitrile and phosphate buffer containing methanol at pH 5.0, a flow rate of 0.8 mL/min and ultraviolet detection at 267 nm. This method was validated in accordance with the Food and Drug Administration (FDA and the International Conference on Harmonisation (ICH guidelines and showed excellent linearity, accuracy, precision, specificity, robustness, ruggedness, and system suitability results within the acceptance criteria. A stability-indicating study was also carried out and indicated that this method can also be used for purity and degradation evaluation of these formulations.

  1. Quickly Screening for Potential α-Glucosidase Inhibitors from Guava Leaves Tea by Bioaffinity Ultrafiltration Coupled with HPLC-ESI-TOF/MS Method.

    Science.gov (United States)

    Wang, Lu; Liu, Yufeng; Luo, You; Huang, Kuiying; Wu, Zhenqiang

    2018-02-14

    Guava leaves tea (GLT) has a potential antihyperglycemic effect. Nevertheless, it is unclear which compound plays a key role in reducing blood sugar. In this study, GLT extract (IC 50 = 19.37 ± 0.21 μg/mL) exhibited a stronger inhibitory potency against α-glucosidase than did acarbose (positive control) at IC 50 = 178.52 ± 1.37 μg/mL. To rapidly identify the specific α-glucosidase inhibitor components from GLT, an approach based on bioaffinity ultrafiltration combined with high performance liquid chromatography coupled to electrospray ionization-time-of-flight-mass spectrometry (BAUF-HPLC-ESI-TOF/MS) was developed. Under the optimal bioaffinity ultrafiltration conditions, 11 corresponding potential α-glucosidase inhibitors with high affinity degrees (ADs) were screened and identified from the GLT extract. Quercetin (IC 50 = 4.51 ± 0.71 μg/mL) and procyanidin B3 (IC 50 = 28.67 ± 5.81 μg/mL) were determined to be primarily responsible for the antihyperglycemic effect, which further verified the established screening method. Moreover, structure-activity relationships were discussed. In conclusion, the BAUF-HPLC-ESI-TOF/MS method could be applied to determine the potential α-glucosidase inhibitors from complex natural products quickly.

  2. Assessment of radiochemical purity of [{sup 18}F]fludeoxyglucose by high pressure liquid chromatography (HPLC)

    Energy Technology Data Exchange (ETDEWEB)

    Lacerda, Aline E.; Silva, Juliana B.; Silveira, Marina B.; Ferreira, Soraya Z., E-mail: radiofarmacoscdtn@cdtn.b [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil). Unidade de Pesquisa e Producao de Radiofarmacos

    2011-07-01

    The quality control of [{sup 18}F]fludeoxyglucose ({sup 18}FDG) has received attention due to its increasing clinical use. Although the quality requirements of {sup 18}FDG are established in various pharmacopoeia, the suitability of all testing methods used should be verified under actual conditions of use and documented. The aim of this study was to develop a high pressure liquid chromatography (HPLC) method for radiochemical purity evaluation of {sup 18}FDG, based on pharmacopoeia references, and to verify its suitability for routine quality control in our centre. HPLC analysis was performed with an Agilent HPLC. {sup 18}FDG and impurities were separated on an anion-exchange column by isocratic elution with 0.1 M NaOH as the mobile phase. Detection was accomplished with refractive index and NaI (Tl) scintillation detectors. The flow rate of the mobile phase was set at 0.8 mL/min and the column temperature was kept at 35 deg C. Specificity, linearity, precision and robustness were assessed to verify if the method was adequate for its intended purpose. Retention time of {sup 18}FDG was not affected by the presence of other components of the formulation and a good peak resolution was achieved. The analytical curve of {sup 18}FDG was linear, with a correlation coefficient value of 0.9995. Intraday repeatable precision, reported as the relative standard deviation, was 0.11%. Analytical procedure remained unaffected by small variations in mobile phase flow rate. Results evidenced that HPLC is suitable for radiochemical purity evaluation of {sup 18}FDG, considering operational conditions of our laboratory. (author)

  3. Size exclusion HPLC of proteins for evaluation of durum wheat quality

    Science.gov (United States)

    The present research aimed to assess size exclusion HPLC (SE-HPLC) in protein molecular weight distribution determination for quality evaluation of durum semolina. Semolina samples were milled from 13 durum genotypes grown at 7 locations in 2009 and 2010 in ND. Sodium dodecyl sulfate (SDS) buffer ...

  4. Chemical Differentiation of Dendrobium officinale and Dendrobium devonianum by Using HPLC Fingerprints, HPLC-ESI-MS, and HPTLC Analyses

    Science.gov (United States)

    Ye, Zi; Dai, Jia-Rong; Zhang, Cheng-Gang; Lu, Ye; Wu, Lei-Lei; Gong, Amy G. W.; Wang, Zheng-Tao

    2017-01-01

    The stems of Dendrobium officinale Kimura et Migo (Dendrobii Officinalis Caulis) have a high medicinal value as a traditional Chinese medicine (TCM). Because of the limited supply, D. officinale is a high priced TCM, and therefore adulterants are commonly found in the herbal market. The dried stems of a closely related Dendrobium species, Dendrobium devonianum Paxt., are commonly used as the substitute; however, there is no effective method to distinguish the two Dendrobium species. Here, a high performance liquid chromatography (HPLC) method was successfully developed and applied to differentiate D. officinale and D. devonianum by comparing the chromatograms according to the characteristic peaks. A HPLC coupled with electrospray ionization multistage mass spectrometry (HPLC-ESI-MS) method was further applied for structural elucidation of 15 flavonoids, 5 phenolic acids, and 1 lignan in D. officinale. Among these flavonoids, 4 flavonoid C-glycosides were firstly reported in D. officinale, and violanthin and isoviolanthin were identified to be specific for D. officinale compared with D. devonianum. Then, two representative components were used as chemical markers. A rapid and reliable high performance thin layer chromatography (HPTLC) method was applied in distinguishing D. officinale from D. devonianum. The results of this work have demonstrated that these developed analytical methods can be used to discriminate D. officinale and D. devonianum effectively and conveniently. PMID:28769988

  5. HPLC-MS/MS measurement of radiation and photo-induced damage in cellular DNA and human skin

    International Nuclear Information System (INIS)

    Cadet, Jean; Douki, Thierry; Ravanat, Jean-Luc

    2010-01-01

    Full text: The measurement of damage induced in cellular DNA by ionizing and solar radiations is of major importance to assess the molecular mode of action and the biological role (mutagenesis, DNA repair) of these genotoxic agents. For this purpose several analytical approaches including immunodetection, post-labeling and chromatographic assays have been designed. However most of them have been shown to suffer from a lack of specificity, sensitivity or quantitative response. It may be noted that the gas-chromatography method in its basal version has been found to lead to overestimated yields of oxidatively generated base lesions by two to three order of magnitude due to the occurrence of artifactual oxidation of the overwhelming purine and pyrimidine bases during the derivatization step of the assay. The advent of HPLC coupled to tandem mass spectrometry operating in the electrospray ionization mode has allowed overcoming most of these drawbacks. Thus, accurate determination of 11 oxidized bases and nucleosides has been achieved in cellular DNA upon exposure to radiation-induced hydroxyl radical and one-electron oxidation agents. This has involved quantitative enzymatic release of lesions from extracted DNA and their accurate detection at the output of the HPLC column using the highly quantitative isotopic dilution technique. Evidence was also provided for the generation of five clustered lesions that all involve a base modification and an altered 2-deoxyribose residue as the result of only one initial radical oxidation hit. These consist of (5'R)-5',8-cyclo-2'-deoxyadenosine and cytosinealdehyde adducts that arise from .OH-mediated hydrogen abstraction at C5 and C4 of the sugar moiety of cellular DNA respectively. The damaging effects of UVA radiation on cellular DNA and human skin were rationalized in terms of predominant 1 O 2 -mediated formation of 8-oxo-7,8-dihydro-2'-deoxyguanosine. Other relevant types of DNA modifications consist in bipyrimidine

  6. Lack of evidence from HPLC 32P-post-labelling for tamoxifen-DNA adducts in the human endometrium.

    Science.gov (United States)

    Carmichael, P L; Sardar, S; Crooks, N; Neven, P; Van Hoof, I; Ugwumadu, A; Bourne, T; Tomas, E; Hellberg, P; Hewer, A J; Phillips, D H

    1999-02-01

    Tamoxifen is associated with an increased incidence of endometrial cancer in women. It is also a potent carcinogen in rat liver and forms covalent DNA adducts in this tissue. A previous study exploring DNA adducts in human endometria, utilizing thin layer chromatography 32P-postlabelling, found no evidence for adducts in tamoxifen-treated women [Carmichael,P.L., Ugwumadu,A.H.N., Neven,P., Hewer,A.J., Poon,G.K. and Phillips,D.H. (1996) Cancer Res., 56, 1475-1479]. However, subsequent work utilizing HPLC 32P-post-labelling [Hemminki,K., Ranjaniemi,H., Lindahl,B. and Moberger,B. (1996) Cancer Res., 56, 4374-4377] suggested that very low levels could be detected. We have sought to investigate this question further by reproducing the HPLC methodology at two centres, and analysing endometrial DNA from 20 patients treated with 20 mg/day tamoxifen for between 22 and 65 months. Liver DNA isolated from tamoxifen-treated rats was used as a positive control. We found no convincing evidence for tamoxifen-derived DNA adducts in human endometrium. HPLC elution profiles of post-labelled DNA from tamoxifen-treated women were indistinguishable from those obtained with DNA from 14 untreated women and from six women taking toremifene, an analogue of tamoxifen.

  7. HPLC-DAD analysis, antioxidant potential and anti-urease activity of Asparagus gracilis collected from District Islamabad.

    Science.gov (United States)

    Shah, Naseer Ali; Khan, Muhammad Rashid; Sattar, Saadia; Ahmad, Bushra; Mirza, Bushra

    2014-09-23

    Asparagus gracilis subspecie of Asparagus capitatus Baker, is described as food and medicine for various ailments. In this study we investigated, its phenolic constituents, in vitro antioxidant potential against various free radicals and anti-urease potential. Asparagus gracilis aerial parts collected from District Islamabad, Pakistan were extracted with crude methanol which was further fractionated into n-hexane, ethyl acetate, n-butanol and aqueous fraction. Total phenolic and flavonoid contents were estimated for extract and all the derived fractions. Diverse in vitro antioxidants assays such as DPPH, H2O2, •OH, ABTS, β-carotene bleaching assay, superoxide radical, lipid peroxidation, reducing power, and total antioxidant capacity were studied to assess scavenging potential. Antiurease activity of methanol extract and its derived fractions was also investigated. HPLC-DAD analysis of crude methanol extract was performed by using different phenolic standards. Ethyl acetate fraction expressed maximum content of flavonoids (240.6 ± 6.1 mg RE/g dry sample), phenolics (615 ± 13 mg GAE/g dry sample) and best antioxidant potential among different fractions of crude methanol extract. Hydrogen peroxide assay and hydroxyl, supeoxide, nitric oxide free radicals antioxidant assays as well as beta carotene assay showed significant correlation with flavonoid content while hydrogen peroxide, ABTS and lipid peroxidation assay displayed significant correlation with phenolic content. HPLC analysis showed the presence of important phenolics i.e. catechin (4.04 ± 0.02 μg/mg sample), caffeic acid (0.89 ± 0.003 μg/mg sample), rutin (24.58 ± 0.1 μg/mg sample), myricetin (1.13 ± 0.07 μg/mg sample) and quercetin (14.91 ± 0.09 μg/mg sample). Ethyl acetate fraction expressed lowest IC50 in antiurease activity. Correlation analysis of antiurease activity expressed significant correlation with flavonoids (P < 0.004) and phenolics (P < 0.02) proposing multipotent activity of

  8. Relationships among depression during pregnancy, social support and health locus of control among Iranian pregnant women.

    Science.gov (United States)

    Moshki, Mahdi; Cheravi, Khadijeh

    2016-03-01

    Prenatal depression is a significant predictor of postpartum depression and is detrimental to fetal development. To examine whether depression during pregnancy is associated with social support and health locus of control (HLC). Data were collected from a sample of 208 Iranian pregnant women using a demographic questionnaire, the Edinburgh Postnatal Depression Scale, the multidimensional HLC Scale and the social support appraisals. Depression was experienced by 37% of participants. Overall, women reported higher level of family support (6.88 ± 1.15) than other supports (6.87 ± 1.29). Protective supports from other resources (6.87 ± 1.29) were higher than those from friends (5.94 ± 1.5). Internal, powerful others and chance beliefs had the highest mean scores. Social support and chance HLC significantly influenced the proposed mediator (depressive mood) in the linear regression model. Bivariate analysis showed significant associations between social support (friend, family and others) and depressive mood. Internal HLC had a significant association with social support and powerful others HLC. However, Pearson correlation coefficient was not significant between depressive mood and all dimensions of HLC. Clinicians could assess social support and chance HLC to identify and treat women at risk of prenatal depression. By providing support during pregnancy, depression levels in women and its effects on the fetus may be decreased, which could prevent postpartum depression. © The Author(s) 2015.

  9. Health-related behavior, profile of health locus of control and acceptance of illness in patients suffering from chronic somatic diseases.

    Directory of Open Access Journals (Sweden)

    Konrad Janowski

    Full Text Available PURPOSE: The purpose of the study was to determine health-related behaviors, profile of health locus of control (HLC, and to assess the relationships between these constructs among patients suffering from chronic somatic diseases. MATERIAL AND METHODS: Three-hundred adult patients suffering from various chronic diseases participated in the study. The patients' mean age was 54.6 years (SD = 17.57. RESULTS: No statistically significant differences were found between the different clinical groups in health-related behavior, acceptance of illness, internal HLC or chance HLC. Patients with neurologic conditions showed slightly lower powerful others HLC than did some other clinical groups. Health-related behavior was significantly positively related to all three categories of HLC, with most prominent associations observed with powerful others HLC. Only one type of health-related behavior--preventive behavior--correlated significantly and negatively with acceptance of illness. Differences in the frequency of health-related behavior were also found due to gender (women showing more healthy nutritional habits than men, age (older subjects showing more frequent health-promoting behavior, education (higher education was associated with less frequent health-promoting behavior and marital status (widowed subjects reporting more frequent health-promoting behavior. CONCLUSIONS: Health-related behavior in patients with chronic diseases seems to be unrelated to a specific diagnosis; however it shows associations with both internal and external HLC. Sociodemographic factors are also crucial factors determining frequency of health-related behavior in such patients.

  10. Determination of some psychotropic drugs in serum and saliva samples by HPLC-DAD and HPLC MS.

    Science.gov (United States)

    Petruczynik, A; Wróblewski, K; Szultka-Młyńska, M; Buszewski, B; Karakuła-Juchnowicz, H; Gajewski, J; Morylowska-Topolska, J; Waksmundzka-Hajnos, M

    2016-08-05

    A simple, rapid and sensitive HPLC-DAD method has been developed and validated for the simultaneous determination of seven psychotropic drugs (risperidone, citalopram, clozapine,quetiapine, levomepromazine, perazine and aripiprazole) in human serum or saliva samples. The chromatographic analyses were performed on a XSELECT CSH Phenyl-Hexyl column with a mobile phase containing methanol, acetate buffer at pH 3.5 and 0.025mL(-1) diethylamine. The influence of concentration of methanol in injection samples and injection volume on peak symmetry and system efficiency was examined.The full separation of all investigated drugs, good peaks' symmetry and simultaneously high systems efficiency were obtained in applied chromatographic system. The method is suitable for the analysis of investigated drugs in human plasma or saliva for psychiatric patients for control of pharmacotherapy, particularly in combination therapy. HPLC-MS was applied for verification of the presence of drugs and their metabolites in serum and saliva samples from patients. Copyright © 2016 Elsevier B.V. All rights reserved.

  11. ANALISIS LAYANAN VOIP PADA JARINGAN MANET DENGAN CODEC YANG BERBEDA

    Directory of Open Access Journals (Sweden)

    Randa Oktavada Zein

    2016-12-01

    Full Text Available Voice Over Internet Protocol (VoIP merupakan layanan bersifat real-time, parameter yang dapat mempengaruhi kulitas layanan seperti delay, jitter dan packet loss. Dalam proses pengkodean sinyal analog menjadi sinyal digital menyebabkan terjadiya delay pada VoIP. Sistem pengcodean ini disebut codec, setiap codec memiliki bitrate yang berbeda pengkodeannya. Pada penelitian ini menggunakan codec G.711, G729 dan codec G.723.1 sebagai perbandingan untuk mengetahui qulity of service (QoS VoIP jika diterapkan pada jaringan MANET. Dengan penambahan aplikasi Hypertext Transfer Protovol (HTTP untuk mendapatkan parameter QoS VoIP dari codec G.711, G.729 dan G.723.1. Hasil yang didapat pada codec G.723.1 lebih baik jika dibandingkan dengan codec g.711 dan G.729 dilihat dari nilai dari parameter QoS seperti delay, jitter dan packet loss. Sesuai standar ITU-T G114 dimana perhitunan teoritis parameter dari codec G.723.1 didapat hasil terendah 7,68 kbps.

  12. Target-guided isolation and purification of antioxidants from Selaginella sinensis by offline coupling of DPPH-HPLC and HSCCC experiments.

    Science.gov (United States)

    Zhang, Yuping; Shi, Shuyun; Wang, Yuanxi; Huang, Kelong

    2011-01-15

    Selaginella sinensis (Selaginellaceae) is used extensively in traditional Chinese medicine (TCM) for the treatment of many kinds of chronic diseases. In this study, fractionation of the methanol extract of S. sinensis by different polarity solvents indicated the ethyl acetate fraction exhibited an potent 1,1-diphenyl-2-picryhydrazyl (DPPH) radical scavenging activity with the IC(50) value of 44.9 μM. In order to evaluate the scientific basis, antioxidant peaks were firstly screened using DPPH spiking test through high performance liquid chromatography (DPPH-HPLC). Under the target-guidance of DPPH-HPLC experiment, two flavonoids and six biflavonoids, quercetin (1), apigenin (2), amentoflavone (3), robustaflavone (4), 2,3-dihydroamentaflavone (5), hinokiflavone (6), 4'-O-methyl-robustaflavone (7) and ginkgetin (8) were separated by high-speed counter-current chromatography (HSCCC) method using n-hexane-ethyl acetate-methanol-water (8:8:9:7) as the solvent system with purities 98.2%, 97.6%, 99.4%, 92.3%, 98.5%, 98.9% and 99.6%, respectively. The structures were identified by electrospray ionization mass spectrometry (ESI-MS) and nuclear magnetic resonance (NMR) analysis. Antioxidant activity of eight isolated compounds was assessed by the radical scavenging effect on DPPH radical, compound 1 showed strongest antioxidant activities with IC(50) values of 3.2 μM, while compounds 2-8 showed weak antioxidant activities. This is the first report on simultaneous separation of eight antioxidant compounds from S. sinensis by HSCCC, moreover, apigenin and 4'-O-methyl-robustaflavone were first identified from this plant. Results of the present study indicated that the combinative method using DPPH-HPLC and HSCCC could be widely applied for rapid screening and isolating of antioxidants from complex TCM extract. Copyright © 2010. Published by Elsevier B.V.

  13. OPTIMIZATION OF A HPLC ANALYSIS METHOD FOR TAURINE AND CAFFEINE IN ENERGY DRINKS

    Directory of Open Access Journals (Sweden)

    RALUCA-IOANA [CHIRITA] TAMPU

    2018-03-01

    Full Text Available This paper presents the optimization of a rapid, inexpensive, reliable and selective isocratic high performance liquid chromatographic (HPLC method for the simultaneous determination of caffeine and taurine in energy drinks with two common detectors in series: evaporating light scattering detector (ELSD and an ultraviolet (UV detector. Satisfactory analysis results were obtained on an Astec apHera NH2 column using methanol/water (30:70 v/v as mobile phase. The optimized method was used for the analysis of commercial energy drinks containing large amounts of carbohydrates (100 g·L-1 and considerably lower amounts of taurine and caffeine (4 and 0.6 g·L-1, respectively. The advantages of this method consist of its lack of preliminary samples treatment and also the fact that basic LC instrumentation was employed.

  14. Determination of bisphenol A in thermal printing papers treated by alkaline aqueous solution using the combination of single-drop microextraction and HPLC.

    Science.gov (United States)

    Gao, Leihong; Zou, Jing; Liu, Haihong; Zeng, Jingbin; Wang, Yiru; Chen, Xi

    2013-04-01

    A method for the quantitative determination of bisphenol A in thermal printing paper was developed and validated. Bisphenol A was extracted from the paper samples using 2% NaOH solution, then the extracted analyte was enriched using single-drop microextraction followed by HPLC analysis. Several parameters relating to the single-drop microextraction efficiency including extraction solvent, extraction temperature and time, stirring rate, and pH of donor phase were studied and optimized. Spiked recovery of bisphenol A at 20 and 5 mg/g was found to be 95.8 and 108%, and the method detection limit and method quantification limit was 0.03 and 0.01 mg/g, respectively. Under the optimized conditions, the proposed method was applied to the determination of bisphenol A in seven types of thermal printing paper samples, and the concentration of bisphenol A was found in the range of 0.53-20.9 mg/g. The considerably minimum usage of organic solvents (5 μL 1-octanol) and high enrichment factor (189-197) in the sample preparation are the two highlighted advantages in comparison with previously published works. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Improvement of Nicotinic Acid and Nicotinamide Analysis in Meats and Meat Products by HPLC and LC-MS/MS with Solid-Phase Extraction.

    Science.gov (United States)

    Hiki, Asako; Yamajima, Yukiko; Uematsu, Yoko

    2016-01-01

    A method for nicotinic acid (NA) and nicotinamide (NAA) analysis in meats was developed. NA and NAA were extracted from meats or meat products with metaphosphate aqueous solution. The extract was cleaned up with an Oasis MCX cartridge. The cartridge was washed with 2% acetic acid (v/v) and acetic acid-methanol solution. NA and NAA were eluted with ammonia-methanol solution. NA and NAA in the eluate were chromatographed on a Scherzo SM-C18 (3.0×150 mm, 3.0 μm) column with 20 mmol/L ammonium acetate containing 0.1% acetic acid-acetonitrile (97 : 3) as a mobile phase and were monitored at 261 nm. Quantification was performed by LC and LC-MS/MS. Calibration curves showed high linearity (correlation coefficient>0.998) between 1-25 μg/mL for LC and LC-MS/MS. Recoveries were 84-108% (CV≦5.8%) by HPLC and 79-105% (CV≦9.0%) by LC-MS/MS. The limit of quantitation for NA was 0.005-0.01 g/kg and that for NAA was 0.01-0.02 g/kg.

  16. 1.8 cineole decreases gastric compliance in anesthetized rats 1.8 cineol diminui a complacência gástrica de ratos anestesiados

    Directory of Open Access Journals (Sweden)

    José Ricardo Cunha Neves

    2007-02-01

    Full Text Available PURPOSE: To study the effect of 1,8 cineoleee components of the essencial oil of Croton nepetaefolius - plant of North-East of Brasil, used in the popular medicine for riots of the gastrointestinal tract - on the motor behavior of the gut of Wistar rats. METHODS: Used 16 male animals under jejun of 24h weighing 300-350g. The effect of 1.8 cineoleee (1 or 3mg/Kg on gastric compliance had been lead in anaesthetized rats. The variations of the gastric volume (GV, had been measured by plethysmography, while AP, HR and CVP had been monitored continuously by a digital system of data acquisition. RESULTS: Observe reduction of the GV, which was significant on 30, 40, 50 and 60min after treatment (2.0±0.1; 1.9±0.1; 1.8±0.1 and 1.7±0.1mL, versus 2.1±0.2mL. The AP presented significant fall after the administration of 1.8 cineoleee, remaining thus during 60min of monitorization (87.9±7.7; 87.6±7.1; 87.9±6.4; 87.8±5.7; 86.0±5.5 and 87.7±6.0mmHg, respectively versus 94.4±6.2 mmHg, as well as the HR (366.3±13.4; 361.7±11.5; 357.3±10.4; 353.0±10.4; 348.3±11.1 and 350.4±13.7bpm, respectively versus 395.2±11.1bpm. The CVP did not suffer significant variations after treatment. CONCLUSION: Observe the 1.8 cineoleee reduces the gastric compliance in anaesthetized rats besides presenting effect hipotensor and bradicardic; probably for direct action on the gastrointestinal and vascular smooth muscel and moduling the autonomic nervous system.OBJETIVO: Estudar o efeito do 1.8 cineol, componente do Cróton nepetaefolius (planta do Nordeste comumente usada na medicina popular para distúrbios do trato gastrintestinal (TGI, sobre o comportamento motor do TGI de ratos Wistar anestesiados. MÉTODOS: Utilizamos 16 animais machos, pesando entre 300 a 350g. Os estudos de complacência gástrica foram conduzidos em animais sob jejum de 24h. As variações do volume gástrico (VG, foram medidas por pletismografia, enquanto a PA, FC e PVC foram monitoradas

  17. An HPLC-DAD method to quantification of main phenolic compounds from leaves of Cecropia species

    Energy Technology Data Exchange (ETDEWEB)

    Costa, Geison M.; Ortmann, Caroline F.; Schenkel, Eloir P.; Reginatto, Flavio H., E-mail: freginatto@hotmail.co [Universidade Federal de Santa Catarina (UFSC), Florianopolis (Brazil). Centro de Ciencias da Saude. Dept. de Ciencias Farmaceuticas

    2011-07-01

    An efficient and reproducible HPLC-DAD method was developed and validated for the simultaneous quantification of major compounds (chlorogenic acid, isoorientin, orientin and isovitexin) present in the leaves of two Cecropia species, C. glaziovii and C. pachystachya. From the leaves of C. glaziovii and C. pachystachya were isolated the C-glycosylflavones isoorientin and isovitexin and identified on both species chlorogenic acid (3-O-caffeoylquinic acid) and the O-glycosylflavonol isoquercitrin. The C-glycosylflavone orientin was isolated only from C. pachystachya. Chlorogenic acid was the major compound in both species (11.1 mg g{sup -1} of extract of C. glaziovii and 27.2 mg g{sup -1} of extract of C. pachystachya) and for the flavonoids quantified, isovitexin was the main C-glycosylflavonoid for C. glaziovii (4.6 mg g{sup -1} of extract) and isoorientin the main one for C. pachystachya (17.3 mg g{sup -1} of extract). (author)

  18. An HPLC-DAD method to quantification of main phenolic compounds from leaves of Cecropia species

    International Nuclear Information System (INIS)

    Costa, Geison M.; Ortmann, Caroline F.; Schenkel, Eloir P.; Reginatto, Flavio H.

    2011-01-01

    An efficient and reproducible HPLC-DAD method was developed and validated for the simultaneous quantification of major compounds (chlorogenic acid, isoorientin, orientin and isovitexin) present in the leaves of two Cecropia species, C. glaziovii and C. pachystachya. From the leaves of C. glaziovii and C. pachystachya were isolated the C-glycosylflavones isoorientin and isovitexin and identified on both species chlorogenic acid (3-O-caffeoylquinic acid) and the O-glycosylflavonol isoquercitrin. The C-glycosylflavone orientin was isolated only from C. pachystachya. Chlorogenic acid was the major compound in both species (11.1 mg g -1 of extract of C. glaziovii and 27.2 mg g -1 of extract of C. pachystachya) and for the flavonoids quantified, isovitexin was the main C-glycosylflavonoid for C. glaziovii (4.6 mg g -1 of extract) and isoorientin the main one for C. pachystachya (17.3 mg g -1 of extract). (author)

  19. 8q24 rs6983267G variant is associated with increased thyroid cancer risk

    Science.gov (United States)

    Sahasrabudhe, Ruta; Estrada, Ana; Lott, Paul; Martin, Lynn; Echeverry, Guadalupe Polanco; Velez, Alejandro; Neta, Gila; Takahasi, Meiko; Saenko, Vladimir; Mitsutake, Norisato; Jaeguer, Emma; Duque, Carlos Simon; Rios, Alejandro; Bohorquez, Mabel; Prieto, Rodrigo; Criollo, Angel; Echeverry, Magdalena; Tomlinson, Ian; Carvajal Carmona, Luis G.

    2015-01-01

    The G allele of the rs6983267 single nucleotide polymorphism, located on chromosome 8q24, has been associated with increased risk of several cancer types. The association between rs6983267G and thyroid cancer has been tested in different populations, mostly of European ancestry, and has led to inconclusive results. While significant associations have been reported in the British and Polish populations, no association has been detected in populations from Spain, Italy and the USA. To further investigate the role of rs6983267G in thyroid cancer susceptibility, we evaluated rs6983267 genotypes in three populations of different continental ancestry (British Isles, Colombia and Japan), providing a total of 3,067 cases and 8,575 controls. We detected significant associations between rs6983267G and thyroid cancer in the British Isles (Odds Ratio, OR= 1.19, 95% confidence interval, CI: 1.11–1.27, P= 4.03 × 10−7), Japan (OR= 1.20, 95% CI: 1.03–1.41, P= 0.022) and a borderline significant association of similar effect direction and size in Colombia (OR= 1.19, 95% CI: 0.99–1.44, P= 0.069). A meta-analysis of our multi-ethnic study and previously published non-overlapping datasets, which included a total of 5,484 cases and 12,594 controls, confirmed the association between rs6983267G and thyroid cancer (P= 1.23 × 10−7, OR= 1.13, 95% CI: 1.07–1.18). Our results therefore support the notion that rs6983267G is a bona fide thyroid cancer risk variant that increases the risk of disease by ~13%. PMID:26290501

  20. Antioxidant, Biomolecule Oxidation Protective Activities of Nardostachys jatamansi DC and Its Phytochemical Analysis by RP-HPLC and GC-MS

    Directory of Open Access Journals (Sweden)

    Sakina Razack

    2015-03-01

    Full Text Available The study aimed at analyzing the metabolite profile of Nardostachys jatamansi using RP-HPLC, GC-MS and also its antioxidant, biomolecule protective and cytoprotective properties. The 70% ethanolic extract of Nardostachys jatamansi (NJE showed the presence of polyphenols and flavonoids (gallic acid, catechin, chlorogenic acid, homovanillin, epicatechin, rutin hydrate and quercetin-3-rhamnoside analyzed by RP-HPLC, whereas hexane extract revealed an array of metabolites (fatty acids, sesquiterpenes, alkane hydrocarbons and esters by GC-MS analysis. The antioxidant assays showed the enhanced potency of NJE with a half maximal inhibitory concentration (IC50 value of 222.22 ± 7.4 μg/mL for 2,2-diphenyl-1-picrylhydrazyl (DPPH, 13.90 ± 0.5 μg/mL for 2,2′-azino-bis(3-ethyl benzothiazoline-6-sulfonic acid diammonium salt (ABTS, 113.81 ± 4.2 μg/mL for superoxide, 948 ± 21.1 μg/mL for metal chelating and 12.3 ± 0.43 mg FeSO4 equivalent/g of extract for ferric reducing antioxidant power assays and was more potent than hexane extract. NJE effectively inhibited 2,2′-azobis(2-methylpropionamidine dihydrochloride (AAPH-induced oxidation of biomolecules analyzed by pBR322 plasmid DNA damage, protein oxidation of bovine serum albumin and lipid peroxidation assays. The observed effects might be due to the high content of polyphenols, 53.06 ± 2.2 mg gallic acid equivalents/g, and flavonoids, 25.303 ± 0.9 mg catechin equivalents/g, of NJE compared to the hexane fraction. Additionally, the extract abrogated the protein, carbonyl, and ROS formation, and NJE showed cytotoxicity in SH-SY5Y neuronal cells above 75 μg/mL. Thus, the study suggests that the herb unequivocally is a potential source of antioxidants and could aid in alleviating oxidative stress-mediated disorders.

  1. [Separation and identification of beta-carotene and its cis isomers by high pressure liquid chromatography (HPLC)].

    Science.gov (United States)

    Carrillo de Padilla, F

    1996-06-01

    The separation and identification by HPLC of the cis isomers of beta-carotene was studied. A 1.26 mg/ml beta-carotene solution previously isomerized with iodine as a catalyst, was eluted with 2% acetone in hexane, from a Ca(OH)2 chromatographic column in three bands. The fractions were identified by spectrophotometry and the retention times of 2.05, 2.4 and 2.8 min for the 13 cis, all-trans, and 9 cis beta-carotene isomers, determined by HPLC, with 1% acetone in hexane as movil phase. 22.13 mg % of all-trans beta-carotene were found in a sample of canned carrots. It is recommended the analyses of a greater number of samples, the determination of the method's sensitivity, reproductibility, and the use of a standard of reference of a response factor for calculations.

  2. Separation and identification of beta-carotene and its cis isomers by high pressure liquid chromatography (HPLC)

    International Nuclear Information System (INIS)

    Carrillo de Padilla, F.

    1996-01-01

    The separation and identification by HPLC of the cis isomers of beta-carotene was studied. A 1.26 mg/ml beta-carotene solution previously isomerized with iodine as a catalyst, was eluted with 2% acetone in hexane, from a Ca(OH)2 chromatographic column in three bands. The fractions were identified by spectrophotometry and the retention times of 2.05, 2.4 and 2.8 min for the 13 cis, all-trans, and 9 cis beta-carotene isomers, determined by HPLC, with 1% acetone in hexane as Mobil phase. 22.13 mg % of all-trans beta-carotene were found in a sample of canned carrots. It is recommended the analyses of a greater number of samples, the determination of the method's sensitivity, reproducibility, and the use of a standard of reference of a response factor for calculations

  3. Antioxidant capacity and phenolic compounds of Lonicerae macranthoides by HPLC-DAD-QTOF-MS/MS.

    Science.gov (United States)

    Hu, Xin; Chen, Lin; Shi, Shuyun; Cai, Ping; Liang, Xuejuan; Zhang, Shuihan

    2016-05-30

    Lonicerae macranthoides with strong antioxidant activity is commonly used in traditional Chinese medicine and folk tea/beverage. However, detailed information about its antioxidant activity and bioactive compounds is limited. Then at first, we comparatively evaluated total phenolic content (TPC), total flavonoid content (TFC) and antioxidant activities of water extract, petroleum ether, ethyl acetate and n-butanol fractions of L. macranthoides. Ethyl acetate fraction exhibited the highest level of TPC (207.38 mg GAE/g DW), TFC (53.06 mg RE/g DW) and the best DPPH scavenge activity and reducing power. n-Butanol fraction showed the best ABTS(+) and O2(-) scavenging activities. Interestingly, water extract, ethyl acetate and n-butanol fractions showed stronger antioxidant activities than positive control, butylated hydroxytoluene (BHT). After that, thirty-one antioxidant phenolic compounds, including twenty-two phenolic acids and nine flavonoids, were screened by DPPH-HPLC experiment and then identified using HPLC-DAD-QTOF-MS/MS. It is noted that twenty-one compounds (1, 3-4, 6-17, 19, 23, 26, 28-29, and 31), as far as was known, were discovered from L. macranthoide for the first time, and eleven of them (3-4, 10-17, and 23) were reported in Lonicera species for the first time. Results indicated that L. macranthoides could serve as promising source of rich antioxidants in foods, beverages and medicines for health promotion. Copyright © 2016 Elsevier B.V. All rights reserved.

  4. Determination of 5-fluorouracil in plasma with HPLC-tandem mass spectrometry

    NARCIS (Netherlands)

    van Kuilenburg, A. B. P.; van Lenthe, H.; Maring, J. G.; van Gennip, A. H.

    2006-01-01

    In this article, we describe a fast and specific method to measure 5FU with HPLC tandem-mass spectrometry. Reversed-phase HPLC was combined with electrospray ionization tandem mass spectrometry and detection was performed by multiple-reaction monitoring. Stable-isotope-labeled 5FU (1,3-15N2-5FU) was

  5. Simultaneous Chloramphenicol and Florfenicol Determination by A Validated DLLME-HPLC-UV Method in Pasteurized Milk

    OpenAIRE

    Karami-Osboo, Rouhollah; Miri, Ramin; Javidnia, Katayoun; Kobarfard, Farzad

    2016-01-01

    The antibiotic residues in milk are a well-known serious problem and pose several health hazards to consumers. We have described a simple, rapid, and inexpensive DLLME-HPLC/UV technique for the extraction of chloramphenicol and florfenicol residues in milk samples. Under the optimum conditions, linearity of the method was observed over the range 0.02-0.85 ?g/L with correlation coefficients > 0.999. The proposed method has been found to have a good limit of detection (signal to noise ratio = 3...

  6. Level of 8-OHdG in drained dialysate appears to be a marker of peritoneal damage in peritoneal dialysis

    Directory of Open Access Journals (Sweden)

    Morishita Y

    2011-12-01

    Full Text Available Yoshiyuki Morishita, Minami Watanabe, Ichiro Hirahara, Tetsu Akimoto, Shigeaki Muto, Eiji KusanoDivision of Nephrology, Department of Medicine, Jichi Medical University, Tochigi, JapanPurpose: Peritoneal dialysis (PD is a successful renal replacement therapy; however, long-term PD leads to structural and functional peritoneal damage. Therefore, the monitoring and estimation of peritoneal function are important in PD patients. Oxidative stress has been implicated as one possible mechanism of peritoneal membrane damage. The aim of this study was to evaluate the association between an oxidative stress marker, 8-hydroxydeoxyguanosine (8-OHdG, and peritoneal damage in PD patients.Methods: The authors evaluated 8-OHdG in drained dialysate by enzyme immunoassay to investigate the association between 8-OHdG and solute transport rate estimated by peritoneal equilibration test and matrix metalloproteinase-2 (MMP-2 level in 45 samples from 28 PD patients.Results: The 8-OHdG level was significantly correlated with dialysate:plasma creatine ratio (r = 0.463, P < 0.05 and significantly inversely correlated with D/D0 glucose (where D is the glucose level of peritoneal effluents obtained 4 hours after the injection and D0 is the glucose level obtained immediately after the injection (r = -0.474, P < 0.05. The 8-OHdG level was also significantly correlated with MMP-2 level (r = 0.551, P < 0.05, but it was not correlated with the age of subjects, the duration of PD, or blood pressure.Conclusion: The level of 8-OHdG in drained dialysate may be a useful novel marker of peritoneal damage in PD.Keywords: oxidative stress, solute transport rate, MMP-2, peritoneal equilibration test

  7. Development of an HPLC-UV Method for the Analysis of Drugs Used for Combined Hypertension Therapy in Pharmaceutical Preparations and Human Plasma

    Directory of Open Access Journals (Sweden)

    Serife Evrim Kepekci Tekkeli

    2013-01-01

    Full Text Available A simple, rapid, and selective HPLC-UV method was developed for the determination of antihypertensive drug substances: amlodipine besilat (AML, olmesartan medoxomil (OLM, valsartan (VAL, and hydrochlorothiazide (HCT in pharmaceuticals and plasma. These substances are mostly used as combinations. The combinations are found in various forms, especially in current pharmaceuticals as threesome components: OLM, AML, and HCT (combination I and AML, VAL, and HCT (combination II. The separation was achieved by using an RP-CN column, and acetonitrile-methanol-10 mmol orthophosphoric acid pH 2.5 (7 : 13 : 80, v/v/v was used as a mobile phase; the detector wavelength was set at 235 nm. The linear ranges were found as 0.1–18.5 μg/mL, 0.4–25.6 μg/mL, 0.3–15.5 μg/mL, and 0.3–22 μg/mL for AML, OLM, VAL, and HCT, respectively. In order to check the selectivity of the method for pharmaceutical preparations, forced degradation studies were carried out. According to the validation studies, the developed method was found to be reproducible and accurate as shown by RSD ≤6.1%, 5.7%, 6.9%, and 4.6% and relative mean error (RME ≤10.6%, 5.8%, 6.5%, and 6.8% for AML, OLM, VAL, and HCT, respectively. Consequently, the method was applied to the analysis of tablets and plasma of the patients using drugs including those substances.

  8. Quantitative determination of quinolones residues in milk by HPLC-FLD

    Directory of Open Access Journals (Sweden)

    Marilena Gili

    2012-10-01

    Full Text Available Veterinary drugs have become an integral part of the livestock production and play an important role in maintenance of animal welfare. The use of veterinary medicines may be cause of the presence of drug residues in animal food products if appropriate withdrawal periods are not respected or if contaminated feeds are used. This work presents the development of an HPLC-FLD method for the quantitative de-tection of eight quinolones – norfloxacin, ciprofloxacin, danofloxacin, enrofloxacin, difloxacin, oxolinic acid, nalidixic acid, flumequine– in bovine milk. After deproteination and extraction with a metaphos-phoric acid 1% w/v / methanol / acetonitrile (60/20/20 v/v/v solution, the sample is partially evaporated and cleaned up on a reversed phase SPE cartridge.The extract is analyzed using an high performance liquid chromatograph with fluorescence detector. Mean recovery ranged between 65% - 88%. All the an-alytes can be identified and quantified in the concentration range 15 - 60 μg/Kg for danofloxacin and 25 - 150 μg/Kg for the other quinolones.

  9. Application of ICP-MS and HPLC-ICP-MS for diagnosis and therapy of a severe intoxication with hexavalent chromium and inorganic arsenic.

    Science.gov (United States)

    Heitland, Peter; Blohm, Martin; Breuer, Christian; Brinkert, Florian; Achilles, Eike Gert; Pukite, Ieva; Köster, Helmut Dietrich

    2017-05-01

    ICP-MS and HPLC-ICP-MS were applied for diagnosis and therapeutic monitoring in a severe intoxication with a liquid containing hexavalent chromium (Cr(VI)) and inorganic arsenic (iAs). In this rare case a liver transplantation of was considered as the only chance of survival. We developed and applied methods for the determination of Cr(VI) in erythrocytes and total chromium (Cr) and arsenic (As) in blood, plasma, urine and liver tissue by ICP-MS. Exposure to iAs was diagnosed by determination of iAs species and their metabolites in urine by anion exchange HPLC-ICP-MS. Three days after ingestion of the liquid the total Cr concentrations were 2180 and 1070μg/L in whole blood and plasma, respectively, and 4540μg/L Cr(VI) in erythrocytes. The arsenic concentration in blood was 206μg/L. The urinary As species concentrations were <0.5, 109, 115, 154 and 126μg/L for arsenobetaine, As(III), As(V), methylarsonate (V) and dimethylarsinate (V), respectively. Total Cr and As concentrations in the explanted liver were 11.7 and 0.9mg/kg, respectively. Further analytical results of this case study are tabulated and provide valuable data for physicians and toxicologists. Copyright © 2017. Published by Elsevier GmbH.

  10. Multi-Analyte Separation Methods for HPLC Determination of the Active Ingredients of Pesticides

    Energy Technology Data Exchange (ETDEWEB)

    Virtics, I.; Korsós, I.; Homoki, E.; Lantos, J. [Plant Protection and Soil Conservation Service of Szabolcs-Szatmár-Bereg County, Nyíregyháza (Hungary)

    2009-07-15

    The practical quality control of selected pesticides, such as carbamates, organophosphorous compounds, phthalimides, pyrethroids, with HPLC is described. Detailed descriptions are given of materials and methods used, including sample preparation and HPLC operating conditions. The relationship between pH value of the HPLC eluent and the logP{sub ow} is discussed, illustrated by chromatograms, graphics and tables. The results are also compared with those elaborated by. E. Dudar and presented above. (author)

  11. VEGFR-3 signaling is regulated by a G-protein activator, activator of G-protein signaling 8, in lymphatic endothelial cells.

    Science.gov (United States)

    Sakima, Miho; Hayashi, Hisaki; Mamun, Abdullah Al; Sato, Motohiko

    2018-07-01

    Vascular endothelial growth factor C (VEGFC) and its cognate receptor VEGFR-3 play a key role in lymphangiogenesis. We previously reported that an ischemia-inducible Gβγ signal regulator, activator of G-protein signaling 8 (AGS8), regulated the subcellular distribution of vascular endothelial growth factor receptor-2 (VEGFR-2) and influenced VEGFA-induced signaling in vascular endothelial cells. Here, we report that AGS8 regulates VEGFR-3, which is another subtype of the VEGF receptor family, and mediates VEGFC signaling in human dermal lymphatic endothelial cells (HDLECs). VEGFC stimulated the proliferation of HDLECs and tube formation by HDLECs, which were inhibited by knocking down AGS8 by small interfering RNA (siRNA). AGS8 siRNA inhibited VEGFC-mediated phosphorylation of VEGFR-3 and its downstream molecules, including ERK1/2 and AKT. Analysis of fluorescence-activated cell sorting and immunofluorescence staining demonstrated that AGS8 knockdown was associated with a reduction of VEGFR-3 at the cell surface. Endocytosis inhibitors did not rescue the decrease of cell-surface VEGFR-3, suggesting that AGS8 regulated the trafficking of VEGFR-3 to the plasma membrane. An immunoprecipitation assay indicated that VEGFR-3 formed a complex including AGS8 and Gβγ in cells. These data suggest the novel regulation of VEGFC-VEGFR-3 by AGS8 in HDLECs and a potential role for AGS8 in lymphangiogenesis. Copyright © 2018 Elsevier Inc. All rights reserved.

  12. A Simple and Validated Reverse Phase HPLC Methodfor the Determination of Rabeprazole inPharmaceutical Dosage Forms

    Directory of Open Access Journals (Sweden)

    Uma Mahesh Karra

    2010-01-01

    Full Text Available A simple and rapid reverse phase high performance liquid chromatography (RP-HPLC method was developed and validated for quantitative determination of rabeprazole in bulk drug samples and formulations. Rabeprazole was analyzed by using reverse phase LC-GC column (Inertsil ODS, 4.6 mm x 25 cm, 5 microns, with mobile phase consisting of methanol: water (78:22 v/v. The flow rate was set 1.0 mL/min and analysis was performed at wavelength 288 nm using Photo Diode Array (PDA detector at ambient temperature. The method was validated and stability studies were conducted under different conditions. The retention time for rabeprazole was around 4.12 minutes. The calibration curves were linear (r≥0.9998 over a concentration range from 20.0 to 80.0 μg/mL. Limit of detection (LOD and Limit of quantitation (LOQ were 8 ng/mL and 24 ng/mL respectively. The developed method was successfully applied to estimate the amount of rabeprazole in tablet formulations.

  13. The data on health locus of control and its relationship with quality of life in HIV-positive patients

    Directory of Open Access Journals (Sweden)

    Zahra Mostafavian

    2018-06-01

    Full Text Available Locus of control is a concept defined based on social learning theory, and focuses on individuals' beliefs regarding factors that influence their health status. Health Locus of Control (HLC and its relationship with Quality of Life (QOL in HIV positive patients in local population were studied. This was a cross-sectional study on 80 HIV-positive patients. Multidimensional Health Locus of Control (MHLC Scale and Medical Outcome Study Short-Form Health Survey (MOS-SF-36 used to measure patients' HLC and QOL, respectively. Internal, external, and chance HLC mean ± SD scores were 30.31±3.87, 24.17±5.03, and 32.01±4.49, respectively. Positive correlation was found between internal HLC scores and both physical (p <0.001, r = 0.53 and mental quality of life (p <0.001, r = 0.48. Multiple regression analysis showed that internal HLC was the only significant predictor of quality of life. HIV-positive patients who believe their health is mostly influenced by individual's actions and behaviors (internal HLC showed a higher quality of life. These findings suggest that modifying health locus of control beliefs, hypothetically could influence patients' quality of life. Keywords: HIV, Health locus of control, Quality of life, Medicine

  14. HPLC-MS/MS investigation of biochemical markers for the disclosure of erythropoietin abuse in sports

    Science.gov (United States)

    Appolonova, S. A.; Dikunets, M. A.; Rodchenkov, G. M.

    2009-04-01

    The polypeptide hormone erythropoietin (EPO), which is a forbidden doping drug, was determined by high-performance liquid chromatography combined with tandem mass spectrometry (HPLC-MS/MS). The hypothesis about the influence of EPO on the asymmetric dimethylarginine (ADMA)-dimethylargininedime-thylaminohydrolase (DDAH)-NO-synthase system was verified. Changes in this system can serve as indirect biochemical markers of the presence of the forbidden EPO drug in the organism. In the test group, the concentrations of biochemical markers varied from 10 to 40 μg/ml for ADMA and symmetrical DMA (SDMA) and from 0.5 to 10 μg/ml for arginine and citrulline. A single intravenous administration of r-HuEPO (Epocrin, 2000 ME/day) for two volunteers reliably increased ADMA, SDMA, arginine, and citrulline concentrations to 40-270 μg/ml, 40-240μg/ml, 10-60 μg/ml, and 12-140 μg/ml, respectively, with respect to the reference values. The simultaneous increase in arginine, methylarginines, and citrulline contents could be an indirect marker of EPO abuse. The method is recommended for fast screening analysis.

  15. [Analysis of phenylethanoid glycosides of Herba cistanchis by RP-HPLC].

    Science.gov (United States)

    Tu, P F; Wang, B; Deyama, T; Zhang, Z G; Lou, Z C

    1997-04-01

    The Chinese drug "Rou Cong-rong" (Herba Cistanchis) is one of the commonly used drugs in Chinese traditional medicine. It is used to reinforce the vital function of kidney, especially that of the sexual organs and induce laxation, for the treatment of impotence, premature ejaculation in men, infertility, morbid leukorrhea, profuse metrorrhagia in women, and chronic constipation in the aged. This paper deals with the qualitative and quantitative analysis of phenylethanoid glycosides of four species and one variety of Genus Cistanche and 23 lots of commercial crude drugs of Herba Cistanchis by RP-HPLC. The results were as follows: the chemical constituents of Cistanche deserticola Ma, C. salsa (C. A. Mey) G. Beck, C. salsa var. albiflora P. F. Tu et Z. C. Lou and C. tubulosa were similar while those of C. sinensis were different from the others; the contents of echinacoside and acteoside of C. salsa, which were 2.13% and 1.51%, were the highest of the genus Cistanche. An ODS column (Alltima C18, 5 microns, 250 x 4.6 mm) was employed. Linear gradient elution of acetonitrile--1.5% acetic acid was used as mobile phase, and concentration of acetontrile was from 8% to 20% (0-60 min) in the qualitative analysis, and from 11.5 to 20% (0-35 min) in the quantitative analysis. The flow rate was 1.2 ml.min-1. The detection wavelength was set at 335 nm.

  16. Simultaneous qualification and quantification of baccharane glycosides in Impatientis Semen by HPLC-ESI-MSD and HPLC-ELSD.

    Science.gov (United States)

    Li, Hui-Jun; Yu, Jun-Jie; Li, Ping

    2011-03-25

    This study presents a high performance liquid chromatography (HPLC) with electrospray ionization mass spectrometric detection (ESI-MSD) and evaporative light scattering detection (ELSD) method for the simultaneous qualification and quantification of eight major baccharane glycosides, namely hosenlosides A, B, C, F, G, K, L, and M in Impatientis Semen, a Chinese herbal medicine derived from the seeds of Impatiens balsamina L. In order to achieve optimum performance, several extraction parameters (including extraction solvent, extraction mode, extraction time) were optimized. The baccharane glycosides were separated on a Shim-pack CLC-ODS column with gradient elution of water and methanol. Temperature for the ELSD drift tube was set at 98°C and the nitrogen flow rate was 2.7l/min. The unambiguous identities of the analytes were realized by comparing retention times and mass data with those of reference compounds. The developed method was fully validated in terms of linearity, sensitivity, precision, repeatability, recovery as well as robustness, and subsequently applied to evaluate the quality of 14 batches of Impatientis Semen commercial samples from different collections. Copyright © 2010 Elsevier B.V. All rights reserved.

  17. Predominance of new G9P[8] rotaviruses closely related to Turkish strains in Nizhny Novgorod (Russia).

    Science.gov (United States)

    Sashina, T A; Morozova, O V; Epifanova, N V; Novikova, N A

    2017-08-01

    Genotype G9P[8] rotaviruses are rare in the territory of Russia. They were found in Nizhny Novgorod only in 2011-2012 for the first time, when their proportion was 25.9%. During the next two seasons, G9P[8] strains were detected in only 1.8% of cases. Their proportion substantially increased again in 2014, and they became predominant in the city by 2016. Phylogenetic analysis on the basis of gene VP7 nucleotide sequences showed that this increase was accompanied by the emergence of new strains in the population. These isolates were related to Turkish strains, but not to Russian ones detected earlier.

  18. Radio-activity detectors in HPLC

    International Nuclear Information System (INIS)

    Kremers, H.D.

    1984-01-01

    Two different approaches were adopted to put the eluate from the HPLC into contact with the scintillator, i.e. a homogeneous and a heterogeneous system. In the heterogeneous system, the eluate runs directly through a cell filled with a fine-grain solid scintillator. In the homogeneous system, a liquid scintillator is admixed to the eluate or to a proportion of the eluate before flowing through the measurement cell. Both systems are contrasted with the fractionation method according to the criterias of handling, rapidity of analysis and facility cost. On-line detection of radio-activity will be easily settled for when comparing its investment cost with those of materials consumed in fractionation. A device prepared for scintillator admixture contains an integrated scintillator pump and a mixer but is suitable for application of solid scintillator cells, too. Such a system features a wider range of practical applications than a device exclusively designed for the heterogeneous system. A further asset of the detectors in the fact that they are adapted in their performance to up-to-date HPLC facilities in terms of speed and resolution. (orig./HP) [de

  19. Identification of ionic chloroacetanilide-herbicide metabolites in surface water and groundwater by HPLC/MS using negative ion spray

    Science.gov (United States)

    Ferrer, I.; Thurman, E.M.; Barcelo, D.

    1997-01-01

    Solid-phase extraction (SPE) was combined with high-performance liquid chromatography/high-flow pneumatically assisted electrospray mass spectrometry (HPLC/ESP/MS) for the trace analysis of oxanilic and sulfonic acids of acetochlor, alachlor, and metolachlor. The isolation procedure separated the chloroacetanilide metabolites from the parent herbicides during the elution from C18 cartridges using ethyl acetate for parent compounds, followed by methanol for the anionic metabolites. The metabolites were separated chromatographically using reversed-phase HPLC and analyzed by negative-ion MS using electrospray ionization in selected ion mode. Quantitation limits were 0.01 ??g/L for both the oxanilic and sulfonic acids based on a 100-mL water sample. This combination of methods represents an important advance in environmental analysis of chloroacetanilide-herbicide metabolites in surface water and groundwater for two reasons. First, anionic chloroacetanilide metabolites are a major class of degradation products that are readily leached to groundwater in agricultural areas. Second, anionic metabolites, which are not able to be analyzed by conventional methods such as liquid extraction and gas chromatography/mass spectrometry, are effectively analyzed by SPE and high-flow pneumatically assisted electrospray mass spectrometry. This paper reports the first HPLC/MS identification of these metabolites in surface water and groundwater.

  20. Effects of the radiolysis products of sennoside A on HepG2 and PC-3 cell

    International Nuclear Information System (INIS)

    Kim, Dong Ho; Jo, Min Ho

    2016-01-01

    Radiolysis of sennoside A was carried out by gamma irradiation and the anti-cancer activities of the radiolysis product were evaluated. An aqueous solution of sennoside A was exposed to 0.5-3 kGy of gamma irradiation and the radiolysis products were analyzed by HPLC. A fraction of radiolysis product (RLF) of sennoside A was isolated and the RLF was presumed as a rhein-8-β-D-glucoside. The anticancer effect of the RLF was compared with the sennoside and rhein using a in vitro assay system of human prostate cancer cells (PC-3) and human hepatoma HepG2 cells. The cell viability of PC-3 and HepG2 cell was significantly decreased to 12.4±1.2% and 32.4±2.1%, respectively, by the treatment of 0.6 μM of RLF. The sennoside A (range from 0 to 25 μM) had no cytotoxic effect on PC-3 and HepG2 cells, while the rhein had the effect on HepG2 cells with a LD_5_0 at 80 μM

  1. Effects of the radiolysis products of sennoside A on HepG2 and PC-3 cell

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Dong Ho; Jo, Min Ho [Research Division for Biotechnology, Korea Atomic Energy Research Institute, Jeongeup (Korea, Republic of)

    2016-11-15

    Radiolysis of sennoside A was carried out by gamma irradiation and the anti-cancer activities of the radiolysis product were evaluated. An aqueous solution of sennoside A was exposed to 0.5-3 kGy of gamma irradiation and the radiolysis products were analyzed by HPLC. A fraction of radiolysis product (RLF) of sennoside A was isolated and the RLF was presumed as a rhein-8-β-D-glucoside. The anticancer effect of the RLF was compared with the sennoside and rhein using a in vitro assay system of human prostate cancer cells (PC-3) and human hepatoma HepG2 cells. The cell viability of PC-3 and HepG2 cell was significantly decreased to 12.4±1.2% and 32.4±2.1%, respectively, by the treatment of 0.6 μM of RLF. The sennoside A (range from 0 to 25 μM) had no cytotoxic effect on PC-3 and HepG2 cells, while the rhein had the effect on HepG2 cells with a LD{sub 50} at 80 μM.

  2. G8: trois Francais, auteurs presumes de violences à Genève, arretes mercredi

    CERN Multimedia

    2003-01-01

    "Trois Francais, soupconnes d'avoir participe a des violences survenues a Geneve en marge du sommet du G8 en juin dernier, ont ete arretes mercredi a Geneve, apres avoir reconnu les faits qui leur sont reproches, a annonce la police locale" (1/2 page).

  3. Multielemental speciation analysis by advanced hyphenated technique - HPLC/ICP-MS: A review.

    Science.gov (United States)

    Marcinkowska, Monika; Barałkiewicz, Danuta

    2016-12-01

    Speciation analysis has become an invaluable tool in human health risk assessment, environmental monitoring or food quality control. Another step is to develop reliable multielemental speciation methodologies, to reduce costs, waste and time needed for the analysis. Separation and detection of species of several elements in a single analytical run can be accomplished by high performance liquid chromatography hyphenated to inductively coupled plasma mass spectrometry (HPLC/ICP-MS). Our review assembles articles concerning multielemental speciation determination of: As, Se, Cr, Sb, I, Br, Pb, Hg, V, Mo, Te, Tl, Cd and W in environmental, biological, food and clinical samples analyzed with HPLC/ICP-MS. It addresses the procedures in terms of following issues: sample collection and pretreatment, selection of optimal conditions for elements species separation by HPLC and determination using ICP-MS as well as metrological approach. The presented work is the first review article concerning multielemental speciation analysis by advanced hyphenated technique HPLC/ICP-MS. Copyright © 2016 Elsevier B.V. All rights reserved.

  4. HPLC-UV Polyphenolic Profiles in the Classification of Olive Oils and Other Vegetable Oils via Principal Component Analysis

    Directory of Open Access Journals (Sweden)

    Mireia Farrés-Cebrián

    2016-12-01

    Full Text Available High performance liquid chromatography-ultraviolet (HPLC-UV was applied to the analysis and characterization of olive oils and other vegetable oils. A chromatographic separation on a Zorbax Eclipse XDB-C8 reversed-phase column was proposed under gradient elution, employing 0.1% formic acid aqueous solution and methanol as mobile phase, for the determination of 14 polyphenols and phenolic acids, allowing us to obtain compositional profiles in less than 20 min. Acceptable sensitivity (limit of detection (LOD values down to 80 µg/L in the best of cases, linearity (r2 higher than 0.986, good run-to-run and day-to-day precisions (relative standard deviation (RSD values lower than 11.5%, and method trueness (relative errors lower than 6.8% were obtained. The proposed HPLC-UV method was then applied to the analysis of 72 oil samples (47 olive oils and 27 vegetable oils including sunflower, soy, corn, and mixtures of them. Analytes were recovered using a liquid–liquid extraction method employing ethanol:water 70:30 (v/v solution and hexane as extracting and defatting solvents, respectively. HPLC-UV polyphenolic profiles using peak areas were then analysed by principal component analysis (PCA to extract information from the most significant data contributing to the characterization and classification of olive oils against other vegetable oils, as well as among Arbequina and Picual olive oil varieties. PCA results showed a noticeable difference between olive oils and the other classes. In addition, a reasonable discrimination of olive oils as a function of fruit varieties was also encountered.

  5. The use of HPLC identification and quantification of isoflavones content in samples obtained in pharmacies = O uso do HPLC na identificação e quantificação dos teores de isoflavonas em amostras obtidas de farmácias de manipulação = O uso do HPLC na identificação e quantificação dos teores de isoflavonas em amostras obtidas de farmácias de manipulação

    Directory of Open Access Journals (Sweden)

    Daniel Mantovani

    2011-01-01

    Full Text Available Nowadays, there is a great interest in the research and the production of functional foods, such as isoflavones. Which present proven action on the prevention of health problems, such as cancer and cardiovascular diseases. Considering the importance of soybeansupplements standardization, this study aimed identifying and quantifying the isoflavones in products sold at different pharmacies. Isoflavones samples were acquired in six different pharmacies specialized in the production of phytotherapic medications. The isoflavones were extracted, quantified and identified in HPLC. None of the samples, from different pharmacies, presented the isoflavones content presented on the label, i.e., 20 mg. In relation to the isoflavones profile, the highest levels found were of daidzein, with up to 66.8 } 0.09 ƒÊg, being the lowest levels the ones of genistein. It is necessary, therefore, the adoption of methods for thestandardization and characterization of the raw materials used by different pharmacies. It would assure the isoflavones content, once they are essential for the effects prescribed by the professionals in the medical area.O uso do HPLC na identificacao e quantificacao dos teores de isoflavonas em amostras obtidas de farmacias de manipulacao. Atualmente ha um grande interesse na pesquisa e producao de alimentos funcionais, como as isoflavonas, que apresentam comprovada acao na prevencao de males, como o cancer e as doencas cardiovasculares. Considerando a importancia da padronizacao dos suplementos de soja,o objetivo do presente estudo foi de identificar e quantificar as isoflavonas em produtos comercializados em diferentes farmacias de manipulacao. Amostras de isoflavonas foram adquiridas em seis diferentes farmacias especializadas em manipulacao de fitoterapicos. As isoflavonas foram extraidas, identificadas e quantificadas em CLAE. Nenhuma das amostras, das diferentes farmacias de manipulacao, apresentou os teores de isoflavonas indicado no

  6. HPLC FOR CONTROL STABILITY OF QUERCETIN INJECTABLE DOSAGE FORM

    Directory of Open Access Journals (Sweden)

    Martynov AV

    2016-12-01

    Full Text Available Introduction. Quercetin is a flavone derivatives which known like a substances with vitamin activity, high antioxidant, antimutagenic and anticarcinogenic activity and many other types of biological activity. Wide usage of quercetin prevents their polyphenolic nature structure which does not allow a high bioavailability of pure quercetin when administered orally. This is associated with a wide spectrum variety of chemical reactions for the phenolic groups: from interaction with amino acid residues in proteins to reactions with amine heterocyclic alkaloids and polysaccharides. In our days Corvitin – one from the number of quercetin based drugs with sufficiently low levels all types toxicity, allergenic and has no irritating action on intravenous administration. In the same time quercetin cannot be used in full measure because of the limited number of publications with analysis methods, especially HPLC. Determining the stability over time of concentrate quercetin solution, as well as determining the stability of the concentrate to the original autoclave sterilization conditions is a promising direction in creating new drugs. Materials and methods The objective was to research quercetin soluble formulation samples in different conditions: 1 fresh dilute concentrate (0.9% sodium chloride; 2 the original dilute concentrate, which was stored at room temperature for 14 days in light and 3 similar to the first sample dilute concentrate, which went before breeding in autoclaving at 120 0 C for 20 minutes. The objects used in the studies were industrial drug-substance quercetin (Sinkea manufactured (China, the original pharmaceutical composition as the soluble form of quercetin for injection and aerosol applications, glycerol (Sigma, Polysorbat 80 (Merk, ethanol 96 %. For the HPLC – analysis, chromatograph "Milichrom A-02" (SiChrom, Knauer (Econova, Novosibirsk, Russia was used. Results and discussion Quercetin was identified using information on its

  7. Preparation of self-supporting molecularly imprinted films via transition layer construction and RAFT polymerization, and their use in HPLC

    International Nuclear Information System (INIS)

    Ding, Peng; Tang, Shengfu; Shi, Liyi; Li, Zongzhou; Song, Na

    2013-01-01

    Molecularly imprinted films with self-supporting property (SS-MIFs) have been prepared by using the strategy of transition layer construction followed by reversible addition-fragmentation chain transfer (RAFT) polymerization. The structure, composition and selectivity of the SS-MIFs as well as the mechanism of mass transfer were characterized by scanning electron microscopy, X-ray diffraction, Fourier transform IR spectrometry, specific surface area analysis, thermogravimetric analysis, and HPLC. Surface area analysis showed the samples possessed specific surface areas as high as 80.5 m 2 .g −1 . This is almost 9 times more than that of the original porous anodic aluminum oxide substrate. Thermogravimetric analysis also showed the samples to be thermally stable up to 350 °C. The separating power was investigated by HPLC and revealed a selective separation effect for the target molecules theobromine. The separation factor is 5.37. (author)

  8. Development and validation of an HPLC method for simultaneous determination of trimethoprim and sulfamethoxazole in human plasma.

    Science.gov (United States)

    Sayar, Esin; Sahin, Selma; Cevheroglu, Semsettin; Hincal, A Atilla

    2010-09-01

    The combination of trimethoprim (TMP) and sulfamethoxazole (SMX) is used in the treatment of many common infections such as urinary, respiratory and gastrointestinal tract infections. The aim of this study was to determine TMP and SMX simultaneously in human plasma samples by high performance liquid chromatography (HPLC) using antipyrine as the internal standard. Separation of the compounds was achieved on a reverse-phase C8 column packed with 5 microm dimethyl octadecylsilyl bonded amorphous silica (4.6 mm x 250 mm) column using a mobile phase consisted of potassium hydrogen phosphate, acetonitrile, methanol and water adjusted to pH 6.2. The mobile phase was delivered at a flow rate of 1 mL min- and the effluent was monitored using Max plot technique at 25 derees C. Retention times were 5 min for TMP, 7 min for antipyrine and 9 min for SMX. Quantitation limits were 10 ng mL(-1) for TMP and 50 ng mL(-1) for SMX. Our findings indicated that the developed HPLC method was precise, accurate, specific and sensitive for simultaneous determination of TMP and SMX. Proposed HPLC method was successfully applied for the analysis of TMP and SMX in human plasma after oral administration of a co-trimoxazole tablet to human volunteers.

  9. Measurements of urinary kinins by HPLC-radioimmunoassay

    International Nuclear Information System (INIS)

    Fejes-Toth, G.; Naray-Fejes-Toth, A.; Froelich, J.C.

    1984-01-01

    In this paper the authors describe a method for the individual determination of urinary kinins. Extraction from the urine is performed on an Amberlite CG-50 column and kinins are eluted with formic acid. The samples are further purified and kinins are separated by reversed phase HPLC. Bradykinin and lysylbradykinin are quantified by a sensitive radioimmunoassay capable of detecting 0.1 fmol of either peptide. Procedural losses are monitored by measuring the recovery of [ 3 H]bradykinin and [ 3 H]lysylbradykinin. Simple methods for labeling of bradykinin and lysylbradykinin with tritium are also presented. Recoveries of [ 3 H]bradykinin and [ 3 H]lysylbradykinin from biological material ranged between 77 and 91%. The combination of HPLC with radioimmunoassay makes it possible to determine kinin concentrations of biological samples with a higher sensitivity and greater specificity than previous methods. (Auth.)

  10. WWF Climate Scorecards. Comparison of the climate performance of the G8 countries

    International Nuclear Information System (INIS)

    Hoehne, N.; Wartmann, S.; Graus, W.

    2005-07-01

    Climate change is a serious and urgent threat to global society. It adds stress to unique and already threatened ecosystems, increases the frequency and intensity of extreme weather events, such as storms and droughts, and adds stress to agriculture and food production. In addition, glaciers are melting around the world as is the Arctic, contributing to sea level rise. Climate change also increases the risk of large-scale singular events such as the melting of the West Antarctic Ice Sheet and the shutdown of the thermohaline circulation. The level at which climate change becomes 'dangerous' depends on the values attached to the threatened systems. Several countries, most prominently the EU, but also e.g. the Philippines and Micronesia, have agreed that global average temperature increase in comparison to pre-industrial levels should be kept below 2C. As a consequence, global greenhouse gas emissions will have to peak in the next decade or two and then decline to a fraction of current levels. Leaving some room for growth for developing countries, industrialized countries need to decrease their emission by the order of 80% by the year 2050. This is a major challenge, as current trends are going in the opposite direction with high emissions in developed countries and growing emissions in most developing countries. Individual countries have reacted differently to this challenge. Each country is unique in its starting position, including the economic activities that result in greenhouse gas emissions, its level of development, industrial structure, availability of natural resources and public perceptions. Since the problem was recognized internationally (1992 with the adoption of the United Nations Framework Convention on Climate Change), governments and the public have reacted differently, also depending on national circumstances. These climate scorecards provide a comparable snapshot of the current situation across the G8 countries (Canada, France, Germany, Italy

  11. WWF Climate Scorecards. Comparison of the climate performance of the G8 countries

    Energy Technology Data Exchange (ETDEWEB)

    Hoehne, N.; Wartmann, S.; Graus, W. [Ecofys GmbH, Koeln (Germany)

    2005-07-01

    Climate change is a serious and urgent threat to global society. It adds stress to unique and already threatened ecosystems, increases the frequency and intensity of extreme weather events, such as storms and droughts, and adds stress to agriculture and food production. In addition, glaciers are melting around the world as is the Arctic, contributing to sea level rise. Climate change also increases the risk of large-scale singular events such as the melting of the West Antarctic Ice Sheet and the shutdown of the thermohaline circulation. The level at which climate change becomes 'dangerous' depends on the values attached to the threatened systems. Several countries, most prominently the EU, but also e.g. the Philippines and Micronesia, have agreed that global average temperature increase in comparison to pre-industrial levels should be kept below 2C. As a consequence, global greenhouse gas emissions will have to peak in the next decade or two and then decline to a fraction of current levels. Leaving some room for growth for developing countries, industrialized countries need to decrease their emission by the order of 80% by the year 2050. This is a major challenge, as current trends are going in the opposite direction with high emissions in developed countries and growing emissions in most developing countries. Individual countries have reacted differently to this challenge. Each country is unique in its starting position, including the economic activities that result in greenhouse gas emissions, its level of development, industrial structure, availability of natural resources and public perceptions. Since the problem was recognized internationally (1992 with the adoption of the United Nations Framework Convention on Climate Change), governments and the public have reacted differently, also depending on national circumstances. These climate scorecards provide a comparable snapshot of the current situation across the G8 countries (Canada, France, Germany

  12. Recent developments in HPLC analysis of β-blockers in biological samples.

    Science.gov (United States)

    Saleem, Kishwar; Ali, Imran; Kulsum, Umma; Aboul-Enein, Hassan Y

    2013-09-01

    β-Adrenergic blockers represent a very important class of drugs that are used worldwide for treating various cardiac diseases. The present article describes the state-of-the art of analyses of β-adrenergic blockers using high-performance liquid chromatography (HPLC). Sample preparation techniques such as liquid-liquid extraction, solid-phase extraction and solid-phase microextraction have been discussed, which are essential prior to HPLC analysis. Additionally, applications of liquid chromatography coupled with tandem mass spectrometry are included. HPLC methods have been reported to include 0.6-26 min as the run times and 0.01 ng/mL to 25 µg/mL as detection limits. The most commonly used columns were C18 with various buffers as the mobile phases, along with various organic modifiers. The optimization of HPLC conditions has been discussed. It has been observed that the reported methods are quite satisfactory for the analyses of β-adrenergic blockers in biological samples. Future perspectives in the hyphenation of solid-phase microextraction-nano-liquid chromatography-tandem mass spectrometry have also been highlighted to achieve detections at nanogram and picogram levels. The present article is very useful for academicians, scientists, drug and pharmaceutical personnel and government regulatory authorities.

  13. Pharmacognostic evaluation, and development and validation of a HPLC-DAD technique for gallocatechin and epigallocatechin in rhizomes from Limonium brasiliense

    Directory of Open Access Journals (Sweden)

    Andressa Blainski

    Full Text Available ABSTRACT Limonium brasiliense (Boiss. Kuntze, Plumbaginaceae, is a plant from the southern coast of Brazilian that is used for the treatment of premenstrual syndrome, menstrual disorders and genito-urinary infections. The aim of the present study was to determine the quality control parameters for rhizomes collected during different periods by pharmacopoeial and non-pharmacopoeial methods, and to develop and validate a HPLC-DAD method for quantitative control of marker substances. The measured parameters were: granulometric analysis (d50 = 0.21–0.48 mm, loss on drying (11.1–12.4%, total ash (4.9–5.7%, dry residue by extraction with acetone:water (7:3, v/v (30.6–39.5%, total polyphenol content (8.5–15.8%, and chromatographic fingerprint by HPLC and TLC. Besides, the acetone:water (7:3, v/v extraction solvent in combination with a turbo-extractor, yielded the crude extract with a significant increase in tannins (F4,20 = 37.0, p < 0.001. The antioxidant potential of the crude acetone:water (7:3, v/v extract, as well as the ethyl acetate and water fractions obtained after the partition process was evaluated by DPPH and the results were, respectively: IC50 6.87, 5.91, and 6.92 µg/ml. The validation parameters for the HPLC-DAD method showed adequate specificity, precision and accuracy. The gallo- and epigallocatechin contents were, respectively, 0.8–2.7% and 1.2–2.2%. These data contribute to analysis of the pharmacognostic quality control of the commonly used part from this species.

  14. RP-HPLC Method for the Estimation of Nebivolol in Tablet Dosage Form

    Directory of Open Access Journals (Sweden)

    M. K. Sahoo

    2009-01-01

    Full Text Available A reverse phase HPLC method is described for the determination of nebivolol in tablet dosage form. Chromatography was carried on a Hypersil ODS C18 column using a mixture of methanol and water (80:20 v/v as the mobile phase at a flow rate of 1.0 mL/min with detection at 282 nm. Chlorzoxazone was used as the internal standard. The retention times were 3.175 min and 4.158 min for nebivolol and chlorzoxazone respectively. The detector response was linear in the concentration of 1-400 μg/mL. The limit of detection and limit of quantification was 0.0779 and 0.2361 μg/mL respectively. The percentage assay of nebivolol was 99.974%. The method was validated by determining its sensitivity, accuracy and precision. The proposed method is simple, fast, accurate and precise and hence can be applied for routine quality control of nebivolol in bulk and tablet dosage form.

  15. Optimization of supercritical fluid extraction and HPLC identification of wedelolactone from Wedelia calendulacea by orthogonal array design

    Directory of Open Access Journals (Sweden)

    Ajit A. Patil

    2014-11-01

    Full Text Available The purpose of this work is to provide a complete study of the influence of operational parameters of the supercritical carbon dioxide assisted extraction (SC CO2E on yield of wedelolactone from Wedelia calendulacea Less., and to find an optimal combination of factors that maximize the wedelolactone yield. In order to determine the optimal combination of the four factors viz. operating pressure, temperature, modifier concentration and extraction time, a Taguchi experimental design approach was used: four variables (three levels in L9 orthogonal array. Wedelolactone content was determined using validated HPLC methodology. Optimum extraction conditions were found to be as follows: extraction pressure, 25 MPa; temperature, 40 °C; modifier concentration, 10% and extraction time, 90 min. Optimum extraction conditions demonstrated wedelolactone yield of 8.01 ± 0.34 mg/100 g W. calendulacea Less. Pressure, temperature and time showed significant (p < 0.05 effect on the wedelolactone yield. The supercritical carbon dioxide extraction showed higher selectivity than the conventional Soxhlet assisted extraction method.

  16. Integration of HPLC-based fingerprint and quantitative analyses for differentiating botanical species and geographical growing origins of Rhizoma coptidis.

    Science.gov (United States)

    Lv, Xiumei; Li, Yan; Tang, Ce; Zhang, Yi; Zhang, Jing; Fan, Gang

    2016-12-01

    Rhizoma coptidis is a broadly used traditional Chinese medicine (TCM). The investigation of the influence of species and geographical origins on the phytochemicals of R. coptidis is crucial for its reasonable application and quality control. Development of an effective method to systematically study the phytochemical variations of the rhizomes of three Coptis species (Ranunculaceae) (Coptis chinensis Franch, Coptis deltoidea C.Y. Cheng et Hsiao and Coptis teeta Wall.) and a species (i.e., C. chinensis) obtained from both Daodi and non-Daodi production regions. The three species had significant differences in their phytochemicals. The rhizome of C. chinensis contained more epiberberine (13.52 ± 2.65 mg/g), palmatine (18.20 ± 2.89 mg/g), coptisine (23.32 ± 4.27 mg/g) and columbamine (4.89 ± 1.16 mg/g), whereas the rhizomes of C. deltoidea and C. teeta showed the highest level of jatrorrhizine (8.52 ± 1.36 mg/g) and berberine (81.06 ± 4.83 mg/g), respectively. Moreover, the rhizome of C. chinensis from three Daodi production regions (Shizhu, Lichuan and Emeishan) contained more alkaloids than those from three non-Daodi production regions (Mianyang, Shifang and Zhenping). It is necessary to use the three R. coptidis species differentially in TCM clinical practice. Daodi C. chinensis medicinal materials have better quality than most non-Daodi ones, and so they should be preferred for TCM prescription. The combination of HPLC-based fingerprint analysis and quantification of multi-ingredients with statistical analysis provided an effective approach for species discrimination and quality evaluation of R. coptidis.

  17. Determination of glyphosate and aminomethylphosphonic acid for assessing the quality tap water using SPE and HPLC

    Directory of Open Access Journals (Sweden)

    Eduardo Luiz Delmonico

    2014-02-01

    Full Text Available The use of pesticides in agriculture is one of the current problems that may result in contamination of both ground and surface water and groundwater. Considering the environmental importance and the increasing use of herbicides in Maringá region, in the present work methods for extraction and determination of glyphosate (GLYP and aminomethylphosphonic acid (AMPA using solid phase extraction (SPE and high performance liquid chromatography (HPLC were developed. For SPE, anion exchange resin was used and elution was done with hydrochloric acid 50.0 mmol L-1, achieving recovery rates of 82.5-116.2% and 67.1-104.0% for AMPA and GLYP, respectively. For HPLC determination the analytes were derivatized and injected in the HPLC with a C18 column and using mobile phase consisting of phosphate buffer 0.20 mol L-1 at pH 3.0 and acetonitrile (85:15; the monitoring was done at 240 nm. The analysis was performed in 8 min with the same limit of detection and limit of quantification for AMPA and GLYP of 0.09 and 0.20 mg L-1, respectively. The methods were applied to analysis of public water supply samples and concentrations from 2.1 up to 2.9 µg L-1 for AMPA and from 2.3 up to 3.3 µg L-1 for glyphosate were found.

  18. Quantification of urea in serum by isotope dilution HPLC/MS

    International Nuclear Information System (INIS)

    Lee, Hwa Shim; Park, Sang Ryoul

    2005-01-01

    Urea in blood has been measured as an effective marker for diagnosis of renal function. Urea which is the end-product of nitrogen containing metabolites such as proteins is filtered through glomeruli of kidneys and then excreted as urine. If the renal function is deteriorated, the urea concentration in blood will be increased, from which the healthiness of renal function is judged. In order to improve the confidence of diagnosis results, the results must keep traceability chain to certified reference materials, which was certified by primary reference method. In this study, we proposed Isotope Dilution-Liquid Chromatography/Mass Spectrometry (ID-LC/MS) as a candidate primary method, in which 15 N 2 -urea is used as an internal reference material. The developed method is highly accurate in principle and is convenient as it does not require cumbersome derivatization 0.1 mmol/L ammonium chloride was selected as a mobile phase for HPLC because it provide low interference in MS analysis of relatively low molecular weighted urea. HPLC and MS were connected with an ElectroSpry Ionization(ESI) interface of positive mode, which provided high sensitivity and reproducibility. The developed method was validated with internationally recognized reference materials, and we have obtained satisfactory results in an international ring trial. The expanded uncertainty calculated according to ISO guide was 1.8% at 95% confidence interval. The developed method is being used as a primary reference measurement method such as for certification of serum Certified Reference Materials (CRMs)

  19. The Second SeaWiFS HPLC Analysis Round-Robin Experiment (SeaHARRE-2)

    Science.gov (United States)

    2005-01-01

    Eight international laboratories specializing in the determination of marine pigment concentrations using high performance liquid chromatography (HPLC) were intercompared using in situ samples and a variety of laboratory standards. The field samples were collected primarily from eutrophic waters, although mesotrophic waters were also sampled to create a dynamic range in chlorophyll concentration spanning approximately two orders of magnitude (0.3 25.8 mg m-3). The intercomparisons were used to establish the following: a) the uncertainties in quantitating individual pigments and higher-order variables (sums, ratios, and indices); b) an evaluation of spectrophotometric versus HPLC uncertainties in the determination of total chlorophyll a; and c) the reduction in uncertainties as a result of applying quality assurance (QA) procedures associated with extraction, separation, injection, degradation, detection, calibration, and reporting (particularly limits of detection and quantitation). In addition, the remote sensing requirements for the in situ determination of total chlorophyll a were investigated to determine whether or not the average uncertainty for this measurement is being satisfied. The culmination of the activity was a validation of the round-robin methodology plus the development of the requirements for validating an individual HPLC method. The validation process includes the measurements required to initially demonstrate a pigment is validated, and the measurements that must be made during sample analysis to confirm a method remains validated. The so-called performance-based metrics developed here describe a set of thresholds for a variety of easily-measured parameters with a corresponding set of performance categories. The aggregate set of performance parameters and categories establish a) the overall performance capability of the method, and b) whether or not the capability is consistent with the required accuracy objectives.

  20. Detection of Biogenic Amines in Xuanwei Ham by HPLC%宣威火腿中生物胺的HPLC测定

    Institute of Scientific and Technical Information of China (English)

    廖国周; 王桂瑛; 曹锦轩; 程志斌

    2011-01-01

    Biogenic amines content was investigated in Xuanwei ham.Samples were extracted with 0.4 mol/L HClO4,and then derived with dansyl chloride.Separation was achieved using ZORBAX XDB-C18 column and identification,and a quantitative analysis of biogenic amines fraction was carried out using a HPLC system with DAD.Results showed that the linear ranges were 0.5~20 μg/mL,the limit of detection was 0.05~0.1 μg/mL,the recoveries were 81.58%~95.58% and the relative standard deviation were 2.48%~5.85% for eight biogenic amines.Six biogenic amines were detected in Xuanwei ham,the content of β-phenylethylamine,putrescine,cadaverine,tyramine,spermidine and spermine were 0.56 mg/100g,1.45 mg/100g,0.37 mg/100g,3.62 mg/100g,1.26 mg/100g and 4.28 mg/100g,respectively.%以宣威火腿为对象分析其中8种生物胺含量,样品通过0.4 mol/L高氯酸提取后以丹磺酰氯柱前衍生,经ZORBAX XDB-C18柱分离以配备二极管阵列检测器的HPLC对生物胺进行测定。结果表明,该方法中8种生物胺的线性范围为0.5~20μg/mL,检测限为0.05~0.1μg/mL,回收率为81.58%~95.58%,相对标准偏差为2.48%~5.85%,该方法线性范围广,灵敏度和准确度高,可满足定量分析的要求。在宣威火腿中检测出6种生物胺,其中苯乙胺0.56 mg/100g,腐胺1.45 mg/100g,尸胺0.37 mg/100g,酪胺3.62 mg/100g,亚精胺1.26 mg/100g,精胺4.28 mg/100g。

  1. Stability-Indicating RP-HPLC Methods for the Determination of Fluorometholone in Its Mixtures with Sodium Cromoglycate and Tetrahydrozoline Hydrochloride.

    Science.gov (United States)

    El-Bagary, Ramzia I; Fouad, Marwa A; El-Shal, Manal A; Tolba, Enas H

    2016-07-01

    Two stability-indicating reversed-phase liquid chromatographic methods were developed and validated for the determination of fluorometholone (FLU) in its mixtures with sodium cromoglycate (SCG) and tetrahydrozoline hydrochloride (THZ). The first HPLC method (Method 1) was based on isocratic elution of FLU and SCG along with their alkaline degradation products on a reversed phase C18 column (250 × 4.6 mm id)-ACE Generix 5, using a mobile phase consisting of methanol-water (70 : 30, v/v), pH adjusted to 2.5 using orthophosphoric acid at a flow rate of 1.2 mL min(-1) Quantitation was achieved with UV detection at 240 nm. The second HPLC method (Method 2) was based on isocratic elution of FLU, its alkaline degradation product and THZ on a reversed phase C8 column (250 × 4.6 mm)-ACE Generix 5, using a mobile phase consisting of acetonitrile-50 mM potassium dihydrogen orthophosphate (40 : 60, v/v) at a flow rate of 2 mL min(-1) Quantitation was achieved by applying dual-wavelength detection, where FLU and its alkaline degradation product were detected at 240 nm and THZ was detected at 215 nm at ambient temperatures. Linearity, accuracy and precision were found to be acceptable over the concentration range of 5-50 and 10-500 μg mL(-1) for FLU and SCG (Method 1) and over the concentration range of 5-80 and 5-60 μg mL(-1) for FLU and THZ (Method 2), respectively. Besides, the FLU alkaline degradation product was verified using IR, NMR and LC-MS spectroscopy. The two proposed methods could be successfully applied for the routine analysis of the studied drugs either in their pure bulk powders or in their pharmaceutical preparations without any preliminary separation step. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  2. Full genome analysis of rotavirus G9P[8] strains identified in acute gastroenteritis cases reveals genetic diversity: Pune, western India.

    Science.gov (United States)

    Tatte, Vaishali S; Chaphekar, Deepa; Gopalkrishna, Varanasi

    2017-08-01

    Group A rotaviruses (RVA) are the major enteric etiological agents of severe acute gastroenteritis among children globally. As G9 RVA now represents as one of the major human RVA genotypes, studies on full genome of this particular genotype are being carried out worldwide. So far, no such studies on G9P[8] RVAs have been reported from Pune, western part of India. Keeping in view of this, the study was undertaken to understand the degree of genetic diversity of the commonly circulating G9P[8] RVA strains. Rotavirus surveillance studies carried out earlier during the years 2009-2011 showed increase in the prevalence of G9P[8] RVAs. Representative G9P[8] RVA strains from the years 2009, 2010, and 2011 were selected for the study. In general, all the G9 RVA strains showed clustering in the globally circulating sublineage of the VP7 gene and showed nucleotide/amino acid identities of 96.8-99.7%/96.9-99.8% with global G9 RV strains. Full genome analysis, of all three RVAs in this study indicated Wa-like genotype constellation G9-P[8]-I1-R1-C1-M1-A1-N1-T1-E1-H1. Within the strains nucleotide/amino acid divergence of 0.1-3.4%/0.0-4.1% was noted in all the RVA structural and non-structural genes. In conclusion, the present study highlights intra-genotypic variations throughout the RVA genome. The study further emphasizes the need for surveillance and analysis of the whole genomic constellation of the commonly circulating RVA strains of other regions in the country for understanding to a greater degree of the impact of rotavirus vaccination recently introduced in India. © 2017 Wiley Periodicals, Inc.

  3. A HPLC method for the quantification of butyramide and acetamide at ppb levels in hydrogeothermal waters

    Energy Technology Data Exchange (ETDEWEB)

    Gracy Elias; Earl D. Mattson; Jessica E. Little

    2012-01-01

    A quantitative analytical method to determine butyramide and acetamide concentrations at the low ppb levels in geothermal waters has been developed. The analytes are concentrated in a preparation step by evaporation and analyzed using HPLC-UV. Chromatographic separation is achieved isocratically with a RP C-18 column using a 30 mM phosphate buffer solution with 5 mM heptane sulfonic acid and methanol (98:2 ratio) as the mobile phase. Absorbance is measured at 200 nm. The limit of detection (LOD) for BA and AA were 2.0 {mu}g L{sup -1} and 2.5 {mu}g L{sup -1}, respectively. The limit of quantification (LOQ) for BA and AA were 5.7 {mu}g L{sup -1} and 7.7 {mu}g L{sup -1}, respectively, at the detection wavelength of 200 nm. Attaining these levels of quantification better allows these amides to be used as thermally reactive tracers in low-temperature hydrogeothermal systems.

  4. Pathogenic substitution of IVS15 + 5G > A in SLC26A4 in patients of Okinawa Islands with enlarged vestibular aqueduct syndrome or Pendred syndrome.

    Science.gov (United States)

    Ganaha, Akira; Kaname, Tadashi; Yanagi, Kumiko; Naritomi, Kenji; Tono, Tetsuya; Usami, Shin-ichi; Suzuki, Mikio

    2013-05-24

    Pendred syndrome (PS) and nonsyndromic hearing loss associated with enlarged vestibular aqueduct (EVA) are caused by SLC26A4 mutations. The Okinawa Islands are the southwestern-most islands of the Japanese archipelago. And ancestral differences have been reported between people from Okinawa Island and those from the main islands of Japan. To confirm the ethnic variation of the spectrum of SLC26A4 mutations, we investigated the frequencies of SLC26A4 mutations and clinical manifestations of patients with EVA or PS living in the Okinawa Islands. We examined 22 patients with EVA or PS from 21 unrelated families in Okinawa Islands. The patient's clinical history, findings of physical and otoscopic examinations, hearing test, and computed tomography (CT) scan of the temporal bones were recorded. To detect mutations, all 21 exons and the exon-intron junctions of SLC26A4 were sequenced for all subjects. Quantitative reverse-transcription polymerase chain reaction (qRT-PCR) for SLC26A4 and calculations using the comparative CT (2(-ΔΔCT)) method were used to determine the pathogenicity associated with gene substitutions. SLC26A4 mutations were identified in 21 of the 22 patients. We found a compound heterozygous mutation for IVS15 + 5G > A/H723R in nine patients (41%), a homozygous substitution of IVS15 + 5G > A in six patients (27%), and homozygous mutation for H723R in five patients (23%). The most prevalent types of SLC26A4 alleles were IVS15 + 5G > A and H723R, which both accounted for 15/22 (68%) of the patients. There were no significant correlations between the types of SLC26A4 mutation and clinical manifestations. Based on qRT-PCR results, expression of SLC26A4 was not identified in patients with the homozygous substitution of IVS15 + 5G > A. The substitution of IVS15 + 5G > A in SLC26A4 was the most common mutation in uniquely found in patients with PS and EVA in Okinawa Islands. This suggested that the spectrum of SLC26A4 mutation differed

  5. Determination of residues of imazapic and imazaphic in rice (Oryza sativa) by HPLC

    International Nuclear Information System (INIS)

    Silva Trejos, Paulina

    2005-01-01

    A requirement to introduce a pesticide in the harvest of any product for the human consume is imperative to determine that it will not leave residues that can injure the human healthy. In this research the residues of imazapic and imazapyr, both systemic herbicides of the imidazolinone family, were determined in rice (Oryza sativa) by extraction of the samples with the extraction solvent prepared by mixing 40 mL of HC1 1 N, 2400 mL of methanol pesticide grade and 1560 mL of bidistilled water. An aliquot of the extract was concentrated approximately to 10 mL in a rotary evaporator; water was added to the concentrated extract and dissolution to 10 % m/v of lead acetate and it was regulated the pH to 6,2 with dissolution of NaOH 1 N. This dissolution was centrifuged and from the floating liquid and aliquot was measured to regulate the pH to 2,1 with dissolution of HC1 1 N. After it was extracted with dichlormethan and the join extracts were carried to dryness in the rotary evaporator. The residues were dissolved in ultrapure water of pH 2,5 and they were injected in HPLC chromatograph with a C 8 column. The validation of the analytical method obtained were: 5,1 x 10 -2 to 5,1 x 10 -3 μg/mL for linearity; (1,5 x 10 -3 , 5,0 x 10 -3 , 7,8 x 10 -3 , 2,6 x 10 -2 ) μg/mL for imazapyr and imazapic for the detection and quantification limits equivalent to 5,0 x 10 -2 mg/kg in rice; the percent of recovery were 80 % and 125 %, for imazapyr and imazapic and finally, the precision for the retention time, the area and for concentration were: 0,003 % standard deviations, 18 500 and 0,008, respectively. (author) [es

  6. Activation of the Silent Secondary Metabolite Production by Introducing Neomycin-Resistance in a Marine-Derived Penicillium purpurogenum G59

    Directory of Open Access Journals (Sweden)

    Chang-Jing Wu

    2015-04-01

    Full Text Available Introduction of neomycin-resistance into a marine-derived, wild-type Penicillium purpurogenum G59 resulted in activation of silent biosynthetic pathways for the secondary metabolite production. Upon treatment of G59 spores with neomycin and dimethyl sulfoxide (DMSO, a total of 56 mutants were obtained by single colony isolation. The acquired resistance of mutants to neomycin was testified by the resistance test. In contrast to the G59 strain, the EtOAc extracts of 28 mutants inhibited the human cancer K562 cells, indicating that the 28 mutants have acquired the capability to produce bioactive metabolites. HPLC-photodiode array detector (PDAD-UV and HPLC-electron spray ionization (ESI-MS analyses further indicated that diverse secondary metabolites have been newly produced in the bioactive mutant extracts. Followed isolation and characterization demonstrated that five bioactive secondary metabolites, curvularin (1, citrinin (2, penicitrinone A (3, erythro-23-O-methylneocyclocitrinol (4 and 22E-7α-methoxy-5α, 6α-epoxyergosta-8(14,22-dien-3β-ol (5, were newly produced by a mutant, 4-30, compared to the G59 strain. All 1–5 were also not yet found in the secondary metabolites of other wild type P. purpurogenum strains. Compounds 1–5 inhibited human cancer K562, HL-60, HeLa and BGC-823 cells to varying extents. Both present bioassays and chemical investigations demonstrated that the introduction of neomycin-resistance into the marine-derived fungal G59 strain could activate silent secondary metabolite production. The present work not only extended the previous DMSO-mediated method for introducing drug-resistance in fungi both in DMSO concentrations and antibiotics, but also additionally exemplified effectiveness of this method for activating silent fungal secondary metabolites. This method could be applied to other fungal isolates to elicit their metabolic potentials to investigate secondary metabolites from silent biosynthetic pathways.

  7. Novel assay of antibacterial components in manuka honey using lucigenin-chemiluminescence-HPLC

    International Nuclear Information System (INIS)

    Karasawa, Koji; Haraya, Shiomi; Okubo, Sachie; Arakawa, Hidetoshi

    2017-01-01

    Five components (hydrogen peroxide, methylglyoxal, dihydroxyacetone, fructose and glucose) of New Zealand manuka honey (Leptospermum scoparium) were analyzed using lucigenin chemiluminescence high-performance liquid chromatography (lucigenin-CL-HPLC). We focused on active oxygen species produced from the components in order to easily detect these five components contained in manuka honey. H_2O_2 and O_2"− generated from these components were identified by lucigenin-CL and electron spin resonance (ESR), and the bactericidal effect of ROS was confirmed using E. coli. The previously reported assays for Manuka honey components have low specificities and require complicated preprocessing methods. As our results, the detection and identification of these components were possible within 30 min in lucigenin-CL-HPLC system, without any special treatment. It is considered that lucigenin-CL-HPLC is useful for the quality control and the analysis of various honey. - Highlights: • Antibacterial components in manuka honey by HPLC with lucigenin-CL. • Five antibacterial compounds measured via generation of reactive oxygen species. • Simple, sensitive and useful for quality control and analysis of antibacterial honey.

  8. HPTLC and reverse phase HPLC methods for the simultaneous quantification and in vitro screening of antioxidant potential of isolated sesquiterpenoids from the rhizomes of Cyperus rotundus.

    Science.gov (United States)

    Priya Rani, M; Padmakumari, K P

    2012-09-01

    Three sesquiterpenoids solavetivone, aristolone and nootkatone were isolated from the acetone extract of Cyperus rotundus by silica gel column chromatography and identified by spectral studies. Solavetivone has been isolated for the first time from the species. Simple, sensitive and selective HPTLC and HPLC methods with ultraviolet detection (245 nm) were developed and validated for the simultaneous quantification. HPTLC method was validated in terms of their linearity, LOD, LOQ, precision, accuracy and compared with RP-HPLC-UV method. Among the three sesquiterpenoids isolated, nootkatone possessed the highest radical scavenging potential (IC(50) 4.81 μg/ml) followed by aristolone (IC(50) 5.28 μg/ml) and solavetivone (IC(50) 6.82 μg/ml) by DPPH radical scavenging assay. Total antioxidant activity against phosphomolybdenum reagent was also studied. The methods described in this paper were able to identify and quantify sesquiterpenoids from the complex mixtures of phytochemicals and could be extended to the marker based standardization of polyherbal formulations containing C. rotundus. Copyright © 2012 Elsevier B.V. All rights reserved.

  9. Simultaneous determination of glucose, fructose, sucrose and sorbitol in the leaf and fruit peel of different apple cultivars by the HPLC-RI optimized method.

    Science.gov (United States)

    Filip, Miuţa; Vlassa, Mihaela; Coman, Virginia; Halmagyi, Adela

    2016-05-15

    A high performance liquid chromatography method with refractive index detection (HPLC-RI), for simultaneous determination of glucose, fructose, sucrose and sorbitol in leaf and/or apple peel samples from nine apple (Malus domestica Borkh.) cultivars and rootstocks, originating from a germplasm collection, has been developed and validated. Box-Behnken design of response surface methodology was applied for the method optimization. The Carbosep Coregel 87H3 column was used under the optimum conditions predicted: mobile phase of H2SO4 0.005 mol L(-1) solution, flow rate of 0.3 mL min(-1) and column temperature of 35°C. The method was validated for linearity (R(2)>0.99), limits of detection (2.67-4.83 μg mL(-1)) and quantification (8.9-16.1 μg mL(-1)), precision (%RSD<5.05) and recovery (93.94-103.06%) and satisfactory results obtained. The sugars content varied across micropropagated plants in vitro, plants regenerated after cryostorage, growing trees in vivo, and fruit peel. Copyright © 2015 Elsevier Ltd. All rights reserved.

  10. High performance liquid chromatography (HPLC fingerprints and primary structure identification of corn peptides by HPLC-diode array detection and HPLC-electrospray ionization tandem mass spectrometry

    Directory of Open Access Journals (Sweden)

    Chi Wang

    2016-01-01

    Full Text Available Corn peptides (CPs are reported to have many biological functions, such as facilitating alcohol metabolism, antioxidation, antitumor, antihypertension, and hepatoprotection. To develop a method for quality control, the high-performance liquid chromatography (HPLC system was applied. Twenty-eight common peaks were found in all the CPs of corn samples from Enshi, China, based on which, a fingerprinting chromatogram was established for use in quality control in future research. Subsequently, the major chemical constituents of these common peaks were identified respectively using the HPLC-diode-array detection electrospray ionization tandem mass spectrometry (DAD-ESI-MS/MS system, and 48 peptide fractions were determined ultimately. This was the first time for the majority of these peptides to be reported, and many of them contained amino acids of glutamine (Q, L and A, which might play an important role in the exhibition of the bioactivities of CPs. Many peptides had a similar primary structure to the peptides which had been proven to be bioactive such as facilitating alcohol metabolism, scavenging free radicals, and inhibiting lipid peroxidation. This systematical analysis of the primary structure of CPs facilitated subsequent studies on the relationship between the structures and functions, and could accelerate holistic research on CPs.

  11. Identification and determination of the major constituents in traditional Chinese medicine Longdan Xiegan Pill by HPLC-DAD-ESI-MS

    Directory of Open Access Journals (Sweden)

    Hui Liu

    2011-02-01

    Full Text Available A novel and sensitive HPLC-UV method has been developed for the simultaneous determination of twelve major compounds in Longdan Xiegan Pill. The chemical profile of the twelve compounds, including geniposidic acid (1, geniposide(2, gentiopicroside(3, liquiritin(4, crocin(5, baicalin(6, wogonoside(7, baicalein(8, glycyrrhizic acid (9, wogonin (10, oroxylin A (11 and aristolochic acid A (12, was acquired using high-performance liquid chromatography-diode array detector coupled with an electrospray tandem mass spectrometer (HPLC-DAD-ESI-MS. The analysis was performed on a Dikma Platisil ODS C18 column (250 mm × 4. 6 mm, 5 μm with a gradient solvent system of acetonitrile-0. 1% aqueous formic acid. The validation was carried out and the linearities (r > 0. 9996, repeatability (RSD<1. 8%, intra- and inter-day precision (RSD< 1. 3%, and recoveries (ranging from 96. 6% to 103. 4% were acceptable. The limits of detection (LOD of these compounds ranged from 0.29 to 4. 17 ng. Aristolochic acid A, which is the toxic ingredient, was not detected in all the batches of Longdan Xiegan Pill. Furthermore, hierarchical cluster analysis was used to evaluate the variation of the herbal prescription. The proposed method is simple, effective and suitable for the quality control of this traditional Chinese medicine (TCM. Keywords: Longdan Xiegan Pill, high-performance liquid chromatography-diode array detector coupled with an electrospray tandem mass spectrometer (HPLC-DAD-ESI-MS, qualitative evaluation, aristolochic acid A, hierarchical cluster analysis

  12. A Simple, Fast, Low Cost, HPLC/UV Validated Method for Determination of Flutamide: Application to Protein Binding Studies.

    Science.gov (United States)

    Esmaeilzadeh, Sara; Valizadeh, Hadi; Zakeri-Milani, Parvin

    2016-06-01

    The main goal of this study was development of a reverse phase high performance liquid chromatography (RP-HPLC) method for flutamide quantitation which is applicable to protein binding studies. Ultrafilteration method was used for protein binding study of flutamide. For sample analysis, flutamide was extracted by a simple and low cost extraction method using diethyl ether and then was determined by HPLC/UV. Acetanilide was used as an internal standard. The chromatographic system consisted of a reversed-phase C8 column with C8 pre-column, and the mobile phase of a mixture of 29% (v/v) methanol, 38% (v/v) acetonitrile and 33% (v/v) potassium dihydrogen phosphate buffer (50 mM) with pH adjusted to 3.2. Acetanilide and flutamide were eluted at 1.8 and 2.9 min, respectively. The linearity of method was confirmed in the range of 62.5-16000 ng/ml (r(2) > 0.99). The limit of quantification was shown to be 62.5 ng/ml. Precision and accuracy ranges found to be (0.2-1.4%, 90-105%) and (0.2-5.3 %, 86.7-98.5 %) respectively. Acetanilide and flutamide capacity factor values of 1.35 and 2.87, tailing factor values of 1.24 and 1.07 and resolution values of 1.8 and 3.22 were obtained in accordance with ICH guidelines. Based on the obtained results a rapid, precise, accurate, sensitive and cost-effective analysis procedure was proposed for quantitative determination of flutamide.

  13. A validated bioanalytical HPLC method for pharmacokinetic evaluation of 2-deoxyglucose in human plasma.

    Science.gov (United States)

    Gounder, Murugesan K; Lin, Hongxia; Stein, Mark; Goodin, Susan; Bertino, Joseph R; Kong, Ah-Ng Tony; DiPaola, Robert S

    2012-05-01

    2-Deoxyglucose (2-DG), an analog of glucose, is widely used to interfere with glycolysis in tumor cells and studied as a therapeutic approach in clinical trials. To evaluate the pharmacokinetics of 2-DG, we describe the development and validation of a sensitive HPLC fluorescent method for the quantitation of 2-DG in plasma. Plasma samples were deproteinized with methanol and the supernatant was dried at 45°C. The residues were dissolved in methanolic sodium acetate-boric acid solution. 2-DG and other monosaccharides were derivatized to 2-aminobenzoic acid derivatives in a single step in the presence of sodium cyanoborohydride at 80°C for 45 min. The analytes were separated on a YMC ODS C₁₈ reversed-phase column using gradient elution. The excitation and emission wavelengths were set at 360 and 425 nm. The 2-DG calibration curves were linear over the range of 0.63-300 µg/mL with a limit of detection of 0.5 µg/mL. The assay provided satisfactory intra-day and inter-day precision with RSD less than 9.8%, and the accuracy ranged from 86.8 to 110.0%. The HPLC method is reproducible and suitable for the quantitation of 2-DG in plasma. The method was successfully applied to characterize the pharmacokinetics profile of 2-DG in patients with advanced solid tumors. Copyright © 2011 John Wiley & Sons, Ltd.

  14. A hybrid FIA/HPLC system incorporating monolithic column chromatography

    International Nuclear Information System (INIS)

    Adcock, Jacqui L.; Francis, Paul S.; Agg, Kent M.; Marshall, Graham D.; Barnett, Neil W.

    2007-01-01

    We have combined the generation of solvent gradients using milliGAT pumps, chromatographic separations with monolithic columns and chemiluminescence detection in an instrument manifold that approaches the automation and separation efficiency of HPLC, whilst maintaining the positive attributes of flow injection analysis (FIA), such as manifold versatility, speed of analysis and portability. As preliminary demonstrations of this hybrid FIA/HPLC system, we have determined six opiate alkaloids (morphine, pseudomorphine, codeine, oripavine, ethylmorphine and thebaine) and four biogenic amines (vanilmandelic acid, serotonin, 5-hydroxyindole-3-acetic acid and homovanillic acid) in human urine, using tris(2,2'-bipyridyl)ruthenium(III) and acidic potassium permanganate chemiluminescence detection

  15. Determination of emamectin residues in the tissues of Atlantic salmon (Salmo salar L.) using HPLC with fluorescence detection.

    Science.gov (United States)

    Kim-Kang, H; Crouch, L S; Bova, A; Robinson, R A; Wu, J

    2001-11-01

    An accurate, reliable, and reproducible assay for the determination of residual concentrations of emamectin B(1a) in muscle, skin, and intact muscle/skin in natural proportions from Atlantic salmon treated with SCH 58854 (emamectin benzoate) is described. The determinative method was developed and validated using fortified control tissues at five levels over a range of 50-800 ng/g as well as tissues containing incurred levels in the same range. Incurred tissues were obtained from a metabolism study of [(3)H]emamectin benzoate in Atlantic salmon. The assay employs processing of a tissue ethyl acetate extract on a propylsulfonic acid solid phase extraction cartridge, followed by derivatization with trifluoroacetic anhydride in the presence of N-methylimidazole. Following separation using reversed phase HPLC, the amount of derivatized emamectin B(1a) is determined by fluorescence detection. The theoretical limits of detection were determined from the analysis of control tissue matrices to be 2.6, 3.3, and 3.8 ng/g as emamectin B(1a) for muscle, skin, and intact muscle/skin, respectively. Likewise, the theoretical limits of quantitation (LOQ) were determined to be 6.9, 8.1, and 9.5 ng/g as emamectin B(1a) for muscle, skin, and intact muscle/skin, respectively. The lowest fortification level used for method validation was 50 ng/g, which served as the effective LOQ for the method. The overall percent recoveries (+/-% CV) were 94.4 +/- 6.89% (n = 25) for muscle, 88.4 +/- 5.35% (n = 25) for skin, and 88.0 +/- 3.73% for intact muscle/skin (n = 25). Accuracy, precision, linearity, selectivity, and ruggedness were demonstrated. The structure of the final fluorescent derivative of emamectin B(1a) free base was identified by ESI(+)/LC-MS. The frozen storage stability of [(3)H]emamectin B(1a) in tissues with incurred residues was demonstrated for approximately 15 months by radiometric analysis and for an additional approximately 13 months by fluorometric analysis for a total of

  16. Sensitometric effects of varying the intensifying screens used with Agfa Dentus ST8G and RP6 panoramic radiographic films.

    Science.gov (United States)

    Wakoh, M; Farman, A G; Scarfe, W C; Kitagawa, H; Kuroyanagi, K

    1997-07-01

    To compare the sensitometric effects and information yield of varying the intensifying screens used with both Dentus ST8G and RP6 Agfa Gevaert, Dormagen, Germany panoramic radiographic films. Four screen-film combinations were employed for each of the two film types. The screens used were blue fluorescing PX-III (Kasei Optonix, Tokyo, Japan) and Special (Siemens AG, Bensheim, Germany), as well as green fluorescing Lanex Regular (Eastman Kodak, Rochester, NY, USA) and Trimax T16 (3M, Mineapolis, Minnesota, USA). The density response for each screen-film combination was evaluated using the characteristic curves generated. Information yield, as determined by the radiographic detection of defects in an aluminium test object, was evaluated by nine observers. The characteristic curves for ST8G were different when green and blue fluorescing screens were used; however, those for RP6 varied little irrespective of the choice of intensifying screens. Observers were able to perceive defects at significantly lower radiation exposures for ST8G combined with green fluorescing screens compared with blue emitting screens. RP6 with all screen combinations provided similar image detail perceptibility at comparable exposures with ST8G with green-fluorescing screens. RP6 is suitable for use with either the spectrally matched blue emitting screens or green-emitting screens. ST8G radiographic film should always be matched to rare earth screens.

  17. Urinary arsenic speciation and its correlation with 8-OHdG in Chinese residents exposed to arsenic through coal burning

    Energy Technology Data Exchange (ETDEWEB)

    Li, X.; Pi, J.B.; Li, B.; Xu, Y.Y.; Jin, Y.P.; Sun, G.F. [China Medical University, Shenyang (China). Dept. for Occupational & Environmental Health

    2008-10-15

    In contrast to arsenicosis caused by consumption of water contaminated by naturally occurring inorganic arsenic, human exposure to this metalloid through coal burning has been rarely reported. In this study, arsenic speciation and 8-hydroxy-2'-deoxyguanosine (8-OHdG) levels in urine were determined in the Chinese residents exposed to arsenic through coal burning in Guizhou, China, an epidemic area of chronic arsenic poisoning caused by coal burning. The urinary concentrations of inorganic arsenic (iAs), monomethylarsonic acid (MMA), dimethylarsinic acid (DMA) and total arsenic (tAs) of high-arsenic exposed subjects were significantly higher than those of low-arsenic exposed residents. A biomarker of oxidative DNA damage, urinary 8-OHdG level was significantly higher in high-arsenic exposed subjects than that of low exposed. Significant positive correlations were found between 8-OHdG levels and concentrations of iAs, MMA, DMA and tAs, respectively. In addition, a significant negative correlation was observed between 8-OHdG levels and the secondary methylation ratio (DMA/(MMA + DMA)). The results suggest that chronic arsenic exposure through burning coal rich in arsenic is associated with oxidative DNA damages, and that secondary methylation capacity is potentially related to the susceptibility of individuals to oxidative DNA damage induced by arsenic exposure through coal burning in domestic living.

  18. Rapid HPLC-MS method for the simultaneous determination of tea catechins and folates.

    Science.gov (United States)

    Araya-Farias, Monica; Gaudreau, Alain; Rozoy, Elodie; Bazinet, Laurent

    2014-05-14

    An effective and rapid HPLC-MS method for the simultaneous separation of the eight most abundant tea catechins, gallic acid, and caffeine was developed. These compounds were rapidly separated within 9 min by a linear gradient elution using a Zorbax SB-C18 packed with sub 2 μm particles. This methodology did not require preparative and semipreparative HPLC steps. In fact, diluted tea samples can be easily analyzed using HPLC-MS as described in this study. The use of mass spectrometry detection for quantification of catechins ensured a higher specificity of the method. The percent relative standard deviation was generally lower than 4 and 7% for most of the compounds tested in tea drinks and tea extracts, respectively. Furthermore, the method provided excellent resolution for folate determination alone or in combination with catechins. To date, no HPLC method able to discriminate catechins and folates in a quick analysis has been reported in the literature.

  19. Direct-injection HPLC method of measuring micafungin in human plasma using a novel hydrophobic/hydrophilic hybrid ODS column.

    Science.gov (United States)

    Uranishi, Hiroaki; Nakamura, Mitsuhiro; Nakamura, Hiroki; Ikeda, Yukari; Otsuka, Mayuko; Kato, Zenichiro; Tsuchiya, Teruo

    2011-04-15

    A direct-injection HPLC-based method has been developed for determining amounts of micafungin in human plasma using a novel hydrophobic/hydrophilic hybrid ODS column. The method is easy to perform and requires only 10 μL of a filtered plasma sample. The chromatographic separations were carried out with a gradient mode. The fluorescence detection wavelengths of excitation and emission were set at 273 nm and 464 nm, respectively. Retention times for micafungin and IS were 22.4 and 23.7 min, respectively. Micafungin and FR195743 (IS) peaks were completely separated with little tailing, and no interference was observed. The calibration curve of micafungin showed good linearity in the range of 0.5-20.0 μg/mL (r(2)=1.00). The intra-day accuracy ranged from -4.5 to 5.3%. The inter-day accuracy ranged from -9.8 to 1.5%. The precisions were less than 10%. This method is useful for the determination of micafungin in human plasma. Copyright © 2011 Elsevier B.V. All rights reserved.

  20. Development and optimization of the determination of pharmaceuticals in water samples by SPE and HPLC with diode-array detection.

    Science.gov (United States)

    Pavlović, Dragana Mutavdžić; Ašperger, Danijela; Tolić, Dijana; Babić, Sandra

    2013-09-01

    This paper describes the development, optimization, and validation of a method for the determination of five pharmaceuticals from different therapeutic classes (antibiotics, anthelmintics, glucocorticoides) in water samples. Water samples were prepared using SPE and extracts were analyzed by HPLC with diode-array detection. The efficiency of 11 different SPE cartridges to extract the investigated compounds from water was tested in preliminary experiments. Then, the pH of the water sample, elution solvent, and sorbent mass were optimized. Except for optimization of the SPE procedure, selection of the optimal HPLC column with different stationary phases from different manufacturers has been performed. The developed method was validated using spring water samples spiked with appropriate concentrations of pharmaceuticals. Good linearity was obtained in the range of 2.4-200 μg/L, depending on the pharmaceutical with the correlation coefficients >0.9930 in all cases, except for ciprofloxacin (0.9866). Also, the method has revealed that low LODs (0.7-3.9 μg/L), good precision (intra- and interday) with RSD below 17% and recoveries above 98% for all pharmaceuticals. The method has been successfully applied to the analysis of production wastewater samples from the pharmaceutical industry. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Measurement of menadione in urine by HPLC.

    Science.gov (United States)

    Al Rajabi, Ala; Peterson, James; Choi, Sang-Woon; Suttie, John; Barakat, Susan; Booth, Sarah L

    2010-09-15

    Menadione is a metabolite of vitamin K that is excreted in urine. A high performance liquid chromatography (HPLC) method using a C(30) column, post-column zinc reduction and fluorescence detection was developed to measure urinary menadione. The mobile phase was composed of 95% methanol with 0.55% aqueous solution and 5% DI H(2)O. Menaquinone-2 (MK-2) was used as an internal standard. The standard calibration curve was linear with a correlation coefficient (R(2)) of 0.999 for both menadione and MK-2. The lower limit of quantification (LLOQ) was 0.3pmole menadione/mL urine. Sample preparation involved hydrolysis of menadiol conjugates and oxidizing the released menadiol to menadione. Using this method, urinary menadione was shown to increase in response to 3 years of phylloquinone supplementation. This HPLC method is a sensitive and reproducible way to detect menadione in urine. Copyright (c) 2010 Elsevier B.V. All rights reserved.

  2. [Effect of Recombinant Adenovirus AdE-SH2-Caspase 8 on the Apoptosis of Imatinib-resistant K562/G01 Cell Line].

    Science.gov (United States)

    Wang, Lin; Fei, Chang; Huang, Zheng-Lan; Li, Hui; Liu, Zhang-Lin; Feng, Wen-Li

    2015-08-01

    To investigate the effect of SH2-Caspase 8 fusion protein expressed by recombinant adenovirus AdE-SH2-Caspase8-HA-GFP (SC) on the apoptosis of K562/G01 cell line, which is a BCR/ABL positive chronic myeloid leukemia cell line and resistant to imatinib. The K562/G01 cell line was infected with AdE-SH2-Caspase 8-HA-GFP adenovirus (SC), then the cells were divided into 3 groups: AdE-SH2m-Caspase 8-HA-GFP (SmC) group, AdE-GFP (CMV) group and PBS group as control. The infection efficiency was observed under fluorescent microscopy and by flow cytometry. The expression of fusion protein SH2-Caspase 8-HA was measured by Western blot. The morphology of the cells detected by Wright's staining. The apoptosis of the cells were detected by flow cytometry and DNA ladder. The expression of Caspase 3 and PARP were detected by Western blot. The infection efficiency of SC on K562/G01 cells was high which was confirmed by fluorescent microscopy and FCM. SH2-Caspase 8-HA fusion protein were expressed correctly in K562/G01 cells. After treatment with SC the apoptosis of K562/G01 cells could be observed by microscopy. The result of FCM showed that early apoptosis of K562/G01 cells increased significantly as compared with control groups (P SH2-Caspase 8 fusion protein can induces the apoptosis of K562/G01 cells.

  3. HPLC Fingerprinting of Sennosides in Laxative Drugs with Isolation of Standard Substances from Some Senna Leaves

    Directory of Open Access Journals (Sweden)

    L. Omur Demirezer

    2011-01-01

    Full Text Available Senna leaves are one of the oldest medicinal herbs and they are used as laxative. Herbal teas which contain senna leaves are most commonly used to promote weight loss. The quality control of slimming teas which contain Senna leaves and also pharmaceutical preparations including Senna extract enriched by sennoside B was achieved by HPLC fingerprinting method. While the presence of sennoside A and B in laxative drugs was proved, it was seen to be devoid of sennosides in slimming teas. Kaempferol 3-O-β-D-gentiobioside (1, aloe-emodine 8-O-β-D-glucopyranoside (2, rhein 8-O-β-D-glucopyranoside (3, torachrysone 8-O-β-D-glucopyranoside (4, isorhamnetine 3-O-β-D-gentiobioside (5 were also isolated from Senna leaves.

  4. Development of Reverse-Phase HPLC Method for Simultaneous ...

    African Journals Online (AJOL)

    Erah

    Purpose: To develop a simple, sensitive and rapid reverse phase HPLC method for the simultaneous analysis of metoprolol succinate and hydrochlorothiazide in a solid dosage form. Methods: The .... Extraction was carried out three times with.

  5. Xanthine and 8-oxoguanine in G-quadruplexes: formation of a G·G·X·O tetrad.

    Science.gov (United States)

    Cheong, Vee Vee; Heddi, Brahim; Lech, Christopher Jacques; Phan, Anh Tuân

    2015-12-02

    G-quadruplexes are four-stranded structures built from stacked G-tetrads (G·G·G·G), which are planar cyclical assemblies of four guanine bases interacting through Hoogsteen hydrogen bonds. A G-quadruplex containing a single guanine analog substitution, such as 8-oxoguanine (O) or xanthine (X), would suffer from a loss of a Hoogsteen hydrogen bond within a G-tetrad and/or potential steric hindrance. We show that a proper arrangement of O and X bases can reestablish the hydrogen-bond pattern within a G·G·X·O tetrad. Rational incorporation of G·G·X·O tetrads in a (3+1) G-quadruplex demonstrated a similar folding topology and thermal stability to that of the unmodified G-quadruplex. pH titration conducted on X·O-modified G-quadruplexes indicated a protonation-deprotonation equilibrium of X with a pKa ∼6.7. The solution structure of a G-quadruplex containing a G·G·X·O tetrad was determined, displaying the same folding topology in both the protonated and deprotonated states. A G-quadruplex containing a deprotonated X·O pair was shown to exhibit a more electronegative groove compared to that of the unmodified one. These differences are likely to manifest in the electronic properties of G-quadruplexes and may have important implications for drug targeting and DNA-protein interactions. © The Author(s) 2015. Published by Oxford University Press on behalf of Nucleic Acids Research.

  6. Comparative study of the hypocholesterolemic, antidiabetic effects of four agro-waste Citrus peels cultivars and their HPLC standardization

    Directory of Open Access Journals (Sweden)

    Nesrin M. Fayek

    Full Text Available ABSTRACT Citrus is an economically important fruit for Egypt, but its peel also is one of the major sources of agricultural waste. Due to its fermentation, this waste causes many economic and environmental problems. Therefore it is worthwhile to investigate ways to make use of this citrus waste generated by the juice industry. This study was aimed to explore the hypocholesterolemic, antidiabetic activities of four varieties of citrus peels agrowastes, to isolate the main flavonoids in the active fractions and to quantify them by HPLC method for nutraceutical purposes. All the tested samples of the agro-waste Citrus fruits peels showed significant decrease in cholesterol, triacylglyceride and glucose. The most decrease in cholesterol level was observed by mandarin peels aqueous homogenate and its hexane fraction (59.3% and 56.8%, respectively reaching the same effect as the reference drug used (54.7%. Mostly, all samples decrease triacylglyceride (by 36%–80.6% better than the reference drug used (by 35%, while, glucose was decreased (by 71.1%–82.8 and 68.6%–79.6%, respectively mostly by the aqueous homogenates (except lime and alcoholic extracts (except mandarin of Citrus fruits peels better than the reference drug used (by 68.3%. All the isolated pectin, from the four cultivars, has significant effect on the three parameters. The comparative HPLC rapid quantification of nobiletin in the different by-product citrus varieties hexane fractions revealed that nobiletin is present in higher concentration in mandarin (10.14% than the other species. Nobiletin and 4′,5,7,8-tetramethoxy flavone were isolated from mandarin peels hexane fraction by chromatographic fractionation. This is the first report of the comparative HPLC quantification of nobiletin and biological studies of different citrus peels species as agro-waste products. Based on these results, we suggest the possibility that Citrus fruits peels may be considered as an antidiabetic and

  7. Analysis of taxines in Taxus plant material and cell cultures by hplc photodiode array and hplc-electrospray mass spectrometry

    NARCIS (Netherlands)

    Theodoridis, G.; Laskaris, G.; Rozendaal, E.L.M.; Verpoorte, R.

    2001-01-01

    A semi-purified Taxus baccata needles extract was analysed by RP-HPLC. More than 18 taxines and cinnamates were detected by photodiode array detection and LC-MS, 10 of them being positively identified. Furthermore, 10-deacetyl baccatin III (paclitaxel's main precursor) and other taxanes were also

  8. The political process in global health and nutrition governance: the G8's 2010 Muskoka Initiative on Maternal, Child, and Newborn Health.

    Science.gov (United States)

    Kirton, John; Kulik, Julia; Bracht, Caroline

    2014-12-01

    Why do informal, plurilateral summit institutions such as the Group of Eight (G8) major market democracies succeed in advancing costly public health priorities such as maternal, newborn, and child health (MNCH), even when the formal, multilateral United Nations (UN) system fails to meet such goals, when G8 governments afflicted by recession, deficit, and debt seek to cut expenditures, and when the private sector is largely uninvolved, despite the growing popularity of public-private partnerships to meet global health and related nutrition, food, and agriculture needs? Guided by the concert-equality model of G8 governance, this case study of the G8's 2010 Muskoka Initiative on MNCH traces the process through which that initiative was planned within Canada, internationally prepared through negotiations with Canada's G8 partners, produced at Muskoka by the leaders in June, multiplied in its results by the UN summit in September, and reinforced by the new accountability mechanism put in place. It finds that the Muskoka summit succeeded in mobilizing major money and momentum for MNCH. This was due to the initiative and influence of children-focused nongovernmental organizations (NGOs), working with committed individuals and agencies within the host Canadian government, as well as supportive public opinion and the help of those in the UN responsible for realizing its Millennium Development Goals. Also relevant were the democratic like-mindedness of G8 leaders and their African partners, the deference of G8 members to the host's priority, and the need of the G8 to demonstrate its relevance through a division of labor between it and the new Group of Twenty summit. This study shows that G8 summits can succeed in advancing key global health issues without a global shock on the same subject to galvanize agreement and action. It suggests that, when committed, focused NGOs and government officials will lead and the private sector will follow, but that there will be a lag in the

  9. An Inexpensive Digital Gradient Controller for HPLC.

    Science.gov (United States)

    Brady, James E.; Carr, Peter W.

    1983-01-01

    Use of gradient elution techniques in high performance liquid chromatography (HPLC) is often essential for direct separation of complex mixtures. Since most commercial controllers have features that are of marginal value for instructional purposes, a low-cost controller capable of illustrating essential features of gradient elution was developed.…

  10. Sensitometric properties of Agfa Dentus OrthoLux, Agfa Dentus ST8G, and Kodak Ektavision panoramic radiographic film.

    Science.gov (United States)

    Wakoh, M; Nishikawa, K; Kobayashi, N; Farman, A G; Kuroyanagi, K

    2001-02-01

    The purpose of this study was to compare the sensitometric properties of and visualization of anatomical structures with Agfa OrthoLux green-sensitive panoramic radiographic film, Agfa ST8G green sensitive panoramic radiographic film, and Kodak Ektavision green-sensitive panoramic radiographic film used in combination with an Agfa Ortho Regular 400 imaging screen, Kodak Ektavision imaging screen, and Kodak Lanex Regular imaging screen. The density response and resolution of panoramic radiographic film/intensifying screen combinations was evaluated by means of Hunter and Driffield curves, modulation transfer functions, and noise-equivalent number of quanta. Image clarity of selected anatomical structures was rated independently by 6 oral and maxillofacial radiologists. The ISO speed for the Agfa OrthoLux panoramic radiographic film combinations was the fastest, and the ISO speed for the Kodak Ektavision green-sensitive panoramic radiographic film combinations was the slowest. The average gradient for the Agfa ST8G systems was relatively steep in comparison with those for the other film/screen combinations. The modulation transfer functions for the Kodak Ektavision film were higher than those for the other films, irrespective of the screen combination used, and those for Agfa OrthoLux film were slightly higher than those for Agfa ST8G film. The noise-equivalent number of quanta for the Agfa ST8G film/screen combinations was lower than those for the other film/screen combinations. The noise-equivalent number of quanta for the Kodak Ektavision film/screen combinations was well within the high-frequency range, whereas Agfa OrthoLux combined with either the Kodak Ektavision imaging screen or the Kodak Lanex Regular imaging screen produced a noise-equivalent number of quanta similar to those of the Kodak Ektavision film/screen combinations in the low-frequency range. Agfa OrthoLux was perceived to provide clearer images of the selected anatomical details than Agfa ST8G

  11. HPLC/Fluorometric Detection of Carvedilol in Real Human Plasma Samples Using Liquid-Liquid Extraction.

    Science.gov (United States)

    Yilmaz, Bilal; Arslan, Sakir

    2016-03-01

    A simple, rapid and sensitive high-performance liquid chromatography (HPLC) method has been developed to quantify carvedilol in human plasma using an isocratic system with fluorescence detection. The method included a single-step liquid-liquid extraction with diethylether and ethylacetate mixture (3 : 1, v/v). HPLC separation was carried out by reversed-phase chromatography with a mobile phase composed of 20 mM phosphate buffer (pH 7)-acetonitrile (65 : 35, v/v), pumped at a flow rate of 1.0 mL/min. Fluorescence detection was performed at 240 nm (excitation) and 330 nm (emission). The calibration curve for carvedilol was linear from 10 to 250 ng/mL. Intra- and interday precision values for carvedilol in human plasma were plasma averaged out to 91.8%. The limits of detection and quantification of carvedilol were 3.0 and 10 ng/mL, respectively. Also, the method was successfully applied to three patients with hypertension who had been given an oral tablet of 25 mg carvedilol. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  12. High prevalence of exon 8 G533C mutation in apparently sporadic medullary thyroid carcinoma in Greece.

    Science.gov (United States)

    Sarika, H L; Papathoma, A; Garofalaki, M; Vasileiou, V; Vlassopoulou, B; Anastasiou, E; Alevizaki, M

    2012-12-01

    Genetic screening for ret mutation has become routine practice in the evaluation of medullary thyroid carcinoma (MTC). Approximately 25% of these tumours are familial, and they occur as components of the multiple endocrine neoplasia type 2 syndromes (MEN 2A and 2B) or familial MTC. In familial cases, the majority of mutations are found in exons 10, 11, 13, 14 or 15 of the ret gene. A rare mutation involving exon 8 (G533C) has recently been reported in familial cases of MTC in Brazil and Greece; some of these cases were originally thought to be sporadic. The aim of this study was to re-evaluate a series of sporadic cases of MTC, with negative family history, and screen them for germline mutations in exon 8. Genomic DNA was extracted from peripheral lymphocytes in 129 unrelated individuals who had previously been characterized as 'sporadic' based on the negative family history and negative screening for ret gene mutations. Samples were analysed in Applied Biosystems 7500 real-time PCR and confirmed by sequencing. The G533C exon 8 mutation was identified in 10 of 129 patients with sporadic MTC. Asymptomatic gene carriers were subsequently identified in other family members. In our study, we found that 7·75% patients with apparently sporadic MTC do carry G533C mutation involving exon 8 of ret. We feel that there is now a need to include exon 8 mutation screening in all patients diagnosed as sporadic MTC, in Greece. © 2012 Blackwell Publishing Ltd.

  13. Characterization of [8-ethyl]-chlorophyll c3 from Emiliania huxleyi.

    Science.gov (United States)

    Álvarez, Susana; Zapata, Manuel; Garrido, José L; Vaz, Belén

    2012-06-04

    We report herein the isolation and complete characterization of a member of the chlorophyll c family, designated as [8-ethyl]-chlorophyll c(3) ([8-ethyl]-chl c(3)). Structural elucidation of this pigment rested on the analysis of mono- and bidimensional NMR, UV-VIS spectroscopy and ESI-MS data, and the configuration at the 13(2) position on chiral HPLC analysis.

  14. Novel assay of antibacterial components in manuka honey using lucigenin-chemiluminescence-HPLC

    Energy Technology Data Exchange (ETDEWEB)

    Karasawa, Koji, E-mail: koji180@pharm.showa-u.ac.jp; Haraya, Shiomi; Okubo, Sachie; Arakawa, Hidetoshi

    2017-02-15

    Five components (hydrogen peroxide, methylglyoxal, dihydroxyacetone, fructose and glucose) of New Zealand manuka honey (Leptospermum scoparium) were analyzed using lucigenin chemiluminescence high-performance liquid chromatography (lucigenin-CL-HPLC). We focused on active oxygen species produced from the components in order to easily detect these five components contained in manuka honey. H{sub 2}O{sub 2} and O{sub 2}{sup −} generated from these components were identified by lucigenin-CL and electron spin resonance (ESR), and the bactericidal effect of ROS was confirmed using E. coli. The previously reported assays for Manuka honey components have low specificities and require complicated preprocessing methods. As our results, the detection and identification of these components were possible within 30 min in lucigenin-CL-HPLC system, without any special treatment. It is considered that lucigenin-CL-HPLC is useful for the quality control and the analysis of various honey. - Highlights: • Antibacterial components in manuka honey by HPLC with lucigenin-CL. • Five antibacterial compounds measured via generation of reactive oxygen species. • Simple, sensitive and useful for quality control and analysis of antibacterial honey.

  15. Determination of blood cyanide by HPLC-MS.

    Science.gov (United States)

    Tracqui, A; Raul, J S; Géraut, A; Berthelon, L; Ludes, B

    2002-04-01

    An original high-performance liquid chromatographic-mass spectrometric (HPLC-MS) procedure was developed for the determination of cyanide (CN) in whole blood. After the addition of K13C15N as internal standard, blood was placed in a microdiffusion device, the inner well of which was filled with a mixture of taurine (50mM in water)/naphthalene-2,3-dicarboxaldehyde (NDA, 10mM in methanol)/methanol/ concentrated (approximately 20%) ammonia solution (25:25:45:5, v/v). Concentrated H2SO4 was added to the blood sample, and the microdiffusion chamber was sealed. After 30 min of gentle agitation, 2 microL of the contents of the inner vial were pipetted and directly injected onto a NovaPak C18 HPLC column. Separation was performed by a gradient of acetonitrile in 2mM NH4COOH, pH 3.0 buffer (35-80% in 10 min). Detection was done with a Perkin-Elmer Sciex API-100 mass analyzer with an ionspray interface, operated in the negative ionization mode. MS data were collected as either TIC or SIM at m/z (299 + 191) and (301 + 193) for the derivatives formed with CN and 13C15N, respectively. Inspired by previous works dealing with the complexation of CN by NDA + taurine to form a 1-cyano [f] benzoisoindole derivative analyzed by HPLC-fluorimetry, this method appears simple, rapid, and extremely specific. Limits of detection and quantitation for blood CN are 5 and 15 ng/mL, respectively. The use of 13C15N as internal standard allows the quantitation of CN with elegance and accuracy in comparison with previously reported methods.

  16. Simultaneous determination of 15 phenolic constituents of Chinese black rice wine by HPLC-MS/MS with SPE.

    Science.gov (United States)

    Wang, Yutang; Liu, Yuanyuan; Xiao, Chunxia; Liu, Laping; Hao, Miao; Wang, Jianguo; Liu, Xuebo

    2014-06-01

    This study established a new method for quantitative and qualitative determination of certain components in black rice wine, a traditional Chinese brewed wine. Specifically, we combined solid-phase extraction and high-performance liquid chromatography (HPLC) with triple quadrupole mass spectrometry (MS/MS) to determine 8 phenolic acids, 3 flavonols, and 4 anthocyanins in black rice wine. First, we clean samples with OASIS HLB cartridges and optimized extraction parameters. Next, we performed separation on a SHIM-PACK XR-ODS column (I.D. 3.0 mm × 75 mm, 2.2 μm particle size) with a gradient elution of 50% aqueous acetonitrile (V/V) and water, both containing 0.2% formic acid. We used multiple-reaction monitoring scanning for quantification, with switching electrospray ion source polarity between positive and negative modes in a single chromatographic run. We detected 15 phenolic compounds properly within 38 min under optimized conditions. Limits of detection ranged from 0.008 to 0.030 mg/L, and average recoveries ranged from 60.8 to 103.1% with relative standard deviation ≤8.6%. We validated the method and found it to be sensitive and reliable for quantifying phenolic compounds in rice wine matrices. This study developed a new, reliable HPLC-MS/MS method for simultaneous determination of 15 bioactive components in black rice wine. This method was validated and found to be sensitive and reliable for quantifying phenolic compounds in rice wine. © 2014 Institute of Food Technologists®

  17. Estimation of Ziprasidone Hydrochloride Monohydrate in Bulk and Capsules by Reverse Phase HPLC

    Directory of Open Access Journals (Sweden)

    B. Sudha Rani

    2006-01-01

    Full Text Available A reverse phase HPLC method is described for the determination of Ziprasidone HCl mono hydrate in bulk and pharmaceutical dosage forms. Chromatography was carried out on an ODS C18 column using a mixture of methanol and phosphate buffer (55:45v/v as the mobile phase at a flow rate of 1mL/min. Detection was carried out at 314nm. The retension time of the drug was 4.522 min. The method produced linear responses in the concentration range of 0.5-30 μg /mL of Ziprasidone HCl mono hydrate.The method was found to be applicable for determination of the drug in capsules.

  18. Serum 8-OHdG and HIF-1α levels: do they affect the development of malignancy in patients with hypoactive thyroid nodules?

    Science.gov (United States)

    Ece, Harman; Mehmet, Erdogan; Cigir, Biray Avci; Yavuz, Dodurga; Muammer, Karadeniz; Cumhur, Gunduz; Mustafa, Harman; Sevki, Cetinkalp; Fusun, Saygılı; Gokhan, Ozgen Ahmet

    2013-01-01

    This study aimed to evaluate 8-OHdG and hypoxia-inducible factor 1 (HIF-1α) levels in patients with hypoactive thyroid nodules (toxic multi-nodular goiter, Graves' disease, and Hashimoto's thyroiditis), as these parameters may be related to oxidative stress and the pathogenesis of cancer. The study included patients diagnosed with Graves' disease (n = 20), toxic multinodular goiter (n = 20), and Hashimoto thyroiditis (n = 20), and 20 healthy controls. HIF-1α levels were measured in blood samples and 8-OHdG levels were measured in urine - both via ELISA. HIF-1α and 8-OHdG levels were significantly higher in the patient groups than in the control group (p 0.05). There was no significant difference in 8-OHdG or HIF-1α levels between the patients with biopsy results that were benign, malignant, and non-diagnostic (p > 0.05). Serum HIF-1α and urine 8-OHdG levels were significantly higher in the patients with thyroid diseases; however, a relationship with cancer was not observed.

  19. Automated synthesis with HPLC purification of 18F-FMISO as specific molecular imaging probe of tumor hypoxia

    International Nuclear Information System (INIS)

    Wang Mingwei; Zhang Yingjian; Zhang Yongping

    2012-01-01

    An improved automated synthesis of 1-H-1-(3-[ 18 F] fluoro-2-hydroxypropyl)-2-nitro-imidazole ( 18 F-FMISO), a specific molecular imaging probe of tumor hypoxia, was developed using an upgraded Explora GN module integrated with Explora LC for HPLC purification in this study. The radiochemical synthesis of 18 F-FMISO was started with precursor 1-( 2'-nitro-1'-imidazolyl)-2-O-tetrahydropyranyl-3-O-tosyl-propanediol (NITTP) and included nucleophilic [ 18 F] radio-fluorination at 120℃ for 5 min and hydrolysis at 130℃ for 8 min. The automated synthesis of 18 F-FMISO, presenting fast, reliable and multi-run features, could be completed with the total synthesis time of less than 65 min and radiochemical yield of 25%∼35% (without decay correction). The quality control of 18 F-FMISO was identical with the radiopharmaceutical requirements, especially the radiochemical purity of greater than 99% and high chemical purity and specific activity own to HPLC purification. (authors)

  20. Assay of flavonoid aglycones from the species of genus Sideritis (Lamiaceae) from Macedonia with HPLC-UV DAD.

    Science.gov (United States)

    Janeska, Bisera; Stefova, Marina; Alipieva, Kalina

    2007-09-01

    Flavonoids obtained from Sideritis species (Lamiaceae), S. raeseri and S. scardica, grown in Macedonia were studied. Qualitative and quantitative analyses of the flavonoid aglycones were performed using high-performance liquid chromatography (HPLC) with a UV diode array detector. Extracts were prepared by acid hydrolysis in acetone, re-extraction in ethyl acetate and evaporation to dryness; the residue dissolved in methanol was subjected to HPLC analysis.Isoscutellarein, chryseriol and apigenin were identified in the extracts. Also, a 4'-methyl ether derivative of isoscutellarein was found, together with hypolaetin and its methyl ether derivative, which were identified according to previously isolated glycosides and literature data. Quantitation was performed using calibration with apigenin.According to this screening analysis, the samples of the genus Sideritis from Macedonia are rich in polyhydroxy flavones and analogous with the previously studied Mediterranean Sideritis species from the Ibero-North African and Greek Sideritis species with respect to the presence of 8-OH flavones and their derivatives.

  1. Determination of cadmium and lead species and phytochelatins in pea (Pisum sativum) by HPLC-ICPMS and HPLC-ESIMSn

    International Nuclear Information System (INIS)

    Baralkiewicz, D.; Magorzata, K.; Piechalak, A.; Tomaszewska, B.

    2009-01-01

    Full text: Trace elements play an important role in the functioning of life on our planet. Some of them can be highly toxic, whereas others can be essential. These effects are very often related to particular form in which the element is present. Often these different chemical forms of a particular element or its compounds are referred to as 'species'. Cadmium and lead are widespread heavy metal pollutants released into the environment by human activities. The presence of Pb 2+ and Cd 2+ in the environment leads to a numerous disturbances in many metabolic processes in plants. Inhibition of growth is a major symptom. Hyphenated techniques, such as HPLC-ICPMS and HPLC-ESIMSn seem to be the best analytical instruments to study metal speciation in plants. In our study, we used hyphenated techniques to identify compounds engaged in Cd and Pb metabolism and to perform analysis of metal complexes induced in Pisum sativum exposed to cadmium and lead. These identified compounds might be valuable source of information to study metal accumulation mechanism for bioremediation processes. (author)

  2. 77 FR 13232 - Security Zones; G8/North Atlantic Treaty Organization (NATO) Summit, Chicago, IL

    Science.gov (United States)

    2012-03-06

    ... political figures, the G8/NATO Summit is expected to draw significant domestic and international media... mitigate the threat of violence and ensure the safety and security of those who attend, participate, and... NATO; the high concentration of dignitaries and political figures; the expected interest of domestic...

  3. Determination of Tinopal CBS-X in rice papers and rice noodles using HPLC with fluorescence detection and LC-MS/MS.

    Science.gov (United States)

    Ko, Kyung Yuk; Lee, Chae A; Choi, Jae Chon; Kim, Meehye

    2014-01-01

    To date there have been no reports of methods to determine Tinopal CBS-X. We developed a rapid and simple method to determine the Tinopal CBS-X content in rice noodles and rice papers using HPLC equipped with fluorescence detection. Heating the rice noodles and rice papers to 80°C after adding 75% methanol solution induced the release of Tinopal CBS-X from processed rice products. Tinopal CBS-X was separated using an isocratic mobile phase comprising 50% acetonitrile/water containing 0.4% tetrabutyl ammonium hydrogen sulphate at pH 8.0. The samples suspected to be positive by HPLC analysis were then confirmed by LC-MS/MS analysis. This study also investigated the Tinopal CBS-X content of three rice noodle products and two rice papers. The limits of quantification for rice papers and rice noodles were 1.58 and 1.51 µg kg(-1), respectively, and their correlation curves showed good linearity with r(2) ≥ 0.9997 and ≥ 0.9998, respectively. Moreover, rice papers had recoveries of 70.3-83.3% with precision ranging from 5.0% to 7.9%, whereas rice noodles had slightly lower recoveries of 63.4-78.7% and precisions of 8.5-11.5%. Only one rice noodle product contained Tinopal CBS-X, at around 2.1 mg kg(-1), whereas it was not detected in four other samples. Consequently, Tinopal CBS-X from rice noodles and rice papers can be successfully detected using the developed pre-treatment and ion-pairing HPLC system coupled with fluorescence detection.

  4. Determination of hydroxyurea in human plasma by HPLC-UV using derivatization with xanthydrol.

    Science.gov (United States)

    Legrand, Tiphaine; Rakotoson, Marie-Georgine; Galactéros, Frédéric; Bartolucci, Pablo; Hulin, Anne

    2017-10-01

    A simple and rapid high performance liquid chromatography (HPLC) method using ultraviolet (UV) detection was developed to determine hydroxyurea (HU) concentration in plasma sample after derivatization with xanthydrol. Two hundred microliters samples were spiked with methylurea (MeU) as internal standard and proteins were precipitated by adding methanol. Derivatization of HU and MeU was immediately performed by adding 0.02M xanthydrol and 1.5M HCl in order to obtain xanthyl-derivatives of HU and MeU that can be further separated using HPLC and quantified using UV detection at 240nm. Separation was achieved using a C18 column with a mobile phase composed of 20mM ammonium acetate and acetonitrile in gradient elution mode at a flow rate of 1mL/min. The total analysis time did not exceed 18min. The method was found linear from 5 to 400μM and all validation parameters fulfilled the international requirements. Between- and within-run accuracy error ranged from -4.7% to 3.2% and precision was lower than 12.8%. This simple method requires small volume samples and can be easily implemented in most clinical laboratories to develop pharmacokinetics studies of HU and to promote its therapeutic monitoring. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. The effect of vitamin C and E combination on sperm quality and cement 8-OHdG level of smoke exposed rats

    Directory of Open Access Journals (Sweden)

    Eviana Budiartanti Sutanto

    2017-09-01

    Full Text Available Introduction: Cigarette smoke causes oxidative stress which results in reduced sperm concentration, motility and morphology, also increased levels of 8-OHdG as a marker of DNA damage. Vitamin C and E have potential role in repairing spermatozoa damages. The aim of this study was to determine the effect of vitamin C and E combination on sperm quality and cement 8-OHdG level of smoke exposed rats. Methods: This study used a post test only control group design among 18 male Wistar rats subject, aged 8 week, 150-200 grams body weight (BW. The subject was randomly divided into 3 groups, K1: control, K2: cigarettes smoke exposed, K3: cigarettes smoke exposed and given a combination of 0.045 mg/gBW vitamin C and 0.036 IU/gBW vitamin E per oral. Analysis was done on day 21 using one-way ANOVA and post-hoc LSD for sperm concentration, motility and morphology; using Kruskal-Wallis and Mann-Whitney tests for cement 8- OHdG levels. Results: The lowest sperm concentration was found in   K2 (K2  32.59  million/mL,  K1 47.91 million/mL, K 339.43 million/mL; the lowest normal sperm motility was found in K2 (K 238.97%, K 164.57%, K3 51.43%; the lowest normal sperm morphology was found in K2 (K2 27.56%, K 138.36%, K 331.18%; and the highest cement 8- OHdG level was found in K2 (K2 20.18ng/mL, K1 3.43ng/mL, K3 5.28ng/mL. Conclusion: Combination of vitamin C and E can improve sperm concentration, motility and morphology and decrease cement 8-OHdG levels of smoke exposed rats.

  6. Enantiomeric separation of iridium (III) complexes using HPLC chiral stationary phases based on amylose derivatives

    International Nuclear Information System (INIS)

    Kim, Hee Eun; Seo, Na Hyeon; Hyun, Myung Ho

    2016-01-01

    Cyclometalated iridium (III) complexes formed with three identical cyclometalating (C-N) ligands (homoleptic) or formed with two cyclometalating (C-N) ligands and one ancillary (LX) ligand (heteroleptic) have been known as highly phosphorescent materials and, thus, they have been utilized as efficient phosphorescent dopants in organic light emitting diodes (OLEDs) 1–3 or as effective phosphorescent chemosensors. 4–7 Cylometalated iridium (III) complexes are chiral compounds consisting of lambda (Λ, left-handed) and delta (Δ, right-handed) isomers. Racemic cyclometa- lated iridium (III) complexes emit light with no net polarization, but optically active cyclometalated iridium (III) complexes emit circularly polarized light. 8,9 Circularly polarized light can be used in various fields including highly efficient three dimensional electronic devices, photo nic devices for optical data storage, biological assays, and others. 8,9 In order to obtain optically active cylometalated iridium (III) complexes and to determine the enantiomeric composition of optically active cylometalated iridium (III) complexes, liquid chromatogr aphic enantiomer separation method on chiral stationary phases (CSPs) has been used. For example, Okamoto and coworkers first reported the high performance liquid chromatographic (HPLC) direct enantiomeric separation of two homoleptic cylometalated iridium (III) complexes on immobilized amylose tris(3,5- dimethylphenylcarbamate) (Chiralpak IA), coated cellulose tris(3,5-dimethylphenylcarbamate) (Chiralc el OD), and coated cellulose tris(4-methylbenzoate) (Chiralce l OJ). 10 Supercritical fluid chromatography (SFC) was also used by Bernhard and coworkers for the enantiomeric separation of cylometalated iridium (III) complexes on coated amylose tris(3,5-dimethylphenylcarbamate) (Chiralpak AD-H). 8 However, the general use of the HPLC method for the direct enantiomeric separation of homoleptic

  7. Enantiomeric separation of iridium (III) complexes using HPLC chiral stationary phases based on amylose derivatives

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Hee Eun; Seo, Na Hyeon; Hyun, Myung Ho [Dept. of Chemistry and Chemistry Institute for Functional Materials, Pusan National University, Busan (Korea, Republic of)

    2016-12-15

    Cyclometalated iridium (III) complexes formed with three identical cyclometalating (C-N) ligands (homoleptic) or formed with two cyclometalating (C-N) ligands and one ancillary (LX) ligand (heteroleptic) have been known as highly phosphorescent materials and, thus, they have been utilized as efficient phosphorescent dopants in organic light emitting diodes (OLEDs) 1–3 or as effective phosphorescent chemosensors. 4–7 Cylometalated iridium (III) complexes are chiral compounds consisting of lambda (Λ, left-handed) and delta (Δ, right-handed) isomers. Racemic cyclometa- lated iridium (III) complexes emit light with no net polarization, but optically active cyclometalated iridium (III) complexes emit circularly polarized light. 8,9 Circularly polarized light can be used in various fields including highly efficient three dimensional electronic devices, photo nic devices for optical data storage, biological assays, and others. 8,9 In order to obtain optically active cylometalated iridium (III) complexes and to determine the enantiomeric composition of optically active cylometalated iridium (III) complexes, liquid chromatogr aphic enantiomer separation method on chiral stationary phases (CSPs) has been used. For example, Okamoto and coworkers first reported the high performance liquid chromatographic (HPLC) direct enantiomeric separation of two homoleptic cylometalated iridium (III) complexes on immobilized amylose tris(3,5- dimethylphenylcarbamate) (Chiralpak IA), coated cellulose tris(3,5-dimethylphenylcarbamate) (Chiralc el OD), and coated cellulose tris(4-methylbenzoate) (Chiralce l OJ). 10 Supercritical fluid chromatography (SFC) was also used by Bernhard and coworkers for the enantiomeric separation of cylometalated iridium (III) complexes on coated amylose tris(3,5-dimethylphenylcarbamate) (Chiralpak AD-H). 8 However, the general use of the HPLC method for the direct enantiomeric separation of homoleptic.

  8. Climate paradox of the G-8: legal obligations, policy declarations and implementation gap

    Directory of Open Access Journals (Sweden)

    Hans Guenter Brauch

    2012-01-01

    Full Text Available This article analyzes the climate policy performance of the G-8 from 1992 to 2012 based on their legal commitments (Annex-1 and Annex-B countries under the UNFCCC (1992 and the Kyoto Protocol (1997 and their policy declarations on their GHG reduction goals until 2050. A climate paradox has emerged due to a growing implementation gap in Canada, USA and Japan, while Russia, Germany, UK, France and Italy fulfilled their GHG reduction obligation.

  9. Identification and quantification of caffeoylquinic acids and flavonoids from artichoke (Cynara scolymus L.) heads, juice, and pomace by HPLC-DAD-ESI/MS(n).

    Science.gov (United States)

    Schütz, Katrin; Kammerer, Dietmar; Carle, Reinhold; Schieber, Andreas

    2004-06-30

    A method for the identification and quantification of phenolic compounds from artichoke (Cynara scolymus L.) heads, juice, and pomace by HPLC with diode array and mass spectrometric detection was developed. Among the 22 major compounds, 11 caffeoylquinic acids and 8 flavonoids were detected. Quantification of individual compounds was carried out by external calibration. Apigenin 7-O-glucuronide was found to be the major flavonoid in all samples investigated. 1,5-Di-O-caffeoylquinic acid represented the major hydroxycinnamic acid, with 3890 mg/kg in artichoke heads and 3269 mg/kg in the pomace, whereas in the juice 1,3-di-O-caffeoylquinic acid (cynarin) was predominant, due to the isomerization during processing. Total phenolic contents of approximately 12 g/kg on a dry matter basis revealed that artichoke pomace is a promising source of phenolic compounds that might be recovered and used as natural antioxidants or functional food ingredients.

  10. Mass-gathering Medicine: Risks and Patient Presentations at a 2-Day Electronic Dance Music Event.

    Science.gov (United States)

    Lund, Adam; Turris, Sheila A

    2015-06-01

    Music festivals, including electronic dance music events (EDMEs), increasingly are common in Canada and internationally. Part of a US $4.5 billion industry annually, the target audience is youth and young adults aged 15-25 years. Little is known about the impact of these events on local emergency departments (EDs). Drawing on prospective data over a 2-day EDME, the authors of this study employed mixed methods to describe the case mix and prospectively compared patient presentation rate (PPR) and ambulance transfer rate (ATR) between a first aid (FA) only and a higher level of care (HLC) model. There were 20,301 ticketed attendees. Seventy patient encounters were recorded over two days. The average age was 19.1 years. Roughly 69% were female (n=48/70). Forty-six percent of those seen in the main medical area were under the age of 19 years (n=32/70). The average length of stay in the main medical area was 70.8 minutes. The overall PPR was 4.09 per 1,000 attendees. The ATR with FA only would have been 1.98; ATR with HLC model was 0.52. The presence of an on-site HLC team had a significant positive effect on avoiding ambulance transfers. Twenty-nine ambulance transfers and ED visits were avoided by the presence of an on-site HLC medical team. Reduction of impact to the public health care system was substantial. Electronic dance music events have predictable risks and patient presentations, and appropriate on-site health care resources may reduce significantly the impact on the prehospital and emergency health resources in the host community.

  11. Isolation and characterization of a microperoxidase-8 with a modified histidine axial ligand

    NARCIS (Netherlands)

    Primus, J.L.; Boeren, S.; Nielen, M.W.F.; Vervoort, J.; Banci, L.; Rietjens, I.M.C.M.

    2002-01-01

    Microperoxidase-8, Fe(III)MP-8, the heme octapeptide obtained by horse heart cytochrome c digestion, was studied in the presence of H 2O 2. A modified form of the catalyst was isolated by HPLC and showed a UV/visible spectrum similar to that of Fe(III)MP-8. ESI-MS measurements revealed a 16 Da

  12. Identification of G-phase in aged cast CF 8 type stainless steel

    International Nuclear Information System (INIS)

    Bentley, J.; Miller, M.K.; Brenner, S.S.; Spitznagel, J.A.

    1985-01-01

    The microstructure of as-cast and aged CF 8 type stainless steel, used for the primary coolant pipes in pressurized light-water nuclear reactors, is being studied by analytical electron microscopy (AEM) and atom probe field-ion microscopy (APFIM). The phase transformations of the ferrite (approx. 19 vol % of the duplex structure) that occur after aging at 673 K for 7500 h are described by Miller et al. The present work deals with the identification of G-phase (prototype compound Ni 16 Ti 6 Si 7 ) observed in the ferrite of aged material. 2 references, 3 figures

  13. Screening and Analysis of the Potential Bioactive Components of Poria cocos (Schw. Wolf by HPLC and HPLC-MSn with the Aid of Chemometrics

    Directory of Open Access Journals (Sweden)

    Ling-Fang Wu

    2016-02-01

    Full Text Available The aim of the present study was to establish a new method based on Similarity Analysis (SA, Cluster Analysis (CA and Principal Component Analysis (PCA to determine the quality of different samples of Poria cocos (Schw. Wolf obtained from Yunnan, Hubei, Guizhou, Fujian, Henan, Guangxi, Anhui and Sichuan in China. For this purpose 15 samples from the different habitats were analyzed by HPLC-PAD and HPLC-MSn. Twenty-three compounds were detected by HPLC-MSn, of which twenty compounds were tentatively identified by comparing their retention times and mass spectrometry data with that of reference compounds and reviewing the literature. The characteristic fragmentations were summarized. 3-epi-Dehydrotumulosic acid (F13, 3-oxo-16α,25-dihydroxylanosta-7,9(11,24(31-trien-21-oic acid (F4, 3-oxo-6,16α-dihydroxylanosta-7,9(11,24(31-trien-21-oic acid (F7 and dehydropachymic acid (F15 were deemed to be suitable marker compounds to distinguish between samples of different quality according to CA and PCA. This study provides helpful chemical information for further anti-tumor activity and active mechanism research on P. cocos. The results proved that fingerprint combined with a chemometric approach is a simple, rapid and effective method for the quality discrimination of P. cocos.

  14. A new methodology for sampling blackflies for the entomological surveillance of onchocerciasis in Brazil.

    Directory of Open Access Journals (Sweden)

    Érika S do Nascimento-Carvalho

    Full Text Available The effectiveness of the MosqTent® trap was evaluated in endemic area to onchocerciasis in Brazil. This study seeks to provide subsidies for the monitoring of the onchocerciasis transmission in the country. The study was carried out at the Homoxi and Thirei villages, located in the Yanomami Indigenous Land, in the state of Roraima. This area presents hyperendemicity, high blackflies densities, large population migrations and mining activities. The Homoxi and Thirei villages are assisted by the Brazilian Ministry of Health. To conduct the present study, the village leader, health leaders and the Brazilian Ethics Committee were consulted. Blackflies captures were carried out simultaneously at the Homoxi and Thirei, using systematized methods to allow for comparisons between the traditional Human Landing Catch (HLC and HLC protected by the MosqTent®. The female blackflies were captured at two equidistant capture stations per locality, by two collectors per station, for five consecutive days. Individuals captured by interval/station/day were counted, identified and maintained at -20°C. The underlying probability distributions and the differences between the methods for the independent sample data were verified in a comparative statistical analysis between the use of the MosqTent® and the HLC. A total of 10,855 antropophilic blackflies were captured by both methodologies. A total of 7,367 (67.87% blackflies belonging to seven species were captured by MosqTent® -Simulium incrustatum s.l (99.06%; S. guianense s.l (0.74%, S. oyapockense s.l (0.01%, S. exiguum (0.10%, S. metallicum (0.05%, S. ochraceum (0.03% and S. minusculum s.l (0.01%. Moreover, 3,488 (32.14% blackflies belonging to four species were captured by HLC-S. incrustatum s.l (98.33%; S. guianense s.l (1.38%, S. oyapockense s.l (0.26% and S. metallicum (0.03%. The MosqTent® was more effective and efficient when compared to HLC. When comparing total blackflies captured/day, the Mosq

  15. A new methodology for sampling blackflies for the entomological surveillance of onchocerciasis in Brazil.

    Science.gov (United States)

    Nascimento-Carvalho, Érika S do; Cesário, Raquel de Andrade; do Vale, Vladimir Fazito; Aranda, Arion Tulio; Valente, Ana Carolina Dos Santos; Maia-Herzog, Marilza

    2017-01-01

    The effectiveness of the MosqTent® trap was evaluated in endemic area to onchocerciasis in Brazil. This study seeks to provide subsidies for the monitoring of the onchocerciasis transmission in the country. The study was carried out at the Homoxi and Thirei villages, located in the Yanomami Indigenous Land, in the state of Roraima. This area presents hyperendemicity, high blackflies densities, large population migrations and mining activities. The Homoxi and Thirei villages are assisted by the Brazilian Ministry of Health. To conduct the present study, the village leader, health leaders and the Brazilian Ethics Committee were consulted. Blackflies captures were carried out simultaneously at the Homoxi and Thirei, using systematized methods to allow for comparisons between the traditional Human Landing Catch (HLC) and HLC protected by the MosqTent®. The female blackflies were captured at two equidistant capture stations per locality, by two collectors per station, for five consecutive days. Individuals captured by interval/station/day were counted, identified and maintained at -20°C. The underlying probability distributions and the differences between the methods for the independent sample data were verified in a comparative statistical analysis between the use of the MosqTent® and the HLC. A total of 10,855 antropophilic blackflies were captured by both methodologies. A total of 7,367 (67.87%) blackflies belonging to seven species were captured by MosqTent® -Simulium incrustatum s.l (99.06%); S. guianense s.l (0.74%), S. oyapockense s.l (0.01%), S. exiguum (0.10%), S. metallicum (0.05%), S. ochraceum (0.03%) and S. minusculum s.l (0.01%). Moreover, 3,488 (32.14%) blackflies belonging to four species were captured by HLC-S. incrustatum s.l (98.33%); S. guianense s.l (1.38%), S. oyapockense s.l (0.26%) and S. metallicum (0.03%). The MosqTent® was more effective and efficient when compared to HLC. When comparing total blackflies captured/day, the MosqTent® was

  16. Clinical applications of HPLC-competitive protein binding assay for serum 25-hydroxyvitamin D

    International Nuclear Information System (INIS)

    Yang Shouli

    1989-01-01

    This report describes the clinical applications of HPLC-competitive protein binding assay for serum 25(OH) Vit D in 156 cases. Serum 25(OH) Vit D of normal human was 33.1 +- 14.8 nmol/L (13.2 +- 5.9 ng/ml), while for various diseases are as follows: rickets, 18.0 +- 9.0 nmol/L (7.2 +- 3.6 ng/ml, n = 36, P 0.1); pneumonia of children, 33.8 +- 14.8 nmol/L (13.5 +- 5.9 ng/ml, n = 10, P > 0.5); cirrhosis, 13.8 +- 11.3 nmol/L (5.5 +- 4.5 ng/ml, n = 9, P 0.2); administration of anticonvulsant (1 to 15 years), 19.0 +- 6.5 nmol/L (7.6 +- 2.6 ng/ml, n = 19, P 6 months), 15.3 +- 5.0 nmol/L (6.1 +- 2.0 ng/ml, n = 6, P 0.5); pregnant women, 39.8 +- 16.5 nmol/L (15.9 +- 6.6 ng/ml, n = 7, P > 0.1). We found it is a useful reference value for most of the above diseased state especially for differentiation between rickets and hypervitaminosis

  17. A systematic approach to the accurate quantification of selenium in serum selenoalbumin by HPLC-ICP-MS

    International Nuclear Information System (INIS)

    Jitaru, Petru; Goenaga-Infante, Heidi; Vaslin-Reimann, Sophie; Fisicaro, Paola

    2010-01-01

    In this paper, two different methods are for the first time systematically compared for the determination of selenium in human serum selenoalbumin (SeAlb). Firstly, SeAlb was enzymatically hydrolyzed and the resulting selenomethionine (SeMet) was quantified using species-specific isotope dilution (SSID) with reversed phase-HPLC (RP-HPLC) hyphenated to (collision/reaction cell) inductively coupled plasma-quadrupole mass spectrometry (CRC ICP-QMS). In order to assess the enzymatic hydrolysis yield, SeAlb was determined as an intact protein by affinity-HPLC (AF-HPLC) coupled to CRC ICP-QMS. Using this approach, glutathione peroxidase (GPx) and selenoprotein P (SelP) (the two selenoproteins present in serum) were also determined within the same chromatographic run. The levels of selenium associated with SeAlb in three serum materials, namely BCR-637, Seronorm level 1 and Seronorm level 2, obtained using both methods were in a good agreement. Verification of the absence of free SeMet, which interferes with the SeAlb determination (down to the amino acid level), in such materials was addressed by analyzing the fraction of GPx, partially purified by AF-HPLC, using RP-HPLC (GPx only) and size exclusion-HPLC (SE-HPLC) coupled to CRC ICP-QMS. The latter methodology was also used for the investigation of the presence of selenium species other than the selenoproteins in the (AF-HPLC) SelP and SeAlb fractions; the same selenium peaks were detected in both control and BCR-637 serum with a difference in age of ca. 12 years. It is also for the first time that the concentrations of selenium associated with SeAlb, GPx and SelP species in such commercially available serums (only certified or having indicative levels of total selenium content) are reported. Such indicative values can be used for reference purposes in future validation of speciation methods for selenium in human serum and/or inter-laboratory comparisons.

  18. A systematic approach to the accurate quantification of selenium in serum selenoalbumin by HPLC-ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Jitaru, Petru, E-mail: Petru.Jitaru@lne.fr [Laboratoire National de Metrologie et d' Essais (LNE), Department of Biomedical and Inorganic Chemistry, 1 rue Gaston Boissier, 75015 Paris (France); Goenaga-Infante, Heidi [LGC Limited, Queens Road, Teddington, TW11 OLY, Middlesex (United Kingdom); Vaslin-Reimann, Sophie; Fisicaro, Paola [Laboratoire National de Metrologie et d' Essais (LNE), Department of Biomedical and Inorganic Chemistry, 1 rue Gaston Boissier, 75015 Paris (France)

    2010-01-11

    In this paper, two different methods are for the first time systematically compared for the determination of selenium in human serum selenoalbumin (SeAlb). Firstly, SeAlb was enzymatically hydrolyzed and the resulting selenomethionine (SeMet) was quantified using species-specific isotope dilution (SSID) with reversed phase-HPLC (RP-HPLC) hyphenated to (collision/reaction cell) inductively coupled plasma-quadrupole mass spectrometry (CRC ICP-QMS). In order to assess the enzymatic hydrolysis yield, SeAlb was determined as an intact protein by affinity-HPLC (AF-HPLC) coupled to CRC ICP-QMS. Using this approach, glutathione peroxidase (GPx) and selenoprotein P (SelP) (the two selenoproteins present in serum) were also determined within the same chromatographic run. The levels of selenium associated with SeAlb in three serum materials, namely BCR-637, Seronorm level 1 and Seronorm level 2, obtained using both methods were in a good agreement. Verification of the absence of free SeMet, which interferes with the SeAlb determination (down to the amino acid level), in such materials was addressed by analyzing the fraction of GPx, partially purified by AF-HPLC, using RP-HPLC (GPx only) and size exclusion-HPLC (SE-HPLC) coupled to CRC ICP-QMS. The latter methodology was also used for the investigation of the presence of selenium species other than the selenoproteins in the (AF-HPLC) SelP and SeAlb fractions; the same selenium peaks were detected in both control and BCR-637 serum with a difference in age of ca. 12 years. It is also for the first time that the concentrations of selenium associated with SeAlb, GPx and SelP species in such commercially available serums (only certified or having indicative levels of total selenium content) are reported. Such indicative values can be used for reference purposes in future validation of speciation methods for selenium in human serum and/or inter-laboratory comparisons.

  19. Comparing the performance of flat and hierarchical Habitat/Land-Cover classification models in a NATURA 2000 site

    Science.gov (United States)

    Gavish, Yoni; O'Connell, Jerome; Marsh, Charles J.; Tarantino, Cristina; Blonda, Palma; Tomaselli, Valeria; Kunin, William E.

    2018-02-01

    The increasing need for high quality Habitat/Land-Cover (H/LC) maps has triggered considerable research into novel machine-learning based classification models. In many cases, H/LC classes follow pre-defined hierarchical classification schemes (e.g., CORINE), in which fine H/LC categories are thematically nested within more general categories. However, none of the existing machine-learning algorithms account for this pre-defined hierarchical structure. Here we introduce a novel Random Forest (RF) based application of hierarchical classification, which fits a separate local classification model in every branching point of the thematic tree, and then integrates all the different local models to a single global prediction. We applied the hierarchal RF approach in a NATURA 2000 site in Italy, using two land-cover (CORINE, FAO-LCCS) and one habitat classification scheme (EUNIS) that differ from one another in the shape of the class hierarchy. For all 3 classification schemes, both the hierarchical model and a flat model alternative provided accurate predictions, with kappa values mostly above 0.9 (despite using only 2.2-3.2% of the study area as training cells). The flat approach slightly outperformed the hierarchical models when the hierarchy was relatively simple, while the hierarchical model worked better under more complex thematic hierarchies. Most misclassifications came from habitat pairs that are thematically distant yet spectrally similar. In 2 out of 3 classification schemes, the additional constraints of the hierarchical model resulted with fewer such serious misclassifications relative to the flat model. The hierarchical model also provided valuable information on variable importance which can shed light into "black-box" based machine learning algorithms like RF. We suggest various ways by which hierarchical classification models can increase the accuracy and interpretability of H/LC classification maps.

  20. Intramolecular cyclization in irradiated nucleic acids: correlation between high-performance liquid chromatography and an immunochemical assay for 8,5'-cycloadenosine in irradiated poly(A)

    International Nuclear Information System (INIS)

    Fuciarelli, A.F.; Shum, F.Y.; Raleigh, J.A.

    1987-01-01

    A correlation between high-performance liquid chromatography (HPLC) analysis and an in situ enzyme-linked immunosorbent assay (ELISA) for 8,5'-cycloadenosine formation in irradiated poly(A) has been established. The correlation shows that the ELISA precisely reflects changes in the combined yield of R- and S-8,5'-cycloadenosine but that a correction factor must be applied to the ELISA values for accuracy. The HPLC analysis reveals that the intramolecular cyclization proceeds stereoselectively in irradiated poly(A) to preferentially produce the R isomer at pH 7.0 which is similar to the result for irradiated adenosine but in contrast to the result for 5'-AMP where the S isomer predominates at neutral pH. The HPLC analysis shows that two events originating in hydroxyl radical attack at the sugar phosphate backbone in poly(A); that is, adenine release and 8,5'-cycloadenosine formation have somewhat different dose-yield responses. The formation of 8-hydroxyadenosine was detected in the HPLC chromatograms of poly(A) irradiated under N2O at neutral pH, and the yield of this compound was similar to the yield observed in 5'-AMP or adenosine irradiated under similar conditions

  1. In vitro cytotoxic activity of medicinal plants from Nigeria ethnomedicine on Rhabdomyosarcoma cancer cell line and HPLC analysis of active extracts.

    Science.gov (United States)

    Ogbole, Omonike O; Segun, Peter A; Adeniji, Adekunle J

    2017-11-22

    Cancer is a leading cause of death world-wide, with approximately 17.5 million new cases and 8.7 million cancer related deaths in 2015. The problems of poor selectivity and severe side effects of the available anticancer drugs, have demanded the need for the development of safer and more effective chemotherapeutic agents. The present study was aimed at determining the cytotoxicities of 31 medicinal plants extracts, used in Nigerian ethnomedicine for the treatment of cancer. The plant extracts were screened for cytotoxicity, using the brine shrimp lethality assay (BSLA) and MTT cytotoxicity assay. Rhabdomyosarcoma (RD) cell line, normal Vero cell line and the normal prostate (PNT2) cell line were used for the MTT assay, while Artemia salina nauplii was used for the BSLA. The phytochemical composition of the active plant extracts was determined by high performance liquid chromatography (HPLC) analysis. The extract of Eluesine indica (L.) Gaertn (Poaceae), with a LC 50 value of 76.3 μg/mL, had the highest cytotoxicity on the brine shrimp larvae compared to cyclophosphamide (LC 50  = 101.3 μg/mL). Two plants extracts, Macaranga barteri Mull. Arg. (Euphorbiaceae) and Calliandra portoricensis (Jacq.) Benth (Leguminosae) exhibited significant cytotoxic activity against the RD cell line and had comparable lethal activity on the brine shrimps. Further cytotoxic investigation showed that the dichloromethane fraction of Macaranga barteri (DMB) and the ethyl acetate fraction of Calliandra portoricensis (ECP), exhibited approximately 6-fold and 4-fold activity, respectively, compared to cyclophosphamide on RD cell line. Determination of selective index (SI) using Vero and PNT2 cell line indicated that DMB and ECP displayed a high degree of selectivity against the cancer cell under investigation. HPLC analysis showed that 3,5dicaffeoylquinic acid, acteoside, kampferol-7-O-glucoside and bastadin 11 were the major components of DMB while the major components of ECP were

  2. HPLC quantification of phenolic content and assessment of ...

    African Journals Online (AJOL)

    omotayo

    2016-03-02

    Mar 2, 2016 ... detection (HPLC-DAD) fingerprinting of phenolic content. Furthermore, the .... Briefly, deionised water (0.5 ml) and 125 μl of Folin–Colcalteu reagent were added to ..... to be organ-specific and can leak from a damaged or an.

  3. A high-throughput method for the simultaneous determination of multiple mycotoxins in human and laboratory animal biological fluids and tissues by PLE and HPLC-MS/MS.

    Science.gov (United States)

    Cao, Xiaoqin; Wu, Shuangchan; Yue, Yuan; Wang, Shi; Wang, Yuting; Tao, Li; Tian, Hui; Xie, Jianmei; Ding, Hong

    2013-12-30

    A high-throughput method for the determination of 28 mycotoxins involving pressurised liquid extraction (PLE) coupled with liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) has been optimised and validated for determination in various biological fluids and tissues of human and laboratory animals. High-throughput analysis was achieved using PLE pre-treatment and without the need for any cleanup. The extraction solvent was acetonitrile/water/acetic acid (80/19/1, v/v/v). The static extraction time was 5min. The extraction pressure and temperature were 1500psi and 140°C, respectively. The flush volume was 60%. The limits of detection, which were defined as CCα, varied from 0.01μg/kg (μg/L) to 0.69μg/kg (μg/L). The recoveries of spiked samples from 0.20μg/kg (μg/L) to 2μg/kg (μg/L) ranged from 71% to 100.5% with relative standard deviations of less than 17.5%, except FB1 and FB2 recoveries, which were lower than 60%. The method was successfully applied in real samples, and the data indicate that this technique is a useful analytical method for the determination of mycotoxins from humans and animals. To the best of our knowledge, this method is the first for the large-scale testing of multi-class mycotoxins in all types of biological fluids and tissues that uses PLE and HPLC-MS/MS. Copyright © 2013 Elsevier B.V. All rights reserved.

  4. Whole genome sequencing of a rare rotavirus from archived stool sample demonstrates independent zoonotic origin of human G8P[14] strains in Hungary.

    Science.gov (United States)

    Marton, Szilvia; Dóró, Renáta; Fehér, Enikő; Forró, Barbara; Ihász, Katalin; Varga-Kugler, Renáta; Farkas, Szilvia L; Bányai, Krisztián

    2017-01-02

    Genotype P[14] rotaviruses in humans are thought to be zoonotic strains originating from bovine or ovine host species. Over the past 30 years only few genotype P[14] strains were identified in Hungary totalinghuman rotaviruses whose genotype had been determined. In this study we report the genome sequence and phylogenetic analysis of a human genotype G8P[14] strain, RVA/Human-wt/HUN/182-02/2001/G8P[14]. The whole genome constellation (G8-P[14]-I2-R2-C2-M2-A11-N2-T6-E2-H3) of this strain was shared with another Hungarian zoonotic G8P[14] strain, RVA/Human-wt/HUN/BP1062/2004/G8P[14], although phylogenetic analyses revealed the two rotaviruses likely had different progenitors. Overall, our findings indicate that human G8P[14] rotavirus detected in Hungary in the past originated from independent zoonotic events. Further studies are needed to assess the public health risk associated with infections by various animal rotavirus strains. Copyright © 2016. Published by Elsevier B.V.

  5. [Simultaneous Determination of Three Kinds of Effective Constituents in Cannabis Plants by Reversed-phase HPLC].

    Science.gov (United States)

    Fu, Q; Shu, Z; Deng, K; Luo, X; Zeng, C G

    2016-08-01

    To establish a high performance liquid chromatographic (HPLC) method for simultaneous determination of three effective constituents, including tetrahydrocannabinol (THC), cannabidiol (CBD) and cannabinol (CBN) in Cannabis plants. A C₁₈ column was used in this study, and acetonitrile-phosphate buffer (0.015 mol/L KH₂PO₄) was used as mobile phase at a flow rate of 1.0 mL/min. At a detection wavelength of 220 mm, UV absorption spectra were collected at the wavelength range of 190-400 nm, and the spectra and retention time were counted as qualitative evidence. THC, CBD and CBN could be well separated by this method. Three components had good linear relationship in the range of 0.4-40 μg/mL ( R ²≥0.999 3). The recoveries were over 87%. The limits of detection were 1.8 ng, 2.0 ng and 1.3 ng, respectively. The relative standard deviation (RSD) were less than 5% for both inter-day and intra-day precisions. Reversed-phase HPLC method is simple, rapid and accurate, and it is suitable for the qualitative and quantitative detection of THC, CBD and CBN in Cannabis plants. Copyright© by the Editorial Department of Journal of Forensic Medicine

  6. Correlation of levels of alpha-defensins determined by HPLC-ESI-MS in bronchoalveolar lavage fluid with the diagnosis of pneumonia in premature neonates.

    Science.gov (United States)

    Tirone, Chiara; Boccacci, Simona; Inzitari, Rosanna; Tana, Milena; Aurilia, Claudia; Fanali, Chiara; Cabras, Tiziana; Messana, Irene; Castagnola, Massimo; Romagnoli, Costantino; Vento, Giovanni

    2010-08-01

    The presence of alpha-defensins in bronchoalveolar lavage fluid (BALF) was investigated in a cohort of preterm newborns with gestational age (GA) groups: pneumonia group of nine neonates suffering from pulmonary infection (GA: 26.1 +/- 2.1 wk; birth weight: 787.4 +/- 309.9 g), with or without associated bloodstream infection, and nonpneumonia group of 15 neonates (GA: 27.7 +/- 2.0 wk; birth weight: 1019.0 +/- 319.8 g). BALF culture was positive for CONS (n = 5), Staphylococcus aureus (n = 1), and Candida spp (n = 3). BALF samples were analyzed by HPLC-electrospray Ionization-mass spectrometer. The alpha-defensins 1-4 concentration, absolute and differential white cells count were measured. Relative amounts of alpha-defensins 1-4 and the absolute number of neutrophils were found significantly higher in the pneumonia group with respect to the nonpneumonia group (p < 0.05). Moreover, positive significant correlations between the number of neutrophils and the alpha-defensins 1-3 levels were observed. In conclusion, our data show that preterm newborns, also at the lower GA, are able to produce alpha-defensins, underlining that their innate defense system is already active before the at-term delivery date.

  7. Spinal Stiffness in Prone and Upright Postures During 0-1.8 g Induced by Parabolic Flight.

    Science.gov (United States)

    Swanenburg, Jaap; Meier, Michael L; Langenfeld, Anke; Schweinhardt, Petra; Humphreys, B Kim

    2018-06-01

    The purpose of this study was to analyze posterior-to-anterior spinal stiffness in Earth, hyper-, and microgravity conditions during both prone and upright postures. During parabolic flight, the spinal stiffness of the L3 vertebra of a healthy 37-yr-old man was measured in normal Earth gravity (1.0 g), hypergravity (1.8 g), and microgravity (0.0 g) conditions induced in the prone and upright positions. Differences in spinal stiffness were significant across all three gravity conditions in the prone and upright positions. Most effect sizes were large; however, in the upright posture, the effect size between Earth gravity and microgravity was medium. Significant differences in spinal stiffness between the prone and upright positions were found during Earth gravity and hypergravity conditions. No difference was found between the two postures during microgravity conditions. Based on repeated measurements of a single individual, our results showed detectable changes in posterior-to-anterior spinal stiffness. Spinal stiffness increased during microgravity and decreased during hypergravity conditions. In microgravity conditions, posture did not impact spinal stiffness. More data on spinal stiffness in variable gravitational conditions is needed to confirm these results.Swanenburg J, Meier ML, Langenfeld A, Schweinhardt P, Humphreys BK. Spinal stiffness in prone and upright postures during 0-1.8 g induced by parabolic flight. Aerosp Med Hum Perform. 2018; 89(6):563-567.

  8. Carotenoid composition of jackfruit (Artocarpus heterophyllus), determined by HPLC-PDA-MS/MS.

    Science.gov (United States)

    de Faria, A F; de Rosso, V V; Mercadante, A Z

    2009-06-01

    Carotenoids are pigments responsible for the yellow-reddish color of many foods and are related to important functions and physiological actions, preventing several chronic-degenerative diseases. The objective of this study was to confirm the carotenoid composition of jackfruit by high-performance liquid chromatography connected to photodiode array and mass spectrometry detectors (HPLC-PDA-MS/MS). The main carotenoids were all-trans-lutein (24-44%), all-trans-beta-carotene (24-30%), all-trans-neoxanthin (4-19%), 9-cis-neoxanthin (4-9%) and 9-cis-violaxanthin (4-10%). Either qualitative or quantitative differences, mainly related to the lutein proportion, were found among three batches of jackfruit. Since the fruits from batch A showed significantly lower contents for almost all carotenoids, it also had the lowest total carotenoid content (34.1 microg/100 g) and provitamin A value, whereas the total carotenoid ranged from 129.0 to 150.3 microg/100 g in the other batches. The provitamin A values from batches B and C were 3.3 and 4.3 microg RAE/100 g, respectively. The carotenoid composition of jackfruit was successfully determined, where 14 of the 18 identified carotenoids were reported for first time. Differences among batches may be due to genetic and/or agricultural factors.

  9. The Determination of Food Dyes in Vitamins by RP-HPLC

    Directory of Open Access Journals (Sweden)

    Monika Šuleková

    2016-10-01

    Full Text Available Reversed-phase high performance liquid chromatography (RP-HPLC for the determination of five synthetic food dyes (Quinoline Yellow E104, Sunset Yellow E110, Ponceau 4R E124, Tartrazine E102 and Carmine E120 in vitamins was used. The dyes were analyzed within 10 min using a column with stationary phase C 18 (250 mm × 4.6 mm, 5 μm at 40 °C with isocratic elution, and the mobile phase contained acetonitrile and a mixture of CH3COONa:CH3OH (85:15, v/v in a ratio of 10:90 (v/v for yellow-colored capsules and 20:80 (v/v for red-colored capsules, respectively. A diode-array detector was used to monitor the dyes between 190 and 800 nm. It was established that the analyzed samples contained synthetic dyes in a concentration range from 79.5 ± 0.01 μg/capsule of Ponceau 4R, E124 to 524 ± 0.01 μg/capsule of Tartrazine, E102. The obtained results were compared with existing acceptable daily intakes (ADIs for individual dyes. This paper provides information about the content of dyes in samples of vitamins. This information is not generally available to consumers.

  10. Simultaneous HPLC quantitative analysis of mangostin derivatives in Tetragonula pagdeni propolis extracts

    Directory of Open Access Journals (Sweden)

    Sumet Kongkiatpaiboon

    2016-04-01

    Full Text Available Propolis has been used as indigenous medicine for curing numerous maladies. The one that is of ethnopharmacological use is stingless bee propolis from Tetragonula pagdeni. A simultaneous high-performance liquid chromatography (HPLC investigation was developed and validated to determine the contents of bioactive compounds: 3-isomangostin, gamma-mangostin, beta-mangostin, and alpha-mangostin. HPLC analysis was effectively performed using a Hypersil BDS C18 column, with the gradient elution of methanol–0.2% formic acid and a flow rate of 1 ml/min, at 25 °C and detected at 245 nm. Parameters for the validation included accuracy, precision, linearity, and limits of quantitation and detection. The developed HPLC technique was precise, with lower than 2% relative standard deviation. The recovery values of 3-isomangostin, gamma-mangostin, beta-mangostin, and alpha-mangostin in the extracts were 99.98%, 99.97%, 98.98% and 99.19%, respectively. The average contents of these mixtures in the propolis extracts collected from different seasons were 0.127%, 1.008%, 0.323% and 2.703% (w/w, respectively. The developed HPLC technique was suitable and practical for the simultaneous analysis of these mangostin derivatives in T. pagdeni propolis and would be a valuable guidance for the standardization of its pharmaceutical products.

  11. Brief on -Hyphenated Methods of HPLC for Determining the Presence of Solutes.

    Directory of Open Access Journals (Sweden)

    Mohamad Taleuzzaman

    2017-02-01

    Full Text Available HPLC is the tool in liquid chromatography is unique because of particle size, smaller particle in the stationary phase, increase efficiency of a separation. However, if the particles are made smaller, capillary action increases and it becomes more difficult to drain the column under gravity. For quantitative analysis different types of detector is used in conjunction with HPLC which give precise and accurate result and it is apply according to the nature of the substance. Various types of detectors used in HPLC are mass spectrometry, infrared spectroscopy, visible spectroscopy, ultraviolet spectroscopy, fluorescence spectroscopy, nuclear magnetic resonance, conductivity measurement, and refractive index measurement. Each detector has its assets, limitations and sample types for which it is most effective. The recent development of the so-called hyphenated techniques has improved the ability to separate and identify multiple entities within a mixture.

  12. New approaches to detect 8-hydroxyguanine in γ-irradiated cellular DNA

    International Nuclear Information System (INIS)

    Mei, Nan; Tamae, Kazuyoshi; Hirano, Takeshi; Kasai, Hiroshi; Kunugita, Naoki

    2003-01-01

    This report describes an assay to detect 8-hydroxydeoxyguanosine 5'-monophosphate (8-OH-dGMP) in cellular DNA by modification of enzyme treatment after DNA extraction, using a high-performance liquid chromatography system equipped with an electrochemical detector (HPLC-ECD). This modification greatly reduces the measured background level of 8-hydroxyguanine (8-OH-Gua) in DNA, and improves the HPLC-ECD sensitivity to measure oxidative DNA damage. The 8-OH-Gua value in the DNA was expressed by the ratio of 8-OH-dGMP to deoxycytidine 5'-monophosphate (dCMP). Background level of 8-OH-Gua in DNA under our conditions was several times lower than that by a previous method. The human lung carcinoma cells (A549) were exposed to γ-rays of 20-100 Gy. A dose-dependent increase in oxidative DNA damage of 8-OH-Gua was observed. Furthermore, using commercial FITC-kit of an immunohistochemical type procedure, 8-OH-Gua was clearly detected in A549 cells and the fluorescence intensity of cells with oxidative DNA damage increased with the doses of γ-irradiation. Using an 8-OH-Gua repair activity assay, we also found that γ-rays decreased the repair enzyme activity. We conclude that the 8-OH-Gua level in human cellular DNA increases partly by the generation of reactive oxygen species (ROS) and partly by the inhibition of repair activity for 8-OH-Gua. (author)

  13. Quantitative HPLC determination of [99mTc]-pertechnetate in radiopharmaceuticals and biological samples: Pt. 1

    International Nuclear Information System (INIS)

    Tianze Zhou; Hirth, W.W.; Heineman, W.R.; Deutsch, Edward

    1988-01-01

    Techniques have been developed which allow HPLC (high performance liquid chromatography) to be used for the quantitative determination of [ 99m Tc]pertechnetate in radiopharmaceuticals and biological samples. An instrumental technique accounts for 99m Tc species which do not elute from the HPLC column, while a chemical technique obviates interferences caused by Sn(II). These two techniques are incorporated into an anion exchange HPLC procedure which is applied to the determination of [ 99m Tc]pertechnetate in 99m Tc-diphosphonate radiopharmaceuticals and biological samples. (author)

  14. Detection in Japan of an equine-like G3P[8] reassortant rotavirus A strain that is highly homologous to European strains across all genome segments.

    Science.gov (United States)

    Kikuchi, Wakako; Nakagomi, Toyoko; Gauchan, Punita; Agbemabiese, Chantal Ama; Noguchi, Atsuko; Nakagomi, Osamu; Takahashi, Tsutomu

    2018-03-01

    Equine-like G3P[8] rotavirus A strains with DS-1-like backbone genes have emerged since 2013. An equine-like RVA/Human-wt/JPN/15R429/2015/G3P[8] strain possessing I2-R2-C2-M2-A2-N2-T2-E2-H2 was detected in Japan in 2015. Its VP7 gene was ≥ 99.3% identical to those of equine-like G3P[4] strains detected in Japan, and the remaining 10 genes were 98.6-99.8% identical to G1P[8] double-gene reassortants detected in Japan, Thailand and the Philippines. Thus, 15R429 was likely generated through reassortment between the equine-like G3P[4] and G1P[8] reassortant strains. Notably, 15R429 was 98.5-99.8% identical across all 11 genes of the equine-like G3P[8] strains detected in Spain and Hungary in 2015.

  15. TOXICOLOGICAL DRUG SCREENING BY GC-MS VERSUS HPLC-DAD USING A COMMON EFFICIENT EXTRACTION PROCEDURE SCREENING TOXICOLOGIQUE DES MEDICAMENTS PAR HPLC-DAD ET GC-MS: PROTOCOLE D’EXTRACTION UNIQUE

    Directory of Open Access Journals (Sweden)

    SELOUA ELMRABEH

    2015-05-01

    Full Text Available This paper presents a common extraction method for toxicological drug screening by gas chromatography-mass spectrometry (GC-MS and high-performance liquid chromatography with diode-array detection (HPLC-DAD. Liquid-liquid extraction was performed using plasma of 104 samples at the Laboratory of Moroccan Poison Control and Pharmacovigilance Center during a period of 12 months. The results obtained by HPLC-DAD are compared with those determined with GC-MS. 76 cases (73.08 % were found positive for at least by one of these two techniques. HPLC-DAD identified 59.87 % of all positive results, and 10 molecules were identified only by HPLC-DAD. GC/MS identified 40.13 % of all positives, and 4 molecules were identified only by GC/MS. In order to evaluate the performance of this extraction method, an extraction yield was calculated for three classes of drugs. All the analyzed molecules were obtained in satisfactory yields (higher than 50 % except for carbamazepine, amitriptyline and nortriptyline. Overall, the results indicate that the extraction method is well adapted for toxicological drug screening. The use of common extraction simultaneously for the two techniques can reduce workload and costs of screening, while increasing the validity and reliability of the results.

  16. Principles of Developing Multi-Pesticide Methods Based on HPLC Determination

    Energy Technology Data Exchange (ETDEWEB)

    Dudar, E. [Plant Protection & Soil Conservation Service of Budapest, Budapest (Hungary)

    2009-07-15

    Principles for the development of multi-pesticide methods based on HPLC determination are outlined. Flow charts and block diagrams give guidance on how to proceed stepwise in the set-up of respective analytical methods. Detailed information is provided on what to take into consideration for setting up a pesticide formulation analysis method. HPLC variables like the types of column, solvents and their strength, pH value, eluent modifiers, column temperature, etc, and the influence on the separation and resolution of chromatographic peaks are discussed as well as the necessity and benefits of internal standardization. Examples of system suitability testing experiments are given for illustration. (author)

  17. Comparison of a point-of-care analyser for the determination of HbA1c with HPLC method.

    Science.gov (United States)

    Grant, D A; Dunseath, G J; Churm, R; Luzio, S D

    2017-08-01

    As the use of Point of Care Testing (POCT) devices for measurement of glycated haemoglobin (HbA1c) increases, it is imperative to determine how their performance compares to laboratory methods. This study compared the performance of the automated Quo-Test POCT device (EKF Diagnostics), which uses boronate fluorescence quenching technology, with a laboratory based High Performance Liquid Chromatography (HPLC) method (Biorad D10) for measurement of HbA1c. Whole blood EDTA samples from subjects (n=100) with and without diabetes were assayed using a BioRad D10 and a Quo-Test analyser. Intra-assay variation was determined by measuring six HbA1c samples in triplicate and inter-assay variation was determined by assaying four samples on 4 days. Stability was determined by assaying three samples stored at -20 °C for 14 and 28 days post collection. Median (IQR) HbA1c was 60 (44.0-71.2) mmol/mol (7.6 (6.17-8.66) %) and 62 (45.0-69.0) mmol/mol (7.8 (6.27-8.46) %) for D10 and Quo-Test, respectively, with very good agreement (R 2 =0.969, Pglucose intolerance (IGT and T2DM) and 100% for diagnosis of T2DM. Good agreement between the D10 and Quo-Test was seen across a wide HbA1c range. The Quo-Test POCT device provided similar performance to a laboratory based HPLC method.

  18. Semi-preparative HPLC preparation and HPTLC quantification of tetrahydroamentoflavone as marker in Semecarpus anacardium and its polyherbal formulations.

    Science.gov (United States)

    Aravind, S G; Arimboor, Ranjith; Rangan, Meena; Madhavan, Soumya N; Arumughan, C

    2008-11-04

    Application of modern scientific knowledge coupled with sensitive analytical technique is important for the quality evaluation and standardization of polyherbal formulations. Semecarpus anacardium, an important medicinal plant with wide medicinal properties, is frequently used in a large number of traditional herbal preparations. Tetrahydroamentoflavone (THA), a major bioactive biflavonoid was selected as a chemical marker of S. anacardium and RP-semi-preparative HPLC conditions were optimized for the isolation of tetrahydroamentoflavone. HPTLC analytical method was developed for the fingerprinting of S. anacardium flavonoids and quantification of tetrahydroamentoflavone. The method was validated in terms of their linearity, LOD, LOQ, precision and accuracy and compared with RP-HPLC-DAD method. The methods were demonstrated for the chemical fingerprinting of S. anacardium plant parts and some commercial polyherbal formulations and the amount of tetrahydroamentoflavone was quantified. HPTLC analysis showed that S. anacardium seed contained approximately 10 g kg(-1) of tetrahydroamentoflavone. The methods were able to identify and quantify tetrahydroamentoflavone from complex mixtures of phytochemicals and could be extended to the marker-based standardization of polyherbal formulations, containing S. anacardium.

  19. New Stability Indicating RP-HPLC Method for the Estimation of Cefpirome Sulphate in Bulk and Pharmaceutical Dosage Forms.

    Science.gov (United States)

    Rao, Kareti Srinivasa; Kumar, Keshar Nargesh; Joydeep, Datta

    2011-01-01

    A simple stability indicating reversed-phase HPLC method was developed and subsequently validated for estimation of Cefpirome sulphate (CPS) present in pharmaceutical dosage forms. The proposed RP-HPLC method utilizes a LiChroCART-Lichrosphere100, C18 RP column (250 mm × 4mm × 5 μm) in an isocratic separation mode with mobile phase consisting of methanol and water in the proportion of 50:50 % (v/v), at a flow rate 1ml/min, and the effluent was monitored at 270 nm. The retention time of CPS was 2.733 min and its formulation was exposed to acidic, alkaline, photolytic, thermal and oxidative stress conditions, and the stressed samples were analyzed by the proposed method. The described method was linear over a range of 0.5-200μg/ml. The percentage recovery was 99.46. F-test and t-test at 95% confidence level were used to check the intermediate precision data obtained under different experimental setups; the calculated value was found to be less than the critical value.

  20. HPLC-DAD-ESI/MS(n) analysis of phenolic compounds for quality control of Grindelia robusta Nutt. and bioactivities.

    Science.gov (United States)

    Ferreres, Federico; Grosso, Clara; Gil-Izquierdo, Angel; Valentão, Patrícia; Azevedo, Carolina; Andrade, Paula B

    2014-06-01

    The phenolic composition of herbal tea (HT) and hydromethanolic extract (HME) obtained from Grindelia robusta Nutt. was studied by HPLC-DAD-ESI/MS(n). Thirty six flavonoids and hydroxycinnamic acids were detected, from which thirty are described for the first time in this species. Quantification by HPLC-DAD showed that diosmetin-7-O-glucuronide-3'-O-pentoside+apigenin-7-O-glucuronide-4'-O-pentoside, apigenin-7-O-glucuronide+diosmetin-7-O-glucuronide and 3,5-dicaffeoylquinic acid+3,4-dicaffeoylquinic acid were the major compounds. Since the health-promoting effects of natural phenolic compounds against brain disorders is of increasing interest, HT and HME were also tested against oxygen and nitrogen reactive species and against enzymes related with Alzheimer's disease and depression. Extracts displayed strong in vitro scavenging activity and monoamine oxidase-A (MAO-A) inhibitory activity. The anti-MAO-A capacity was observed at non-toxic concentrations for SH-SY5Y human neuroblastoma cell line, reinforcing the benefits of G. robusta HT. However, no protection against hydrogen peroxide treatment was observed. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. Development of Isocratic RP-HPLC Method for Separation and Quantification of L-Citrulline and L-Arginine in Watermelons

    Directory of Open Access Journals (Sweden)

    Rasdin Ridwan

    2018-01-01

    Full Text Available Watermelons (Citrullus lanatus are known to have sufficient amino acid content. In this study, watermelons grown and consumed in Malaysia were investigated for their amino acid content, L-citrulline and L-arginine, by the isocratic RP-HPLC method. Flesh and rind watermelons were juiced, and freeze-dried samples were used for separation and quantification of L-citrulline and L-arginine. Three different mobile phases, 0.7% H3P04, 0.1% H3P04, and 0.7% H3P04 : ACN (90 : 10, were tested on two different columns using Zorbax Eclipse XDB-C18 and Gemini C18 with a flow rate of 0.5 mL/min and a detection wavelength at 195 nm. Efficient separation with reproducible resolution of L-citrulline and L-arginine was achieved using 0.1% H3P04 on the Gemini C18 column. The method was validated and good linearity of L-citrulline and L-arginine was obtained with R2 = 0.9956, y=0.1664x+2.4142 and R2=0.9912, y=0.4100x+3.4850, respectively. L-citrulline content showed the highest concentration in red watermelon of flesh and rind juice extract (43.81 mg/g and 45.02 mg/g, whereas L-arginine concentration was lower than L-citrulline, ranging from 3.39 to 11.14 mg/g. The isocratic RP-HPLC method with 0.1% H3P04 on the Gemini C18 column proved to be efficient for separation and quantification of L-citrulline and L-arginine in watermelons.

  2. A Simple and Specific Stability- Indicating RP-HPLC Method for Routine Assay of Adefovir Dipivoxil in Bulk and Tablet Dosage Form.

    Science.gov (United States)

    Darsazan, Bahar; Shafaati, Alireza; Mortazavi, Seyed Alireza; Zarghi, Afshin

    2017-01-01

    A simple and reliable stability-indicating RP-HPLC method was developed and validated for analysis of adefovir dipivoxil (ADV).The chromatographic separation was performed on a C 18 column using a mixture of acetonitrile-citrate buffer (10 mM at pH 5.2) 36:64 (%v/v) as mobile phase, at a flow rate of 1.5 mL/min. Detection was carried out at 260 nm and a sharp peak was obtained for ADV at a retention time of 5.8 ± 0.01 min. No interferences were observed from its stress degradation products. The method was validated according to the international guidelines. Linear regression analysis of data for the calibration plot showed a linear relationship between peak area and concentration over the range of 0.5-16 μg/mL; the regression coefficient was 0.9999and the linear regression equation was y = 24844x-2941.3. The detection (LOD) and quantification (LOQ) limits were 0.12 and 0.35 μg/mL, respectively. The results proved the method was fast (analysis time less than 7 min), precise, reproducible, and accurate for analysis of ADV over a wide range of concentration. The proposed specific method was used for routine quantification of ADV in pharmaceutical bulk and a tablet dosage form.

  3. RP-HPLC Determination of Three Anti-Hyperlipidemic Drugs in Spiked Human Plasma and in Dosage Forms

    Directory of Open Access Journals (Sweden)

    Ola. M. Abdallah

    2011-01-01

    Full Text Available Sensitive, simple and accurate high performance liquid chromatographic (HPLC methods for the determination of atorvastatin (AT, fluvastatin (FL and pravastatin (PV have been developed. The proposed methods involve the use of a 150 mmx4.6 mm Zorbax Extend-C18 column (5 μm particle size and different chromatographic conditions for the separation of the three statins. Linearity range was 5-40, 5-30 and 10-60 μg mL-1 for AT, FL and PV respectively. The developed methods proved to be successful in the determination of all studied drugs in spiked human plasma samples.

  4. Validated RP-HPLC Method for Quantification of Phenolic ...

    African Journals Online (AJOL)

    Purpose: To evaluate the total phenolic content and antioxidant potential of the methanol extracts of aerial parts and roots of Thymus sipyleus Boiss and also to determine some phenolic compounds using a newly developed and validated reversed phase high performance liquid chromatography (RP-HPLC) method.

  5. Determination of sulfonamides and trimethoprim using high temperature HPLC with simultaneous temperature and solvent gradient.

    Science.gov (United States)

    Giegold, Sascha; Teutenberg, Thorsten; Tuerk, Jochen; Kiffmeyer, Thekla; Wenclawiak, Bernd

    2008-10-01

    A fast HPLC method for the analysis of eight selected sulfonamides (SA) and trimethoprim has been developed with the use of high temperature HPLC. The separation could be achieved in less than 1.5 min on a 50 mm sub 2 microm column with simultaneous solvent and temperature gradient programming. Due to the lower viscosity of the mobile phase and the increased mass transfer at higher temperatures, the separation could be performed on a conventional HPLC system obtaining peak widths at half height between 0.6 and 1.3 s.

  6. Simultaneous quantification by HPLC of the phenolic compounds for the crude drug of Prunus serotina subsp. capuli.

    Science.gov (United States)

    Rivero-Cruz, Blanca

    2014-08-01

    Prunus serotina Ehrenb. subsp. capuli (Cav.) McVaugh (Rosaceae), commonly known as "capulin", is a native North American tree, commercialized and used in folk medicine for the treatment of the hypertension, gastrointestinal illnesses, and cough. This work developed a suitable HPLC method for quantifying the major active constituents of the infusion of P. serotina, the most important preparation consumed by populations around the world. The analytical method was performed using a Fortis-RP column (150 mm × 4.6 mm; film thickness 5 µm). The mobile phase consisted of an isocratic acetate buffer solution (pH 2.7; A) and methanol (B) (65:35 v/v) at a flow rate of 1.0 mL min(-1). The proposed method was applied to the quantification of 1-3 in several samples of the leaves of P. serotina. The results indicated that amounts of 1-3 in the samples analyzed are uniform, and greater amounts of chlorogenic acid (2; 479.9 ± 33.6 µg g(-1), dry matter) along with hyperoside (1; 185.7 ± 55.3 µg g(-1), dry matter) were present. On the other hand, benzaldehyde (3; 118.2 ± 12.1 µg g(-1) dry matter) was found to be in lower concentration. A simple, sensitive, precise, and reproducible HPLC method for the simultaneous quantification of 1-3 in P. serotina was developed and validated. This is the first report on the quantification of 1-3 as active principles, and compound 1 was selected as a marker of P. serotina, which could be useful to guarantee the quality of the crude drug and herbal products.

  7. One-pot synthesis of zeolitic imidazolate framework-8/poly (methyl methacrylate-ethyleneglycol dimethacrylate) monolith coating for stir bar sorptive extraction of phytohormones from fruit samples followed by high performance liquid chromatography-ultraviolet detection.

    Science.gov (United States)

    You, Linna; He, Man; Chen, Beibei; Hu, Bin

    2017-11-17

    In this work, zeolitic imidazolate framework-8 (ZIF-8)/poly (methyl methacrylate-ethyleneglycol dimethacrylate) (MMA-EGDMA) composite monolith was in situ synthesized on stir bar by one-pot polymerization. Compared with the neat monolith, ZIF-8/poly(MMA-EGDMA) composite monolith has larger surface area and pore volume. It also exhibits higher extraction efficiency for target phytohormones than poly(MMA-EGDMA) monolith and commercial polyethylene glycol (PEG) coated stir bar. Based on it, a method of ZIF-8/poly(MMA-EGDMA) monolith coated stir bar sorptive extraction (SBSE)-high performance liquid chromatography-ultraviolet detection (HPLC-UV) was established for the analysis of five phytohormones in apple and pear samples. The developed method exhibited low limits of detection (0.11-0.51μg/L), wide linear range (0.5-500μg/L) and good recoveries (82.7-111%), which demonstrated good application potential of the ZIF-8/monolith coated stir bar in trace analysis of organic compounds. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Quality control of radiopharmaceuticals with HPLC using aqueous size exclusion spherogel column

    International Nuclear Information System (INIS)

    Vallabhajosula, S.; Goldsmith, S.J.; Lipszyc, H.

    1982-01-01

    The application of HPLC for the analysis and quality control of 99 Tc-radiopharmaceuticals, using a weakly basic anion exchange column, has been reported. This HPLC method for the separation of the components is based on molecular size. 99 Tc-MDP, 99 Tc-HDP and 99 Tc-DTPA were analysed and UV absorption studies carried out on the components. Components of the 99 Tc-MDP separation were injected into rabbits and renal excretion and serial images studied. (U.K.)

  9. HPLC Analysis of nine corticosteroids in “natural creams” for atopic eczema

    OpenAIRE

    Ameti, Agim; Poposka, Zaklina; Memeti, Shaban; Shishovska, Maja; Mustafa, Zana; Starkoska, Katerina; Arsova-Sarafinovska, Zorica

    2013-01-01

    Purpose: The aim of the study was to determine whether “natural creams” sold for treatment of childhood atopic eczema illegally contain corticosteroids with a newly developed rapid and simple HPLC analysis with UV detection. Material and Methods: HPLC analysis was performed using a Schimadzu LC-2010 chromatographic system (Schimadzu, Kyoto, Japan) consisting of a LC-20AT Prominence liquid chromatography pump with DGU-20A5 Prominence degasser, a SPD-M20A Prominence Diode Array Detector, and...

  10. RP-HPLC Determination of Atomoxetine Hydrochloride in Bulk and Pharmaceutical Formulations

    Directory of Open Access Journals (Sweden)

    H. R. Prajapati

    2011-01-01

    Full Text Available A reversed phase high performance liquid chromatographic (RP–HPLC method was developed and subsequently validated for the determination of atomoxetine hydrochloride in bulk and pharmaceutical formulation. The separation was done by a PerkinElmer Brownlee analytical C8 column (260 mm x 4.6 mm, 5 µm using methanol: 50 mM KH2PO2 buffer (PH adjusted to 6.8 with 0.1 M NaOH, 80:20 v/v as an eluent. UV detection was performed at 270 nm at a flow rate 1.0 mL/min. The validation of the method was performed, and specificity, reproducibility, precision accuracy and ruggedness were confirmed. The correlation coefficient was found to be 0.997 for atomoxetine hydrochloride. The recovery was in the range of 99.94 to 100.98% and limit of quantification was found to be 5.707 µg/mL. The method is simple, rapid, selective and economical too and can be used for the routine analysis of drug in pharmaceutical formulations.

  11. Carbon-14-labeled 2,3,7,8- and 1,2,7,8-tetrachlorodibenzofuran

    International Nuclear Information System (INIS)

    Gray, A.P.; McClellan, W.J.; Dipinto, V.M.

    1981-01-01

    Both 2,3,7,8- and 1,2,7,8- tetrachlorodibenzofuran -U 14 C, specific activity 57 mCi/mmol, have been obtained in low yield but at > 98% purity via Pschorr cyclization of o-phenoxyaniline -U 14 C, chlorination of the resultant dibenzofuran and separation of the tetrachloro isomers by hplc. The lower yields obtained in the Pschorr cyclization of 'hot' o-phenoxyaniline in comparison with the 'cold' material are postulated to result from enhanced homolytic relative to heterolytic cleavage of the 'hot' diazonium ion leading to a 'hot' free radical which polymerizes. The completely anomalous results observed in the attempted palladium acetate-mediated cyclization of diphenyl ether- U 14 C are likewise interpreted in terms of the intervention of a 'hot' free radical. (author)

  12. Molecular epidemiology and genetic evolution of the whole genome of G3P[8] human rotavirus in Wuhan, China, from 2000 through 2013.

    Directory of Open Access Journals (Sweden)

    Yuan-Hong Wang

    Full Text Available Rotaviruses are a major etiologic agent of gastroenteritis in infants and young children worldwide. Since the latter of the 1990s, G3 human rotaviruses referred to as "new variant G3" have emerged and spread in China, being a dominant genotype until 2010, although their genomic evolution has not yet been well investigated.The complete genomes of 33 G3P[8] human rotavirus strains detected in Wuhan, China, from 2000 through 2013 were analyzed. Phylogenetic trees of concatenated sequences of all the RNA segments and individual genes were constructed together with published rotavirus sequences.Genotypes of 11 gene segments of all the 33 strains were assigned to G3-P[8]-I1-R1-C1-M1-A1-N1-T1-E1-H1, belonging to Wa genogroup. Phylogenetic analysis of the concatenated full genome sequences indicated that all the modern G3P[8] strains were assigned to Cluster 2 containing only one clade of G3P[8] strains in the US detected in the 1970s, which was distinct from Cluster 1 comprising most of old G3P[8] strains. While main lineages of all the 11 gene segments persisted during the study period, different lineages appeared occasionally in RNA segments encoding VP1, VP4, VP6, and NSP1-NSP5, exhibiting various allele constellations. In contrast, only a single lineage was detected for VP7, VP2, and VP3 genes. Remarkable lineage shift was observed for NSP1 gene; lineage A1-2 emerged in 2007 and became dominant in 2008-2009 epidemic season, while lineage A1-1 persisted throughout the study period.Chinese G3P[8] rotavirus strains have evolved since 2000 by intra-genogroup reassortment with co-circulating strains, accumulating more reassorted genes over the years. This is the first large-scale whole genome-based study to assess the long-term evolution of common human rotaviruses (G3P[8] in an Asian country.

  13. [Studies on fingerprinting of Flos Buddleja by RP-HPLC].

    Science.gov (United States)

    Han, Peng; Cui, Ya-jun; Guo, Hong-zhu; Guo, De-an

    2004-10-01

    To establish fingerprinting of Flos Buddleja by using RP-HPLC for the quality control. The HPLC condition was as follows: Inertsil ODS-3 C18 analytical column (4.6 mm x 250 mm, 5 microm), gredient eluation with MeCN (0.1% TFA)-H2O (0.1%TFA), flow rate 1.0 mL x min(-1), detection wavelength 254 nm. 10 commercial samples were analyzed to establish a fingerprinting. Among the obtained fingerprinting, most of the detected peaks were separated effectively. The accuracy, repeatability and stability of this method were satisfied. The RSDs of relative retention time and area of aimed peaks which existed in all samples wereless than 5%. Theresults were in accordance with the request of fingerprinting. The established fingerprinting can be used for the quality control of Flos Buddleja.

  14. α-Glucosidase inhibition and antioxidant activity of an oenological commercial tannin. Extraction, fractionation and analysis by HPLC/ESI-MS/MS and (1)H NMR.

    Science.gov (United States)

    Muccilli, Vera; Cardullo, Nunzio; Spatafora, Carmela; Cunsolo, Vincenzo; Tringali, Corrado

    2017-01-15

    Two batches of the oenological tannin Tan'Activ R, (toasted oak wood - Quercus robur), were extracted with ethanol. A fractionation on XAD-16 afforded four fractions for each extract. Extracts and fractions were evaluated for antioxidant activity (DPPH), polyphenol content (GAE) and yeast α-glucosidase inhibitory activity. Comparable results were obtained for both columns, fractions X1B and X2B showing the highest antioxidant activity. Fractions X1C and X2C notably inhibited α-glucosidase, with IC50=9.89 and 8.05μg/mL, respectively. Fractions were subjected to HPLC/ESI-MS/MS and (1)H NMR analysis. The main phenolic constituents of both X1B and X2B were a monogalloylglucose isomer (1), a HHDP-glucose isomer (2), castalin (3) gallic acid (4), vescalagin (5), and grandinin (or its isomer roburin E, 6). X1C and X2C showed a complex composition, including non-phenolic constituents. Fractionation of X2C gave a subfraction, with enhanced α-glucosidase inhibitory activity (IC50=6.15μg/mL), with castalagin (7) as the main constituent. Copyright © 2016 Elsevier Ltd. All rights reserved.

  15. Development and Validation of HPLC-PDA Assay method of Frangula emodin

    Directory of Open Access Journals (Sweden)

    Deborah Duca

    2016-03-01

    Full Text Available Frangula emodin, (1,3,8-trihydroxy-6-methyl-anthraquinone, is one of the anthraquinone derivatives found abundantly in the roots and bark of a number of plant families traditionally used to treat constipation and haemorrhoids. The present study describes the development and subsequent validation of a specific Assay HPLC method for emodin. The separation was achieved on a Waters Symmetry C18, 4.6 × 250 mm, 5 μm particle size, column at a temperature of 35 °C, with UV detection at 287 and 436 nm. An isocratic elution mode consisting of 0.1% formic acid and 0.01% trifluoroacetic acid as the aqueous mobile phase, and methanol was used. The method was successfully and statistically validated for linearity, range, precision, accuracy, specificity and solution stability.

  16. Qualitative and quantitative analysis of flavonoids in Sophora tonkinensis by LC/MS and HPLC.

    Science.gov (United States)

    He, Chang-Ming; Cheng, Zhi-Hong; Chen, Dao-Feng

    2013-11-01

    To develop analytical methods for the identification and determination of the flavonoids in Sophora tonkinensis for comprehensive quality evaluation. An HPLC-DAD-ESI-MS method was used for the separation and characterization of the flavonoids in S. tonkinensis, and a liquid chromatographic method was employed to simultaneously determine five major active flavonoids in this crude drug. Seventeen flavonoids were identified, among which, seven were unambiguously identified as trifolirhizin, quercetin, formononetin, macckiain, kurarinone, sophoranone, and sophoranochromene by comparing their retention times, and UV and MS spectra with those of the authentic compounds, and the other ten flavonoids were tentatively identified by comparing their UV and MS/MS spectra with those of literature data. Furthermore, five major active flavonoids, including trifolirhizin, quercetin, maackiain, sophoranone, and sophoranochromene were determined in S. tonkinensis. All calibration curves expressed good linearity (r > 0.999 8) within the test ranges, and the recovery from this method was 96.40%-104.43%. The developed HPLC method was successfully applied to quantitatively determine the five flavonoids in seventeen samples of S. tonkinensis. The developed method rapidly characterized the bioactive flavonoids of S. tonkinensis, and could be readily utilized to enhance the quality assurance approaches for this traditional Chinese medicine. Copyright © 2013 China Pharmaceutical University. Published by Elsevier B.V. All rights reserved.

  17. Use of cyanopropyl-bonded hplc column for bioassay-directed fractionation of organic extracts from incinerator emissions

    International Nuclear Information System (INIS)

    DeMarini, D.M.; Williams, R.W.; Brooks, L.R.; Taylor, M.S.

    1992-01-01

    The present study has shown that cyanopropyl-(CN) bonded silica HPLC columns are applicable for the fractionation of mass and mutagenic activity of organic extracts from some incinerator emissions. Dichloromethane-extractable organics from particles emitted by two different municipal waste incinerators and by a pilot-scale rotary kiln incinerator that was combusting polyethylene were fractionated by HPLC, and the mutagenicity of the fractions was determined by means of a microsuspension mutagenicity assay with Salmonella TA98. The CN-bonded silica columns provided high (80-100 percent) mass and mutagenicity recoveries for most emission extracts, and it fractionated the mutagenic activity. The results suggest that the emissions from municipal waste incinerators contain a high amount of direct-acting (-S9) mutagenic activity that is resolvable by HPLC using CN-bonded silica. Sub-fractionation of selected mutagenic HPLC fractions and subsequent analysis by gas chromatography/mass spectroscopy can be used to identify mutagenic species within complex incinerator emissions. The coupling of microsuspension bioassays to HPLC fractionation should be a useful tool for this type of analysis

  18. Competitive Nitration of Benzene-Fluorobenzene and Benzene-Toluene Mixtures: Orientation and Reactivity Studies Using HPLC

    Science.gov (United States)

    Blankespoor, Ronald L.; Hogendoorn, Stephanie; Pearson, Andrea

    2007-01-01

    The reactivity and orientation effects of a substituent are analyzed by using HPLC to determine the competitive nitration of the benzene-toluene and benzene-fluorobenzene mixtures. The results have shown that HPLC is an excellent instrumental method to use in analyzing these mixtures.

  19. Separation and HPLC-MS identification of phenolic antioxidants from agricultural residues: Almond hulls and grape pomace

    DEFF Research Database (Denmark)

    Rubilar, M.; Pinelo, Manuel; Shene, C.

    2007-01-01

    Almond hulls and grape pomace are residues abundantly generated by agricultural industries, which could be processed to obtain bioactive products. To this purpose, crude ethanol extracts from both agricultural byproducts were attained and subsequently fractionated in order to obtain an organic....../water fraction (FOW). Extracts and fractions were analyzed for antioxidant power and their phenolic components tentatively identified by HPLC-MS. Chromatographic peaks of almond hull extracts showed the occurrence of hydroxybenzoic and cinnamic acid derivatives, with minor presence of flavan-3-ols (ECG, EGCG...... was assessed by DPPH and TBARS assays. Almond hulls showed inhibition percentages lower than 50% in both assays, while the inhibition percentage ranged from 80% to 90% in pomace extracts. Red grape pomace extract was the most efficient antioxidant, with an EC50 value of 0.91 g/L for TBARS and 0.20 g/L for DPPH...

  20. Comparison of UHPLC and HPLC in Benzodiazepines Analysis of Postmortem Samples

    Science.gov (United States)

    Behnoush, Behnam; Sheikhazadi, Ardeshir; Bazmi, Elham; Fattahi, Akbar; Sheikhazadi, Elham; Saberi Anary, Seyed Hossein

    2015-01-01

    Abstract The aim of this study was to compare system efficiency and analysis duration regarding the solvent consumption and system maintenance in high-pressure liquid chromatography (HPLC) and ultra high-pressure liquid chromatography (UHPLC). In a case–control study, standard solutions of 7 benzodiazepines (BZs) and 73 biological samples such as urine, tissue, stomach content, and bile that screened positive for BZs were analyzed by HPLC and UHPLC in laboratory of forensic toxicology during 2012 to 2013. HPLC analysis was performed using a Knauer by 100-5 C-18 column (250 mm × 4.6 mm) and Knauer photodiode array detector (PAD). UHPLC analysis was performed using Knauer PAD detector with cooling autosampler and Eurospher II 100-3 C-18 column (100 mm × 3 mm) and also 2 pumps. The mean retention time, standard deviation, flow rate, and repeatability of analytical results were compared by using 2 methods. Routine runtimes in HPLC and UHPLC took 40 and 15 minutes, respectively. Changes in mobile phase composition of the 2 methods were not required. Flow rate and solvent consumption in UHPLC decreased. Diazepam and flurazepam were detected more frequently in biological samples. In UHPLC, small particle size and short length of column cause effective separation of BZs in a very short time. Reduced flow rate, solvent consumption, and injection volume cause more efficiency and less analysis costs. Thus, in the detection of BZs, UHPLC is an accurate, sensitive, and fast method with less cost of analysis. PMID:25860209