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Sample records for switching liquid chromatography

  1. A column switching ultrahigh-performance liquid chromatography-tandem mass spectrometry method to determine anandamide and 2-arachidonoylglycerol in plasma samples.

    Science.gov (United States)

    Marchioni, Camila; de Souza, Israel Donizeti; Grecco, Caroline Fernandes; Crippa, José Alexandre; Tumas, Vitor; Queiroz, Maria Eugênia Costa

    2017-05-01

    This study reports a fast, sensitive, and selective column switching ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method to determine the endocannabinoids (eCBs), anandamide (AEA), and 2-arachidonoylglycerol (2-AG) in plasma samples. This bidimensional system used a restricted access media column (RP-8 ADS, 25 mm × 4 mm × 25 μM) in the first dimension and a core-shell Kinetex C18 (100 mm × 2, 1.7 mm × 1 μM) column in the second dimension, followed by detection in a mass spectrometer triple quadrupole (multiple reactions monitoring mode) operating in the positive mode. RP-8 ADS was used for trace enrichment of eCBs (reverse phase partitioning) and macromolecular matrix size exclusion; the core-shell column was used for the chromatographic separation. The column switching UHPLC-MS/MS method presented a linear range spanning from 0.1 ng mL -1 (LOQ) to 6 ng mL -1 for AEA and from 0.04 ng mL -1 (LOQ) to 10 ng mL -1 for 2-AG. Excluding the LLOQ values, the precision assays provided coefficients of variation lower than 8% and accuracy with relative standard error values lower than 14%. Neither carryover nor matrix effects were detected. This high-throughput column switching method compared to conventional methods is time saving as it involves fewer steps, consumes less solvent, and presents lower LLOQ. The column switching UHPLC-MS/MS method was successfully applied to determine AEA and 2-AG in plasma samples obtained from Alzheimer's disease patients. Graphical abstract A column switching ultra high-performance liquid chromatography-tandem mass spectrometry method using RP-8 ADS column and core shell column to determine endocannabinoids in plasma samples.

  2. Determination of 3-hydroxypropylmercapturic acid in urine by three column-switching high-performance liquid chromatography with electrochemical detection using a diamond electrode.

    Science.gov (United States)

    Higashi, Kyohei; Shibasaki, Mana; Kuni, Kyoshiro; Uemura, Takeshi; Waragai, Masaaki; Uemura, Kenichi; Igarashi, Kazuei; Toida, Toshihiko

    2017-09-29

    A three column-switching high-performance liquid chromatography (HPLC) using an electrochemical detector (ECD) equipped with a diamond electrode was established to determine 3-hydroxypropylmercapturic acid (3-HPMA) in urine. An extracted urine sample was consecutively fractionated using a strong anion-exchange column (first column) and a C8 column (second column) via a switching valve before application on an Octa Decyl Silyl (ODS) column (third column), followed by ECD analysis. The% recovery of 3-HPMA standard throughout the three-column process and limit of detection (LOD) were 94±1% and 0.1pmol, respectively. A solid phase extraction step is required for the sensitive analysis of 3-HPMA in urine by column-switching HPLC-ECD despite a decreased% recovery (55%) of urine sample spiked with 100pmol of 3-HPMA. To test the utility of our column-switching HPLC-ECD method, 3-HPMA levels of 27 urine samples were determined, and the correlation between HPLC-ECD and LC-Electrospray ionization (ESI)-MS/MS method was examined. As a result, the median values of μmol 3-HPMA/g Creatinine (Cre) in urine obtained by column-switching HPLC-ECD and LC-MS/MS were 2.19±2.12μmol/g Cre and 2.13±3.38μmol/g Cre, respectively, and the calibration curve (y=1.5171x-1.007) exhibited good linearity within a defined range (r 2 =0.907). These results indicate that the combination of column-switching HPLC and ECD is a powerful tool for the specific, reliable detection of 3-HPMA in urine. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. performance liquid chromatography

    African Journals Online (AJOL)

    user

    2010-11-22

    Nov 22, 2010 ... ISSN 1684–5315 © 2010 Academic Journals. Full Length Research Paper. Determination ... Key words: Processed food, high-performance liquid chromatography, acrylamide, health hazard. INTRODUCTION. In the year 2002, the ... potatoes, breakfast cereals etc. It was thus confirmed that acrylamide has ...

  4. Impact of injection solvent composition on protein identification in column-switching chip-liquid chromatography/mass spectrometry.

    Science.gov (United States)

    Houbart, V; Cobraiville, G; Nys, G; Merville, M-P; Fillet, M

    2016-05-06

    In shotgun proteomics, the gold standard technique is reversed-phase liquid chromatography coupled to mass spectrometry. Many researches have been carried out to study the effects on identification performances of chromatographic parameters such as the stationary phase and column dimensions, mobile phase composition and flow rate, as well as the gradient slope and length. However, little attention is usually paid to the injection solvent composition. In this study, we investigated the effect of the injection solvent on protein identification parameters (number of distinct peptides, amino acid coverage and MS/MS search score) as well as sensitivity. Tryptic peptides from six different proteins, covering a wide range of physicochemical properties, were employed as training set. Design of experiments was employed as a tool to highlight the factors related to the composition of the injection solvent that significantly influenced the obtained results. Optimal results for the training set were applied to analysis of more complex samples. The experiments pointed out optimising the composition of the injection solvent had a strong beneficial effect on all the considered responses. On the basis of these results, an approach to determine optimal conditions was proposed to maximise the protein identification performances and detection sensitivity. Copyright © 2016 Elsevier B.V. All rights reserved.

  5. Determination of lansoprazole enantiomers in dog plasma by column-switching liquid chromatography with tandem mass spectrometry and its application to a preclinical pharmacokinetic study.

    Science.gov (United States)

    Wang, Hao; Sun, Yantong; Meng, Xiangjun; Yang, Bo; Wang, Jian; Yang, Yan; Gu, Jingkai

    2015-09-01

    Lansoprazole, a selective proton pump inhibitor, has a chiral benzimidazole sulfoxide structure and is used for the treatment of gastric acid hypersecretory related diseases. To investigate its stereoselective pharmacokinetics, a column-switching liquid chromatography with tandem mass spectrometry method was developed for the determination of lansoprazole enantiomers in dog plasma using (+)-pantoprazole as an internal standard. After a simple protein precipitation procedure with acetonitrile, matrix components left behind after sample preparation were further eliminated from the sample by reversed-phase chromatography on a C18 column. The fluent was fed to a chiral column for the separation of lansoprazole enantiomers. Baseline separation of lansoprazole enantiomers was achieved on a Chiralcel OZ-RH column using acetonitrile/0.1% formic acid in water (35:65, v/v) as the mobile phase at 40°C. The linearity of the calibration curves ranged from 3 to 800 ng/mL for each enantiomer. Intra- and inter-day precisions ranged from 2.1 to 7.3% with an accuracy of ±1.7% for (+)-lansoprazole, and from 1.6 to 6.9% with an accuracy of ±3.5% for (-)-lansoprazole, respectively. The validated method was successfully applied for the stereoselective pharmacokinetic study of lansoprazole in beagle dog after intravenous infusion. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Rapid determination of 12 antibiotics and caffeine in sewage and bioreactor effluent by online column-switching liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Lima Gomes, Paulo C F; Tomita, Inês N; Santos-Neto, Álvaro J; Zaiat, Marcelo

    2015-11-01

    This study presents a column-switching solid-phase extraction online-coupled to a liquid chromatography/tandem mass spectrometry (SPE-LC-MS/MS) method for simultaneous analysis of 12 antibiotics (7 sulfonamides and 5 fluoroquinolones) and caffeine detected in the sewage and effluent of a pilot anaerobic reactor used in sewage treatment. After acidification and filtration, the samples were directly injected into a simple and conventional LC system. Backflush and foreflush modes were compared based on the theoretical plates and peak asymmetry observed. The method was tested in terms of detection (MDL) and quantification limit (MQL), linearity, relative recovery, and precision intra- and inter-day in lab-made sewage samples. The method presented suitable figures of merit in terms of detection, varying from 8.00 × 10(-5) to 6.00 × 10(-2) ng (0.800 up to 600 ng L(-1); caffeine) with direct injection volume of only 100 μL and 13 min of total analysis time (sample preparation and chromatographic run). When the method was applied in the analysis of sewage and effluent of the anaerobic reactor (n = 15), six antibiotics and caffeine were detected in concentrations ranging from 0.018 to 1097 μg L(-1). To guarantee a reliable quantification, standard addition was used to overcome the matrix effect.

  7. Capillary column switching restricted-access media-liquid chromatography-electrospray ionization-tandem mass spectrometry system for simultaneous and direct analysis of drugs in biofluids.

    Science.gov (United States)

    Santos-Neto, Alvaro J; Markides, Karin E; Sjöberg, Per J R; Bergquist, Jonas; Lancas, Fernando M

    2007-08-15

    Capillary online restricted-access media-liquid chromatography-electrospray ionization-tandem mass spectrometry (RAM-LC-ESI-MS/MS) for direct analysis of drugs and metabolites spiked in biological fluids was developed. Using a column switching setup it was possible to perform effective sample preparation and analysis of raw biological fluids (plasma and urine) without matrix effects in the electrospray mass spectrometric detection step. The peak focusing efficiency of the extraction column was more effective in backflush compared to foreflush mode. The system was able to concentrate diminished samples of polar drugs and their metabolites reaching quantifiable results as low as 1 ng/mL utilizing a sample volume of only 333 nL of biofluids. New column hardware was developed to circumvent clogging problems experienced with plasma injections. The glass fiber filter frit, which is commonly used, was replaced with a short piece of 20 microm i.d. fused silica capillary. The extraction columns were able to handle up to 60 injections and showed a high loading capacity, making the saturation of the MS detector the limiting factor on the linear dynamic range. The simultaneous separation and detection of 10 drugs and metabolites was obtained in 8 min of analysis, including the online sample preparation and enrichment step.

  8. Determination of Myo-Inositol in Infant, Pediatric, and Adult Formulas by Liquid Chromatography-Pulsed Amperometric Detection with Column Switching: Collaborative Study, Final Action 2011.18.

    Science.gov (United States)

    Butler-Thompson, Linda D; Jacobs, Wesley A; Schimpf, Karen J

    2015-01-01

    AOAC First Action Method 2011.18, Myo-Inositol (Free and Bound as Phosphatidylinositol) in Infant and Pediatric Formulas and Adult Nutritionals, was collaboratively studied. With this method free myo-inositol and phosphatidylinositol bound myo-inositol are extracted using two different sample preparation procedures, separated by ion chromatography using a combination of Dionex Carbo Pac PA1 and MA1 columns with column switching, and detected with pulsed amperometry using a gold electrode. Free myo-inositol is extracted from samples with dilute hydrochloric acid and water. Phosphatidylinositol is extracted from samples with chloroform and separated from other fats with silica SPE cartridges. Myo-inositol is then released from the glycerol backbone with concentrated acetic and hydrochloric acids at 120°C. During this collaborative study, nine laboratories from five different countries analyzed blind duplicates of nine infant and pediatric nutritional formulas for both free and phosphatidylinositol bound myo-inositol, and one additional laboratory only completed the free myo-inositol analyses. The method demonstrated acceptable repeatability and reproducibility and met the AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals (SPIFAN) Standard Method Performance Requirements (SMPRs®) for free myo-inositol plus phosphatidylinositol bound myo-inositol for all the matrixes analyzed. SMPRs for repeatability were ≤5% RSD at myo-inositol concentrations of 2-68 mg/100 g ready-to-feed (RTF) liquid. SMPRs for reproducibility were ≤8% RSD in products with myo-inositol concentrations ranging from 2 to 68 mg/100 g RTF liquid. During this collaborative study, repeatability RSDs ranged from 0.51 to 3.22%, and RSDs ranged from 2.66 to 7.55% for free myo-inositol plus phosphatidylinositol bound myo-inositol.

  9. An ultra-sensitive method for the analysis of perfluorinated alkyl acids in drinking water using a column switching high-performance liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Dasu, Kavitha; Nakayama, Shoji F; Yoshikane, Mitsuha; Mills, Marc A; Wright, J Michael; Ehrlich, Shelley

    2017-04-21

    In epidemiological research, it has become increasingly important to assess subjects' exposure to different classes of chemicals in multiple environmental media. It is a common practice to aliquot limited volumes of samples into smaller quantities for specific trace level chemical analyses. A novel method was developed for the determination of 14 perfluorinated alkyl acids (PFAAs) in small volumes (10mL) of drinking water using off-line solid phase extraction (SPE) pre-treatment followed by on-line pre-concentration on a WAX column before analysis on column-switching high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). In general, large volumes (100-1000mL) have been used for the analysis of PFAAs in drinking water. The current method requires approximately 10mL of drinking water concentrated by using an SPE cartridge and eluted with methanol. A large volume injection of the extract was introduced on to a column-switching HPLC-MS/MS using a mix-mode SPE column for the trace level analysis of PFAAs in water. The recoveries for most of the analytes in the fortified laboratory blanks ranged from 73±14% to 128±5%. The lowest concentration minimum reporting levels (LCMRL) for the 14 PFAAs ranged from 0.59 to 3.4ng/L. The optimized method was applied to a pilot-scale analysis of a subset of drinking water samples from an epidemiological study. These samples were collected directly from the taps in the households of Ohio and Northern Kentucky, United States and the sources of drinking water samples are both surface water and ground water, and supplied by different water distribution facilities. Only five PFAAs, perfluoro-1-butanesulfonic acid (PFBS), perfluoro-1- -hexanesulfonic acid (PFHxS), perfluoro-1-octanesulfonic acid (PFOS), perfluoro-n-heptanoic acid (PFHpA) and perfluoro-n-octanoic acid (PFOA) are detected above the LCMRL values. The median concentrations of these five PFAAs detected in the samples was ≤4.1ng/L with PFOS at 7.6ng

  10. Introduction to modern liquid chromatography

    National Research Council Canada - National Science Library

    Snyder, Lloyd R; Kirkland, J. J; Dolan, John W

    2010-01-01

    "High-performance liquid chromatography (HPLC) is today the leading technique for chemical analysis and related applications, with an ability to separate, analyze, and/or purify virtually any sample...

  11. Liquid phase chromatography on microchips

    DEFF Research Database (Denmark)

    Kutter, Jörg Peter

    2012-01-01

    explosive development of, in particular, chromatographic separation systems on microchips, has, however, slowed down in recent years. This review takes a closer, critical look at how liquid phase chromatography has been implemented in miniaturized formats over the past several years, what is important...

  12. Identification and quantification of flavonoids in human urine samples by column switching liquid chromatography coupled to atmospheric pressure chemical ionization mass spectrometry

    DEFF Research Database (Denmark)

    Nielsen, Salka E.; Freese, R.; Cornett, C.

    2000-01-01

    A rapid and sensitive high-performance liquid chromatographic mass spectrometric (HPLC-MS) method is described for the determination and quantification of 12 dietary flavonoid glycosides and aglycons in human urine samples. Chromatographic separation of the analytes of interest was achieved...... by column-switching, using the first column (a Zorbax 300SB C-3 column) for sample cleanup and eluting the heart-cut flavonoid fraction onto the second column (a Zorbax SE C-18 column) for separation and detection by ultraviolet and atmospheric pressure chemical ionization MS using single ion monitoring...... of variation for the analysis of the 12 different flavonoids in quality control urine samples were 12.3% on average (range 11.0-13.7%, n = 24, reproducibility) and the repeatability of the assay were 5.0% (mean, range 0.1-14.8%, it = 12). A subset of 10 urine samples from a human dietary intervention study...

  13. Versatile lipid profiling by liquid chromatography-high resolution mass spectrometry using all ion fragmentation and polarity switching. Preliminary application for serum samples phenotyping related to canine mammary cancer.

    Science.gov (United States)

    Gallart-Ayala, H; Courant, F; Severe, S; Antignac, J-P; Morio, F; Abadie, J; Le Bizec, B

    2013-09-24

    Lipids represent an extended class of substances characterized by such high variety and complexity that makes their unified analyses by liquid chromatography coupled to either high resolution or tandem mass spectrometry (LC-HRMS or LC-MS/MS) a real challenge. In the present study, a new versatile methodology associating ultra high performance liquid chromatography coupled to high resolution tandem mass spectrometry (UHPLC-HRMS/MS) have been developed for a comprehensive analysis of lipids. The use of polarity switching and "all ion fragmentation" (AIF) have been two action levels particularly exploited to finally permit the detection and identification of a multi-class and multi-analyte extended range of lipids in a single run. For identification purposes, both higher energy collision dissociation (HCD) and in-source CID (collision induced dissociation) fragmentation were evaluated in order to obtain information about the precursor and product ions in the same spectra. This approach provides both class-specific and lipid-specific fragments, enhancing lipid identification. Finally, the developed method was applied for differential phenotyping of serum samples collected from pet dogs developing spontaneous malignant mammary tumors and health controls. A biological signature associated with the presence of cancer was then successfully revealed from this lipidome analysis, which required to be further investigated and confirmed at larger scale. Copyright © 2013 Elsevier B.V. All rights reserved.

  14. Simultaneous determination of phentermine and topiramate in human plasma by liquid chromatography-tandem mass spectrometry with positive/negative ion-switching electrospray ionization and its application in pharmacokinetic study.

    Science.gov (United States)

    Ni, Yang; Zhou, Ying; Xu, Mingzhen; He, Xiaomeng; Li, Huqun; Haseeb, Satter; Chen, Hui; Li, Weiyong

    2015-03-25

    A new method for simultaneous determination of phentermine and topiramate by liquid chromatography/electrospray tandem mass spectrometry (LC/MS/MS) operated in positive and negative ionization switching modes was developed and validated. Protein precipitation with acetonitrile was selected for sample preparation. Analyses were performed on a liquid chromatography system employing a Kromasil 60-5CN column (2.1 mm × 100 mm, 5 μm) and an isocratic elution with mixed solution of acetonitrile-20mM ammonium formate containing 0.3% formic acid (40:60, v/v), at a flow rate of 0.35 mL/min. Doxazosin mesylate and pioglitazone were used as the internal standard (IS) respectively for quantification. The determination was carried out on an API 4000 triple-quadrupole mass spectrometer operated in multiple reaction monitoring (MRM) mode using the following transitions monitored simultaneously: positive m/z 150.0/91.0 for phentermine, m/z 452.1/344.3 for doxazosin, and negative m/z 338.3/77.9 for topiramate, m/z 355.0/41.9 for pioglitazone. The method was validated to be linear over the concentration range of 1-800 ng mL(-1) for phentermine, 1-1000 ng mL(-1) for topiramate. Within- and between-day accuracy and precision of the validated method at three different concentration levels were within the acceptable limits of <15% at all concentrations. Blood samples were collected into heparinized tubes before and after administration. The simple and robust LC/MS/MS method was successfully applied for the simultaneous determination of phentermine and topiramate in a pharmacokinetic study in healthy male Chinese volunteers. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. Identification and quantification of flavonoids in human urine samples by column switching liquid chromatography coupled to atmospheric pressure chemical ionization mass spectrometry

    DEFF Research Database (Denmark)

    Nielsen, S. E.; Freese, R.; Cornett, Claus

    2000-01-01

    by column-switching, using the first column (a Zorbax 300SB C-3 column) for sample cleanup and eluting the heart-cut flavonoid fraction onto the second column (a Zorbax SE C-18 column) for separation and detection by ultraviolet and atmospheric pressure chemical ionization MS using single ion monitoring...

  16. Simultaneous determination of carboprost methylate and its active metabolite carboprost in dog plasma by liquid chromatography-tandem mass spectrometry with positive/negative ion-switching electrospray ionization and its application to a pharmacokinetic study.

    Science.gov (United States)

    Yin, Lei; Meng, Xiangjun; Zhou, Xiaotong; Zhang, Tinglan; Sun, Heping; Yang, Zhichao; Yang, Bo; Xiao, Ning; Fawcett, J Paul; Yang, Yan; Gu, Jingkai

    2015-08-15

    A liquid chromatography-tandem mass spectrometric (LC-MS/MS) method using positive/negative electrospray ionization (ESI) switching for the simultaneous quantitation of carboprost methylate and carboprost in dog plasma has been developed and validated. After screening, the esterase inhibitor, dichlorvos was added to the whole blood at a ratio of 1:99 (v/v) to stabilize carboprost methylate during blood collection, sample storage and LLE. Indomethacin was added to plasma to inhibit prostaglandins synthesis after sampling. After liquid-liquid extraction of 500μL plasma with ethyl ether-dichloromethane (75:25, v/v), analytes and internal standard (IS), alprostadil-d4, were chromatographed on a CAPCELL PAK Phenyl column (150×2.0mm, 5μm) using acetonitrile-5mM ammonium acetate as mobile phase. Carboprost methylate was detected by positive ion electrospray ionization followed by multiple reaction monitoring (MRM) of the transition at m/z 400.5→329.3; the carboprost and IS were detected by negative ion electrospray ionization followed by MRM of the transitions at m/z 367.2→323.2, and 357.1→321.2, respectively. The method was linear for both analytes in the concentration range 0.05-30ng/mL with intra- and inter-day precisions (as relative standard deviation) of ≤6.75% and accuracy (as relative error) of ≤7.21% and limit of detection (LOD) values were 10 and 20pg/mL, respectively. The method was successfully applied to a pharmacokinetic study of the analytes in beagle dogs after intravaginal administration of a suppository containing 0.5mg carboprost methylate. Copyright © 2015 Elsevier B.V. All rights reserved.

  17. Improved sensitivity using liquid chromatography mass spectrometry ...

    African Journals Online (AJOL)

    Improved sensitivity using liquid chromatography mass spectrometry (LC-MS) for detection of propyl chloroformate derivatised β-N-methylamino-L-alanine (BMAA) in ... We show a 10-fold increase in sensitivity with the LC-MS method compared to the previously published gas chromatography mass spectrometry (GC-MS) ...

  18. UHPLC: The Greening Face of Liquid Chromatography

    OpenAIRE

    Cielecka-Piontek, Judyta; Zalewski, Przemys?aw; Jeli?ska, Anna; Garbacki, Piotr

    2013-01-01

    Pharmaceutical analysis based on chromatographic separation is an important part of studies aimed at developing routine quality analysis of drugs. High-performance liquid chromatography (HPLC) is one of the main analytical techniques recommended for drug analysis. Although it meets many criteria vital for analysis, it is time-consuming and uses a relatively high amount of organic solvents compared to other analytical techniques. Recently, Ultra-high-performance liquid chromatography (UHPLC) h...

  19. Identification and quantification of flavonoids in human urine samples by column switching liquid chromatography coupled to atmospheric pressure chemical ionization mass spectrometry

    DEFF Research Database (Denmark)

    Nielsen, S. E.; Freese, R.; Cornett, Claus

    2000-01-01

    A rapid and sensitive high-performance liquid chromatographic mass spectrometric (HPLC-MS) method is described for the determination and quantification of 12 dietary flavonoid glycosides and aglycons in human urine samples. Chromatographic separation of the analytes of interest was achieved by co...

  20. Simultaneous determination of asperosaponin VI and its active metabolite hederagenin in rat plasma by liquid chromatography-tandem mass spectrometry with positive/negative ion-switching electrospray ionization and its application in pharmacokinetic study.

    Science.gov (United States)

    Zhu, He; Ding, Li; Shakya, Shailendra; Qi, Xiemin; Hu, Linlin; Yang, Xiaolin; Yang, Zhonglin

    2011-11-15

    A new liquid chromatography-tandem mass spectrometry (LC-MS/MS) method operated in the positive/negative electrospray ionization (ESI) switching mode has been developed and validated for the simultaneous determination of asperosaponin VI and its active metabolite hederagenin in rat plasma. After addition of internal standards diazepam (for asperosaponin VI) and glycyrrhetic acid (for hederagenin), the plasma sample was deproteinized with acetonitrile, and separated on a reversed phase C18 column with a mobile phase of methanol (solvent A)-0.05% glacial acetic acid containing 10 mM ammonium acetate and 30 μM sodium acetate (solvent B) using gradient elution. The detection of target compounds was done in multiple reaction monitoring (MRM) mode using a tandem mass spectrometry equipped with positive/negative ion-switching ESI source. At the first segment, the MRM detection was operated in the positive ESI mode using the transitions of m/z 951.5 ([M+Na](+))→347.1 for asperosaponin VI and m/z 285.1 ([M+H](+))→193.1 for diazepam for 4 min, then switched to the negative ESI mode using the transitions of m/z 471.3 ([M-H](-))→471.3 for hederagenin and m/z 469.4 ([M-H](-))→425.4 for glycyrrhetic acid, respectively. The sodiated molecular ion [M+Na](+) at m/z 951.5 was selected as the precursor ion for asperosaponin VI, since it provided better sensitivity compared to the deprotonated and protonated molecular ions. Sodium acetate was added to the mobile phase to make sure that abundant amount of the sodiated molecular ion of asperosaponin VI could be produced, and more stable and intensive mass response of the product ion could be obtained. For the detection of hederagenin, since all of the mass responses of the fragment ions were very weak, the deprotonated molecular ion [M-H](-)m/z 471.3 was employed as both the precursor ion and the product ion. But the collision energy was still used for the MRM, in order to eliminate the influences induced by the interference

  1. Development and Validation of Liquid Chromatography- Mass ...

    African Journals Online (AJOL)

    HP

    Purpose: To determine naproxen levels in human plasma using a new liquid chromatography-Mass spectroscopy/Mass spectroscopy (LC-MS/MS) method that involves a simple and single step extraction procedure using low-cost reagents. Method: A novel liquid chromatography–tandem mass spectrometry method for the ...

  2. Simultaneous Determination of Celecoxib, Erlotinib, and its Metabolite Desmethyl-Erlotinib (OSI-420) in Rat Plasma by Liquid chromatography/Tandem Mass Spectrometry with Positive/Negative Ion-Switching Electrospray Ionisation.

    Science.gov (United States)

    Thappali, Satheeshmanikandan R S; Varanasi, Kanthikiran; Veeraraghavan, Sridhar; Arla, Rambabu; Chennupati, Sandhya; Rajamanickam, Madheswaran; Vakkalanka, Swaroop; Khagga, Mukkanti

    2012-01-01

    A new method for the simultaneous determination of celecoxib, erlotinib, and its active metabolite desmethyl-erlotinib (OSI-420) in rat plasma, by liquid chromatography/tandem mass spectrometry with positive/negative ion-switching electrospray ionization mode, was developed and validated. Protein precipitation with methanol was selected as the method for preparing the samples. The analytes were separated on a reverse-phase C(18) column (50mm×4.6mm i.d., 3μ) using methanol: 2 mM ammonium acetate buffer, and pH 4.0 as the mobile phase at a flow rate 0.8 mL/min. Sitagliptin and Efervirenz were used as the internal standards for quantification. The determination was carried out on a Theremo Finnigan Quantam ultra triple-quadrupole mass spectrometer, operated in selected reaction monitoring (SRM) mode using the following transitions monitored simultaneously: positive m/z 394.5→278.1 for erlotinib, m/z 380.3→278.1 for desmethyl erlotinib (OSI-420), and negative m/z -380.1→ -316.3 for celecoxib. The limits of quantification (LOQs) were 1.5 ng/mL for Celecoxib, erlotinib, and OSI-420. Within- and between-day accuracy and precision of the validated method were within the acceptable limits of < 15% at all concentrations. The quantitation method was successfully applied for the simultaneous estimation of celecoxib, erlotinib, and desmethyl erlotinib in a pharmacokinetic study in Wistar rats.

  3. Liquid chromatography detection unit, system, and method

    Science.gov (United States)

    Derenzo, Stephen E.; Moses, William W.

    2015-10-27

    An embodiment of a liquid chromatography detection unit includes a fluid channel and a radiation detector. The radiation detector is operable to image a distribution of a radiolabeled compound as the distribution travels along the fluid channel. An embodiment of a liquid chromatography system includes an injector, a separation column, and a radiation detector. The injector is operable to inject a sample that includes a radiolabeled compound into a solvent stream. The position sensitive radiation detector is operable to image a distribution of the radiolabeled compound as the distribution travels along a fluid channel. An embodiment of a method of liquid chromatography includes injecting a sample that comprises radiolabeled compounds into a solvent. The radiolabeled compounds are then separated. A position sensitive radiation detector is employed to image distributions of the radiolabeled compounds as the radiolabeled compounds travel along a fluid channel.

  4. Instrument platforms for nano liquid chromatography

    Czech Academy of Sciences Publication Activity Database

    Šesták, Jozef; Moravcová, Dana; Kahle, Vladislav

    2015-01-01

    Roč. 1421, NOV (2015), s. 2-17 ISSN 0021-9673 R&D Projects: GA MV VG20112015021 Institutional support: RVO:68081715 Keywords : nano liquid chromatography * splitless gradient generation * nano LC platforms Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.926, year: 2015 http://hdl.handle.net/11104/0250900

  5. Validated High Performance Liquid Chromatography Method for ...

    African Journals Online (AJOL)

    Purpose: To develop a simple, rapid and sensitive high performance liquid chromatography (HPLC) method for the determination of cefadroxil monohydrate in human plasma. Methods: Schimadzu HPLC with LC solution software was used with Waters Spherisorb, C18 (5 μm, 150mm × 4.5mm) column. The mobile phase ...

  6. Porphyrins profile by high performance liquid chromatography ...

    African Journals Online (AJOL)

    E. Fateen

    2008-09-07

    Sep 7, 2008 ... tation of urinary porphyrins by liquid chromatography tandem mass spectrometry (LC/MS/MS) and thereby the ... by HPLC/ESI/MS/MS used in this study is a modification for the method Stoev et al. while ion mapping technique is a ..... designed for application by the Biochemical Genetics Depart- ment team.

  7. Ultra Performance Liquid Chromatography Tandem Mass ...

    African Journals Online (AJOL)

    NICOLAAS

    drugs alone.16. After a single oral dose of 120–800 mg of NTB in healthy sub- jects in a fasting state the peak plasma NTB concentration (tmax) was found to be 4–7 h, with a half-life of approximately 9–17 h.17 ... performance liquid chromatography mass spectrometry/mass .... to the likely biological plasma constituents.

  8. Recent development of ionic liquid stationary phases for liquid chromatography.

    Science.gov (United States)

    Shi, Xianzhe; Qiao, Lizhen; Xu, Guowang

    2015-11-13

    Based on their particular physicochemical characteristics, ionic liquids have been widely applied in many fields of analytical chemistry. Many types of ionic liquids were immobilized on a support like silica or monolith as stationary phases for liquid chromatography. Moreover, different approaches were developed to bond covalently ionic liquids onto the supporting materials. The obtained ionic liquid stationary phases show multi-mode mechanism including hydrophobic, hydrophilic, hydrogen bond, anion exchange, π-π, and dipole-dipole interactions. Therefore, they could be used in different chromatographic modes including ion-exchange, RPLC, NPLC and HILIC to separate various classes of compounds. This review mainly summarizes the immobilized patterns and types of ionic liquid stationary phases, their retention mechanisms and applications in the recent five years. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. Comparative determination of phenytoin by spectrophotometry, gas chromatography, liquid chromatography, enzyme immunoassay, and radioimmunoassay

    International Nuclear Information System (INIS)

    Castro, A.; Ibanez, J.; DiCesare, J.L.; Adams, R.F.; Malkus, H.

    1978-01-01

    Sera from patients being treated with phenytoin were analyzed for the drug by spectrophotometry, gas chromatography, radioimmunoasay, enzyme immunoassay, and liquid chromatography. The assay values obtained were intercompared statistically. Enzyme immunoassay and liquid chromatography appear to be attractive alternatives to the more traditional methods of spectrophotometry and gas chromatography. Our radioimmunoassay data correlated poorly with results by the four other methods

  10. High perfomance liquid chromatography in pharmaceutical analyses.

    Science.gov (United States)

    Nikolin, Branko; Imamović, Belma; Medanhodzić-Vuk, Saira; Sober, Miroslav

    2004-05-01

    In testing the pre-sale procedure the marketing of drugs and their control in the last ten years, high performance liquid chromatography replaced numerous spectroscopic methods and gas chromatography in the quantitative and qualitative analysis. In the first period of HPLC application it was thought that it would become a complementary method of gas chromatography, however, today it has nearly completely replaced gas chromatography in pharmaceutical analysis. The application of the liquid mobile phase with the possibility of transformation of mobilized polarity during chromatography and all other modifications of mobile phase depending upon the characteristics of substance which are being tested, is a great advantage in the process of separation in comparison to other methods. The greater choice of stationary phase is the next factor which enables realization of good separation. The separation line is connected to specific and sensitive detector systems, spectrafluorimeter, diode detector, electrochemical detector as other hyphernated systems HPLC-MS and HPLC-NMR, are the basic elements on which is based such wide and effective application of the HPLC method. The purpose high performance liquid chromatography (HPLC) analysis of any drugs is to confirm the identity of a drug and provide quantitative results and also to monitor the progress of the therapy of a disease.1) Measuring presented on the Fig. 1. is chromatogram obtained for the plasma of depressed patients 12 h before oral administration of dexamethasone. It may also be used to further our understanding of the normal and disease process in the human body trough biomedical and therapeutically research during investigation before of the drugs registration. The analyses of drugs and metabolites in biological fluids, particularly plasma, serum or urine is one of the most demanding but one of the most common uses of high performance of liquid chromatography. Blood, plasma or serum contains numerous endogenous

  11. UHPLC: The Greening Face of Liquid Chromatography.

    Science.gov (United States)

    Cielecka-Piontek, Judyta; Zalewski, Przemysław; Jelińska, Anna; Garbacki, Piotr

    2013-01-01

    Pharmaceutical analysis based on chromatographic separation is an important part of studies aimed at developing routine quality analysis of drugs. High-performance liquid chromatography (HPLC) is one of the main analytical techniques recommended for drug analysis. Although it meets many criteria vital for analysis, it is time-consuming and uses a relatively high amount of organic solvents compared to other analytical techniques. Recently, Ultra-high-performance liquid chromatography (UHPLC) has been frequently proposed as an alternative to HPLC, which means introducing an environment-friendly approach to drug analysis achieved by reducing the consumption of solvents. It also offers greater chromatographic resolution and higher sensitivity as well as requiring less time due to faster analysis. This review focuses on the basics of UHPLC, compares that technique with HPLC and discusses the possibilities of applying UHPLC for the analysis of different pharmaceuticals and biopharmaceuticals.

  12. Two-dimensional liquid chromatography and its application in traditional Chinese medicine analysis and metabonomic investigation.

    Science.gov (United States)

    Li, Zheng; Chen, Kai; Guo, Meng-zhe; Tang, Dao-quan

    2016-01-01

    Two-dimensional liquid chromatography has become an attractive analytical tool for the separation of complex samples due to its enhanced selectivity, peak capacity, and resolution compared with one-dimensional liquid chromatography. Recently, more attention has been drawn on the application of this separation technique in studies concerning traditional Chinese medicines, metabonomes, proteomes, and other complex mixtures. In this review, we aim to examine the application of two-dimensional liquid chromatography in traditional Chinese medicine analysis and metabonomic investigation. The classification and evaluation indexes were first introduced. Then, various switching methods were summarized when used in an on-line two-dimensional liquid chromatography system. Finally, the applications of this separation technique in traditional Chinese medicine analysis and metabonomic investigation were discussed on the basis of specific studies. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Flow Rates in Liquid Chromatography, Gas Chromatography and Supercritical Fluid Chromatography: A Tool for Optimization

    Directory of Open Access Journals (Sweden)

    Joris Meurs

    2016-08-01

    Full Text Available This paper aimed to develop a standalone application for optimizing flow rates in liquid chromatography (LC, gas chromatography (GC and supercritical fluid chromatography (SFC. To do so, Van Deemter’s equation, Knox’ equation and Golay’s equation were implemented in a MATLAB script and subsequently a graphical user interface (GUI was created. The application will show the optimal flow rate or linear velocity and the corresponding plate height for the set input parameters. Furthermore, a plot will be shown in which the plate height is plotted against the linear flow velocity. Hence, this application will give optimized flow rates for any set conditions with minimal effort.

  14. Optimizing separations in online comprehensive two-dimensional liquid chromatography.

    Science.gov (United States)

    Pirok, Bob W J; Gargano, Andrea F G; Schoenmakers, Peter J

    2018-01-01

    Online comprehensive two-dimensional liquid chromatography has become an attractive option for the analysis of complex nonvolatile samples found in various fields (e.g. environmental studies, food, life, and polymer sciences). Two-dimensional liquid chromatography complements the highly popular hyphenated systems that combine liquid chromatography with mass spectrometry. Two-dimensional liquid chromatography is also applied to the analysis of samples that are not compatible with mass spectrometry (e.g. high-molecular-weight polymers), providing important information on the distribution of the sample components along chemical dimensions (molecular weight, charge, lipophilicity, stereochemistry, etc.). Also, in comparison with conventional one-dimensional liquid chromatography, two-dimensional liquid chromatography provides a greater separation power (peak capacity). Because of the additional selectivity and higher peak capacity, the combination of two-dimensional liquid chromatography with mass spectrometry allows for simpler mixtures of compounds to be introduced in the ion source at any given time, improving quantitative analysis by reducing matrix effects. In this review, we summarize the rationale and principles of two-dimensional liquid chromatography experiments, describe advantages and disadvantages of combining different selectivities and discuss strategies to improve the quality of two-dimensional liquid chromatography separations. © 2017 The Authors. Journal of Separation Science published by WILEY-VCH Verlag GmbH & Co. KGaA.

  15. Comprehensive two-dimensional liquid chromatography: Ion chromatography × reversed-phase liquid chromatography for separation of low-molar-mass organic acids

    NARCIS (Netherlands)

    Brudin, S.S.; Shellie, R.A.; Haddad, P.R.; Schoenmakers, P.J.

    2010-01-01

    In the work presented here a novel approach to comprehensive two-dimensional liquid chromatography is evaluated. Ion chromatography is chosen for the first-dimension separation and reversed-phase liquid chromatography is chosen for the second-dimension separation mode. The coupling of these modes is

  16. Optimizing separations in online comprehensive two-dimensional liquid chromatography

    NARCIS (Netherlands)

    Pirok, Bob W.J.; Gargano, Andrea F.G.; Schoenmakers, Peter J.

    2018-01-01

    Online comprehensive two-dimensional liquid chromatography has become an attractive option for the analysis of complex nonvolatile samples found in various fields (e.g. environmental studies, food, life, and polymer sciences). Two-dimensional liquid chromatography complements the highly popular

  17. Trends in High Performance Liquid Chromatography for Cultural Heritage.

    Science.gov (United States)

    Degano, Ilaria; La Nasa, Jacopo

    2016-04-01

    The separation, detection and quantitation of specific species contained in a sample in the field of Cultural Heritage requires selective, sensitive and reliable methods. Procedures based on liquid chromatography fulfil these requirements and offer a wide range of applicability in terms of analyte types and concentration range. The main applications of High Performance Liquid Chromatography in this field are related to the separation and detection of dyestuffs in archaeological materials and paint samples by reversed-phase liquid chromatography with suitable detectors. The relevant literature will be revised, with particular attention to sample treatment strategies and future developments. Reversed phase chromatography has also recently gained increasing importance in the analysis of lipid binders and lipid materials in archaeological residues: the main advantages and disadvantages of the new approaches will be discussed. Finally, the main applications of ion chromatography and size exclusion chromatography in the field of Cultural Heritage will be revised in this chapter.

  18. An on-line coupling of nanofibrous extraction with column-switching high performance liquid chromatography - A case study on the determination of bisphenol A in environmental water samples.

    Science.gov (United States)

    Háková, Martina; Chocholoušová Havlíková, Lucie; Chvojka, Jiří; Solich, Petr; Šatínský, Dalibor

    2018-02-01

    Polyamide 6 nanofiber polymers were used as modern sorbents for on-line solid phase extraction (SPE) coupled with liquid chromatography. The on-line SPE system was tested for the determination of bisphenol A in river water samples. Polyamide nanofibers were prepared using needleless electrospinning, inserted into a mini-column cartridge (5 × 4.6mm) and coupled with HPLC. The effect of column packing and the amount of polyamide 6 on extraction efficiency was tested and the packing process was optimized. The proposed method was performed using a 50-µL sample injection followed by an on-line nanofibrous extraction procedure. The influence of the washing mobile phase on the retention of bisphenol A during the extraction procedure was evaluated. Ascentis ® Express C18 (10cm × 4.6mm) core-shell column was used as an analytical column. Fluorescence detection wavelengths (λ ex = 225nm and λ em = 320nm) were used for identification and quantification of Bisphenol A in river waters. The linearity was tested in the range from 2 to 500µgL -1 (using nine calibration points). The limits of detection and quantification were 0.6 and 2µgL -1 , respectively. The developed method was successfully used for the determination of bisphenol A in various samples of river waters in the Czech Republic (The Ohře, Labe, Nisa, Úpa, and Opava Rivers). Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Hydrophilic interaction liquid chromatography (HILIC) in proteomics

    OpenAIRE

    Boersema, Paul J.; Mohammed, Shabaz; Heck, Albert J. R.

    2008-01-01

    In proteomics, nanoflow multidimensional chromatography is now the gold standard for the separation of complex mixtures of peptides as generated by in-solution digestion of whole-cell lysates. Ideally, the different stationary phases used in multidimensional chromatography should provide orthogonal separation characteristics. For this reason, the combination of strong cation exchange chromatography (SCX) and reversed-phase (RP) chromatography is the most widely used combination for the separa...

  20. Simultaneous determination of ten antiepileptic drugs in human plasma by liquid chromatography and tandem mass spectrometry with positive/negative ion-switching electrospray ionization and its application in therapeutic drug monitoring.

    Science.gov (United States)

    Yin, Lei; Wang, Tingting; Shi, Meiyun; Zhang, Ying; Zhao, Xiaojun; Yang, Yan; Gu, Jingkai

    2016-03-01

    A simple, rapid, and high-throughput liquid chromatography with tandem mass spectrometry method for the simultaneous quantitation of ten antiepileptic drugs in human plasma has been developed and validated. The method required only 10 μL of plasma. After simple protein precipitation using acetonitrile, the analytes and internal standard diphenhydramine were separated on a Zorbax SB-C18 column (50 × 4.6 mm, 2.7 μm) using acetonitrile/water as the mobile phase at a flow rate of 0.9 mL/min. The total run time was 6 min for each sample. The validation results of specificity, matrix effects, recovery, linearity, precision, and accuracy were satisfactory. The lower limit of quantification was 0.04 μg/mL for carbamazepine, 0.02 μg/mL for lamotrigine, 0.01 μg/mL for oxcarbazepine, 0.4 μg/mL for 10-hydroxycarbazepine, 0.1 μg/mL for carbamazepine-10,11-epoxide, 0.15 μg/mL for levetiracetam, 0.06 μg/mL for phenytoin, 0.3 μg/mL for valproic acid, 0.03 μg/mL for topiramate, and 0.15 μg/mL for phenobarbital. The intraday precision and interday precision were less than 7.6%, with the accuracy ranging between -8.1 and 7.9%. The method was successfully applied to therapeutic drug monitoring of 1237 patients with epilepsy after administration of standard antiepileptic drugs. The method has been proved to meet the high-throughput requirements in therapeutic drug monitoring. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Millimeter-scale liquid metal droplet thermal switch

    Science.gov (United States)

    Yang, Tianyu; Kwon, Beomjin; Weisensee, Patricia B.; Kang, Jin Gu; Li, Xuejiao; Braun, Paul; Miljkovic, Nenad; King, William P.

    2018-02-01

    Devices capable of actively controlling heat flow have been desired by the thermal management community for decades. The need for thermal control has become particularly urgent with power densification resulting in devices with localized heat fluxes as high as 1 kW/cm2. Thermal switches, capable of modulating between high and low thermal conductances, enable the partitioning and active control of heat flow pathways. This paper reports a millimeter-scale thermal switch with a switching ratio >70, at heat fluxes near 10 W/cm2. The device consists of a silicone channel filled with a reducing liquid or vapor and an immersed liquid metal Galinstan slug. Galinstan has a relatively high thermal conductivity (≈16.5 W/mK at room temperature), and its position can be manipulated within the fluid channel, using either hydrostatic pressure or electric fields. When Galinstan bridges the hot and cold reservoirs (the "ON" state), heat flows across the channel. When the hot and cold reservoirs are instead filled with the encapsulating liquid or vapor (the "OFF" state), the cross-channel heat flow significantly reduces due to the lower thermal conductivity of the solution (≈0.03-0.6 W/mK). We demonstrate switching ratios as high as 15.6 for liquid filled channels and 71.3 for vapor filled channels. This work provides a framework for the development of millimeter-scale thermal switches and diodes capable of spatial and temporal control of heat flows.

  2. Microchip-based monolithic column for high performance liquid chromatography

    Data.gov (United States)

    National Aeronautics and Space Administration — We have developed microchip based monolithic columns that can be used for liquid chromatography of small organic molecules, as well as, macromolecules such as...

  3. Stereoselective determination of unchanged and glucuroconjugated eliprodil, a new anti-ischaemic drug, in human plasma and urine by precolumn derivatization and column-switching high-performance liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Malavasi, B; Ripamonti, M; Rouchouse, A; Ascalone, V

    1996-04-05

    An HPLC method was developed and validated for the determination in human plasma and urine of the enantiomers of eliprodil, (+/-)-alpha-(4-chlorophenyl)-4[(4-fluorophenyl) methyl]piperidine-1-ethanol hydrochloride, a new anti-ischaemic agent administered as a racemate. Both enantiomers are present in human plasma in unchanged and glucuroconjugated form, whereas only the glucuroconjugated form is excreted into urine; as a consequence, such metabolites in human plasma and urine should be submitted to enzymatic deconjugation with beta-glucuronidase (Escherichia coli) before being extracted. The general method involves a liquid-liquid extraction of eliprodil and internal standard from alkalinized plasma or urine with n-hexane, evaporation of the organic phase and derivatization with (S)-(+)-naphthylethyl isocyanate to give carbamate diastereoisomeric derivatives of (S)-(+)- and (R)-(-)-eliprodil and internal standard; after evaporation of the derivatizing mixture and dissolution of the residue in a small volume of phosphate buffer-acetonitrile (60:40, v/v), an aliquot is injected into a column-switching HPLC system. The derivatized sample extract is purified on a precolumn filled with C8-bonded silica material, which is flushed with acetonitrile-water, then diastereoisomers of eliprodil and the internal standard are automatically transferred by the mobile phase to the analytical column. The analytical column is a C8 type, specially deactivated for basic compounds, the mobile phase is 0.025 M phosphate buffer (pH 2.6)-methanol-acetonitrile (42:2:56) at a flow-rate of 1.2 ml min-1 and fluorimetric detector operating at lambda ex = 275 nm and lambda em = 336 nm is used. The retention times, under these conditions, are about 16 and 17 min for (S)-(+)- and (R)-(-)-eliprodil diastereoisomers, respectively, and about 19 min for the first-eluted diastereoisomer of the internal standard. During the analysis time, the precolumn, reset in a different path from that of the

  4. Switching of charged inverse micelles in non-polar liquids.

    Science.gov (United States)

    Prasad, Manoj; Beunis, Filip; Neyts, Kristiaan; Strubbe, Filip

    2015-11-15

    The electrodynamics of micellar ions in nonpolar liquids are well understood for the case that a voltage is applied or switched off. In this work, the electrodynamics of charged inverse micelles (CIMs) are studied when the applied voltage is switched to the opposite polarity, which is relevant for applications such as electrophoretic displays and liquid toner printing. Transient current measurements are used to characterize the switching of CIMs formed in a solution of surfactant polyisobutylene succinimide in n-dodecane. For reverse voltages with amplitude below 10V the measurements are in good agreement with a drift and diffusion model, confirming the established understanding of CIMs in nonpolar liquids. When the charge content is high, the reversal current shows a characteristic peak which is explained on the basis of dynamic space-charge effects. However, for reverse voltages larger than 10V, the transient currents are influenced by electrohydrodynamic flow in the liquid causing the CIMs to switch faster than predicted by the model. The occurrence of electrohydrodynamic flow is verified by optical tracking of tracer particles. Also, when the polarizing voltage is applied for longer times, an additional current peak emerges which is due to the accumulation of newly generated charges at the electrodes. Copyright © 2015 Elsevier Inc. All rights reserved.

  5. Analysis of Tocopherols by High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    B. Edison

    2009-01-01

    Full Text Available : Gas chromatography is the key technique for organic components and also for tocopherols analysis. High performance liquid chromatography has an important role to take part in applications such as the handling of less usual samples, prevention of degradation of heat sensitive functional groups and for micro preparative purposes. Many approaches for development of improved methods are suggested, especially for reversed phase applications.

  6. Simultaneous determination of amino acids and carbohydrates in culture media of Clostridium thermocellum by valve-switching ion chromatography.

    Science.gov (United States)

    Fa, Yun; Yang, Haiyan; Ji, Chengshuai; Cui, He; Zhu, Xinshu; Du, Juan; Gao, Jun

    2013-10-10

    An improved method for the simultaneous determination of 20 amino acids and 7 carbohydrates using one-valve switching after injection, ion chromatography, and integrated pulsed amperometric detection is proposed. The resolution of the amino acids and carbohydrates in the cation trap column was investigated. In addition, parameters including flow liquid type, flow rate, concentration, and valve-switch timing were optimized. The method is time-saving, effective, and accurate for the simultaneous separation of amino acids and carbohydrates, with a mean correlation coefficient of >0.99 and repeatability of 0.5-4.6% for eight replicates. The method was successfully applied in the analysis of amino acids and carbohydrates in aseptic media and in extracellular culture media of three phenotypes of Clostridium thermocellum. Copyright © 2013 Elsevier B.V. All rights reserved.

  7. Fractionation of fecal neutral steroids by high performance liquid chromatography

    International Nuclear Information System (INIS)

    Jackson, E.M.; Kloss, C.A.; Weintraub, S.T.; Mott, G.E.

    1985-01-01

    Fecal neutral steroids were fractionated by high performance liquid chromatography (HPLC) into three major fractions: 5 beta-H, 3-keto steroids; 5 beta-H, 3 beta-hydroxy steroids; and 5 alpha-H and delta 5-3 beta-hydroxy steroids. This separation was achieved in about 10 minutes, with greater than 97% recovery of standards in each fraction. Gas-liquid chromatographic quantitation of fecal steroids fractionated by either HPLC or thin-layer chromatography gave nearly identical results. A method using both C18 reverse phase and silica HPLC to purify radiolabeled sterols is also described

  8. Liquid Chromatography Applied to Space System

    Science.gov (United States)

    Poinot, Pauline; Chazalnoel, Pascale; Geffroy, Claude; Sternberg, Robert; Carbonnier, Benjamin

    Searching for signs of past or present life in our Solar System is a real challenge that stirs up the curiosity of scientists. Until now, in situ instrumentation was designed to detect and determine concentrations of a wide number of organic biomarkers. The relevant method which was and still is employed in missions dedicated to the quest of life (from Viking to ExoMars) corresponds to the pyrolysis-GC-MS. Along the missions, this approach has been significantly improved in terms of extraction efficiency and detection with the use of chemical derivative agents (e.g. MTBSTFA, DMF-DMA, TMAH…), and in terms of analysis sensitivity and resolution with the development of in situ high-resolution mass spectrometer (e.g. TOF-MS). Thanks to such an approach, organic compounds such as amino acids, sugars, tholins or polycyclic aromatic hydrocarbons (PAHs) were expected to be found. However, while there’s a consensus that the GC-MS of Viking, Huygens, MSL and MOMA space missions worked the way they had been designed to, pyrolysis is much more in debate (Glavin et al. 2001; Navarro-González et al. 2006). Indeed, (1) it is thought to remove low levels of organics, (2) water and CO2 could interfere with the detection of likely organic pyrolysis products, and (3) only low to mid-molecular weight organic molecules can be detected by this technique. As a result, researchers are now focusing on other in situ techniques which are no longer based on the volatility of the organic matter, but on the liquid phase extraction and analysis. In this line, micro-fluidic systems involving sandwich and/or competitive immunoassays (e.g. LMC, SOLID; Parro et al. 2005; Sims et al. 2012), micro-chip capillary electrophoreses (e.g. MOA; Bada et al. 2008), or nanopore-based analysis (e.g. BOLD; Schulze-Makuch et al. 2012) have been conceived for in situ analysis. Thanks to such approaches, molecular biological polymers (polysaccharides, polypeptides, polynucleotides, phospholipids, glycolipids

  9. Determination of sulfonamides in bovine milk with column-switching high performance liquid chromatography using surface imprinted silica with hydrophilic external layer as restricted access and selective extraction material.

    Science.gov (United States)

    Xu, Wenjuan; Su, Shufang; Jiang, Ping; Wang, Huaisong; Dong, Xiangchao; Zhang, Min

    2010-11-12

    A novel restricted access-molecularly imprinted material (RA-MIP) with selectivity for sulfonamides was synthesized using initiator-transfer agent-terminator (iniferter) method, a "living"/controlled radical polymerization technique. The material was prepared by grafting two layers with different functions on the silica support. To perform a "grafting from" polymerization, iniferter was immobilized on the surface of silica. The internal sulfamethazine imprinted polymer and the external poly(glycidyl methacrylate) [poly(GMA)] were then grafted successively. The hydrophilic structures were formed on the external layer of the material by the hydrolysis of the linear poly(GMA) for protein removal. The result has shown that this restricted access-MIP grafted silica (RA-MIP-SG) not only has the selectivity for the template and its analog, but also has the ability of exclusion for bovine serum albumin (BSA). It indicated that the material possesses both properties of molecularly imprinted polymer (MIP) and restricted access material (RAM). Using RA-MIP-SG as pre-column, a column-switching HPLC method was established for the determination of sulfonamides in bovine milk. Direct sample injection was performed in the analysis, which provides a convenient analytical procedure. Good linearity in the range of 2-400 ng mL(-1) (R>0.998) has been obtained for seven sulfonamides in the study. The recoveries of all the analytes at three concentration levels are between 93% and 107% with the RSDsulfonamides in bovine milk by direct injection and column-switching HPLC with good efficiency and reliability. Copyright © 2010 Elsevier B.V. All rights reserved.

  10. Liquid Crystals as Stationary Phases in Chromatography.

    Science.gov (United States)

    Grajek, H; Witkiewicz, Z; Purchała, M; Drzewiński, W

    2016-01-01

    The most correct analysis of the compositions of diverse analytes mixtures is significant for analytical studies in different fields; however, many prevalent analytes cannot be identified employing traditional partition gas chromatographic methods. Thus, the increasing requirements on analytes of isomeric compounds and the problems encountered in their separation demand a study of more diverse analytical systems which are characterised by higher selectivity. Therefore, the selectivity and polarities of various liquid crystals (rod-like, banana-shape, biforked, oxygen, sulphur, nitrogen, and metal containing molecules, Schiff-base, and polymeric dendrimers) employed as liquid crystalline stationary phases (LCSPs) have been discussed from both points of views, namely, their analytical applications and thermodynamic characteristics of infinitely diluted probes with different acceptor-donor properties. Extreme particular effort has been paid to the different interdependencies between the bound up chemical structures of liquid crystal molecules with their different acceptor-donor properties and the connected resolution capabilities in the interpretation of the probe-LCSP systems, on the basis of the [Formula: see text] and [Formula: see text] dependencies, with regard to the LCSP compositions, which have been controlled by the counterbalancing of the enthalpy and entropy factors. The properties of binary systems composed of liquid crystalline poly(propyleneimine) dendrimers-rod-like molecules of liquid crystals and effects of the dendrimer structure, the chemical nature, and molecular size of the non-mesogens on the ability to dissolve in the liquid crystalline phases, have been interpreted. Practical applications of metallomesogenes and chiral stationary phases for analytical separation of different organic substances have also been taken into consideration.

  11. Liquid chromatography and liquid chromatography-mass spectrometry analysis of donepezil degradation products

    Directory of Open Access Journals (Sweden)

    Mladenović Aleksandar R.

    2015-01-01

    Full Text Available This study describes the investigation of degradation products of donepezil (DP using stability indicating RP-HPLC method for determination of donepezil, which is a centrally acting reversible acetylcholinesterase inhibitor. In order to investigate the stability of drug and formed degradation products, a forced degradation study of drug sample and finished product under different forced degradation conditions has been conducted. Donepezil hydrochloride and donepezil tablets were subjected to stress degradation conditions recommended by International Conference on Harmonization (ICH. Donepezil hydrochloride solutions were subjected to acid and alkali hydrolysis, chemical oxidation and thermal degradation. Significant degradation was observed under alkali hydrolysis and oxidative degradation conditions. Additional degradation products were observed under the conditions of oxidative degradation. The degradation products observed during forced degradation studies were monitored using the high performance liquid chromatography (HPLC method developed. The parent method was modified in order to obtain LC-MS compatible method which was used to identify the degradation products from forced degradation samples using high resolution mass spectrometry. The mass spectrum provided the precise mass from which derived molecular formula of drug substance and degradation products formed and proved the specificity of the method unambiguously. [Projekat Ministarstva nauke Republike Srbije, br. 172013

  12. Instrumental liquid chromatography: a practical manual on high-performance liquid chromatographic methods

    National Research Council Canada - National Science Library

    Parris, N. A

    1976-01-01

    Available texts on liquid chromatography have tended to emphasize the developments in the theoretical understanding of the technique and methodology or to list numerous applications, complete with experimental details...

  13. Liquid Chromatography – Mass Spectrometry Method for the ...

    African Journals Online (AJOL)

    Purpose: To develop and validate a simple and selective high performance liquid chromatography photo diode array mass spectrometry (HPLC-PDA-MS/MS) method for simultaneous determination and confirmation of seven major active alkaloids (6-Hydroxy-ß-Carboline-1-carboxylic acid, ß-Carboline-1- carboxylic acid, ...

  14. An optimized gossypol high-performance liquid chromatography

    Indian Academy of Sciences (India)

    A comparative study on gossypol content of various genetic types of pigment glands of cotton varieties was conducted through an optimized high-performance liquid chromatography (HPLC) on a C18 column (4.6 mm × 250 mm, 5 m particle) with methanol–0.5% acetic acid aqueous solution, 90 : 10 (v/v), as mobile phase, ...

  15. Transfer of High Performance Liquid Chromatography with Diode ...

    African Journals Online (AJOL)

    2013-08-22

    Aug 22, 2013 ... 7. Transfer of High Performance Liquid Chromatography with Diode Array Detection. Method for Determination in Serum of Psychotropic drugs. Innocent Hahirwa1,2*, Corinne Charlier2, Charles Karangwa1, Raphaël Denooz2. 1Laboratory of Analysis of Foodstuffs, Drugs, Water and Toxics, University of ...

  16. Characterization of porous silicon integrated in liquid chromatography chips

    NARCIS (Netherlands)

    Tiggelaar, Roald M.; Verdoold, Vincent; Eghbali, H.; Desmet, G.; Gardeniers, Johannes G.E.

    2009-01-01

    Properties of porous silicon which are relevant for use of the material as a stationary phase in liquid chromatography chips, like porosity, pore size and specific surface area, were determined with high-resolution SEM and N2 adsorption–desorption isotherms. For the anodization conditions

  17. Characterisation of cholera toxin by liquid chromatography - Electrospray mass spectrometry

    NARCIS (Netherlands)

    Baar, B.L.M. van; Hulst, A.G.; Wils, E.R.J.

    1999-01-01

    Cholera toxin, one of the toxins that may be generated by various strains of the bacterium Vibrio cholerae, can be considered as a substance possibly used in biological warfare. The possibilities of characterising the toxin by liquid chromatography electrospray mass spectrometry (LC-ES-MS) were

  18. Coupling of column liquid chromatography and Fourier transform infrared spectrometry

    NARCIS (Netherlands)

    Somsen, G.W; Gooijer, C; Velthorst, N.H; Brinkman, U.A Th

    1998-01-01

    This paper provides an extensive overview of the literature on the coupling of column liquid chromatography (LC) and Fourier transform infrared spectrometry (FT-IR). Flow-cell-based FT-IR detection and early solvent-elimination interfaces for LC-FT-IR are discussed in brief. A comprehensive

  19. New Highly-Sensitive Ultra-Performance Liquid Chromatography ...

    African Journals Online (AJOL)

    Purpose: To develop and validate a simple, rapid, sensitive and specific ultraperformance liquid chromatography mass spectrometry method for the quantification of the angiotensin II receptor antagonist, telmisartan (TEL), in human plasma. Methods: After simple protein precipitation using acetonitrile and methanol, TEL and ...

  20. Quantification of Tea Flavonoids by High Performance Liquid Chromatography

    Science.gov (United States)

    Freeman, Jessica D.; Niemeyer, Emily D.

    2008-01-01

    We have developed a laboratory experiment that uses high performance liquid chromatography (HPLC) to quantify flavonoid levels in a variety of commercial teas. Specifically, this experiment analyzes a group of flavonoids known as catechins, plant-derived polyphenolic compounds commonly found in many foods and beverages, including green and black…

  1. Alternative solvents can make preparative liquid chromatography greener

    NARCIS (Netherlands)

    Shen, Y.; Chen, B.; Beek, van T.A.

    2015-01-01

    To make preparative Reversed-Phase High Performance Liquid Chromatography (RP-pHPLC) greener, alternative solvents were considered among others in terms of toxicity, cost, safety, workability, chromatographic selectivity and elution strength. The less toxic solvents ethanol, acetone and ethyl

  2. Determination of Caffeine in Beverages by High Performance Liquid Chromatography.

    Science.gov (United States)

    DiNunzio, James E.

    1985-01-01

    Describes the equipment, procedures, and results for the determination of caffeine in beverages by high performance liquid chromatography. The method is simple, fast, accurate, and, because sample preparation is minimal, it is well suited for use in a teaching laboratory. (JN)

  3. The high performance liquid chromatography (HPLC) analysis of ...

    African Journals Online (AJOL)

    A pilot study was done to determine the stability of the secondary compounds with high performance liquid chromatography (HPLC) after the samples were bleached with ultraviolet (UV) radiation and treated with activated charcoal. The chlorophyll a was successfully degraded with UV radiation in all the samples leaving a ...

  4. An optimized gossypol high-performance liquid chromatography ...

    Indian Academy of Sciences (India)

    A comparative study on gossypol content of various genetic types of pigment glands of cotton varieties was conducted through an optimized high-performance liquid chromatography (HPLC) on a C18 column (4.6 mm × 250 mm, 5 m particle) with methanol–0.5% acetic acid aqueous solution, 90 : 10 (v/v), as mobile phase, ...

  5. Towards early detection of the hydrolytic degradation of poly(bisphenol A)carbonate by hyphenated liquid chromatography and comprehensive two-dimensional liquid chromatography

    NARCIS (Netherlands)

    Coulier, L.; Kaal, E.R.; Hankemeier, Th.

    2006-01-01

    The hydrolytic degradation of poly(bisphenol A)carbonate (PC) has been characterized by various liquid chromatography techniques. Size exclusion chromatography (SEC) showed a significant decrease in molecular mass as a result of hydrolytic degradation, while 'liquid chromatography at critical

  6. Detection of Griseofulvin and Dechlorogriseofulvin by Thin-Layer Chromatography and Gas-Liquid Chromatography

    Science.gov (United States)

    Cole, R. J.; Kirksey, J. W.; Holaday, C. E.

    1970-01-01

    A rapid and accurate method is described for the determination of griseofulvin and dechlorogriseofulvin extracted from Penicillium urticae with chloroform. Thinlayer chromatography was used to tentatively identify griseofulvin or dechlorogriseofulvin, or both. Two gas-liquid chromatographic systems provided additional qualitative information and simultaneous quantitation of the individual compounds. PMID:5415206

  7. Optimizing heterosurface adsorbent synthesis for liquid chromatography

    Science.gov (United States)

    Bogoslovskii, S. Yu.; Serdan, A. A.

    2016-03-01

    The structural and geometric parameters of a silica matrix (SM) for the synthesis of heterosurface adsorbents (HAs) are optimized. Modification is performed by shielding the external surfaces of alkyl-modified silica (AS) using human serum albumin and its subsequent crosslinking. The structural and geometric characteristics of the SM, AS, and HA are measured via low-temperature nitrogen adsorption. It is found that the structural characteristics of AS pores with diameters D 9 nm reduces significantly due to adsorption of albumin. It is concluded that silica gel with a maximum pore size distribution close to 5 nm and a minimal proportion of pores with D > 9 nm is optimal for HA synthesis; this allows us to achieve the greatest similarity between the chromatographic retention parameters for HA and AS. The suitability of the synthesized adsorbents for analyzing drugs in biological fluids through direct sample injection is confirmed by chromatography. It was found that the percentage of the protein fraction detected at the outlet of the chromatographic column is 98%.

  8. Application of genetic algorithms for parameter estimation in liquid chromatography

    International Nuclear Information System (INIS)

    Hernandez Torres, Reynier; Irizar Mesa, Mirtha; Tavares Camara, Leoncio Diogenes

    2012-01-01

    In chromatography, complex inverse problems related to the parameters estimation and process optimization are presented. Metaheuristics methods are known as general purpose approximated algorithms which seek and hopefully find good solutions at a reasonable computational cost. These methods are iterative process to perform a robust search of a solution space. Genetic algorithms are optimization techniques based on the principles of genetics and natural selection. They have demonstrated very good performance as global optimizers in many types of applications, including inverse problems. In this work, the effectiveness of genetic algorithms is investigated to estimate parameters in liquid chromatography

  9. 21 CFR 862.2250 - Gas liquid chromatography system for clinical use.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Gas liquid chromatography system for clinical use... Instruments § 862.2250 Gas liquid chromatography system for clinical use. (a) Identification. A gas liquid chromatography system for clinical use is a device intended to separate one or more drugs or compounds from a...

  10. 21 CFR 862.2260 - High pressure liquid chromatography system for clinical use.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 8 2010-04-01 2010-04-01 false High pressure liquid chromatography system for... Clinical Laboratory Instruments § 862.2260 High pressure liquid chromatography system for clinical use. (a) Identification. A high pressure liquid chromatography system for clinical use is a device intended to separate...

  11. Chromatography

    Science.gov (United States)

    ... that are bonded together. For example, water is a chemical bond of oxygen and hydrogen. Proteins are another type of chemical compound. There are different kinds of chromatography. These include gas, high pressure liquid, or ion ...

  12. Ionic Liquid-Liquid Chromatography: A New General Purpose Separation Methodology.

    Science.gov (United States)

    Brown, Leslie; Earle, Martyn J; Gîlea, Manuela A; Plechkova, Natalia V; Seddon, Kenneth R

    2017-08-10

    Ionic liquids can form biphasic solvent systems with many organic solvents and water, and these solvent systems can be used in liquid-liquid separations and countercurrent chromatography. The wide range of ionic liquids that can by synthesised, with specifically tailored properties, represents a new philosophy for the separation of organic, inorganic and bio-based materials. A customised countercurrent chromatograph has been designed and constructed specifically to allow the more viscous character of ionic liquid-based solvent systems to be used in a wide variety of separations (including transition metal salts, arenes, alkenes, alkanes, bio-oils and sugars).

  13. Low pull-in voltage electrostatic MEMS switch using liquid dielectric

    KAUST Repository

    Zidan, Mohammed A.

    2014-08-01

    In this paper, we present an electrostatic MEMS switch with liquids as dielectric to reduce the actuation voltage. The concept is verified by simulating a lateral dual gate switch, where the required pull-in voltage is reduced by more than 8 times after using water as a dielectric, to become as low as 5.36V. The proposed switch is simulated using COMSOL multiphysics using various liquid volumes to study their effect on the switching performance. Finally, we propose the usage of the lateral switch as a single switch XOR logic gate.

  14. Thin-layer chromatography - liquid chromatography, an ideal supplement demonstrated by the separation of lanthanoids

    International Nuclear Information System (INIS)

    Specker, H.; Hufnagel, A.

    1984-01-01

    All lanthanoids have been separated by thin-layer chromatography (TLC) with short retention times by using a mixture of ether/tetrahydrofurane (THF)/bis-(2-ethylhexyl)-phosphate (HDEHP)/nitric acid. The eluent was empirically tested by synergistic effects. The results have been transferred to high-performance liquid chromatography /HPLC). It was possible to use the same eluent in TLC and HPLC both for the analytical separation of all lanthanoids and for the separation of fission products. The experimental experience gained in HPLC could be applied to the pre-concentration of isotopes in TLC. Both methods excellently supplemented each other in the separation of lanthanoids. (orig.) [de

  15. Applications of Ultra High Performance Liquid Chromatography for Natural Products

    International Nuclear Information System (INIS)

    Rosniza Razali; Hazlina Ahmad Hassali; Azfar Hanif Abd Aziz; Daryl Jesus Arapoc

    2015-01-01

    Ultra high performance liquid chromatography (UHPLC) is a very powerful and versatile chromatographic technique for the separation of natural products in complex matrices, such as crude extracts for quantification or general profiling. The method is widespread and has been adapted to the analysis of a broad range of natural products generally without the need for complex sample preparation. The present paper overviews regarding the UHPLC and its applications for natural products. (author)

  16. High performance liquid chromatography in studies of radiolabeled antibodies

    International Nuclear Information System (INIS)

    Hnatowich, D.J.

    1986-01-01

    High performance liquid chromatography (HPLC) as applied to the separation of antibodies displays the same advantages as in its other applications, namely good resolution accompanied by fast analysis. It is therefore not surprising that many HPLC columns designed for use with antibodies and other proteins are now available commercially. The properties of proteins which provide the separation are size, hydrophobicity, charge and affinity. The features of each are discussed. (author)

  17. Carbon nanotubes-A resin for electrochemically modulated liquid chromatography.

    Science.gov (United States)

    Brammen, Markus; Fraga-García, Paula; Berensmeier, Sonja

    2017-03-01

    Electrochemically modulated liquid chromatography is a special form of ion exchange chromatography in which the separation process is controlled by applying an electric potential to the stationary phase. This form of chromatography has so far only been applied in research studies. The present study shows that multiwalled carbon nanotubes are an effective resin material for an electrochemically modulated chromatography process. The experiments are carried out in a newly designed column that enables the packing of nanomaterials. We investigate the influence of the applied potential on the retention and elution of maleic acid, determine the dynamic binding capacity, and calculate the utilization degree of the electrical charge in the adsorption process. Moreover, the stability of the resin and the membrane over more than 200 working hours are presented. In addition to the stability, their sturdiness and inexpensive price are important qualities that make multiwalled carbon nanotubes interesting for application as the stationary phase in an electrochemically driven process. The investigated chromatography technique represents a promising separation process for future applications as a preparative step in biotechnology as well as other life science fields. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Protein separations using enhanced-fluidity liquid chromatography.

    Science.gov (United States)

    Bennett, Raffeal; Olesik, Susan V

    2017-11-10

    Enhanced-fluidity liquid chromatography (EFLC) methods using methanol/H 2 O/CO 2 and hydrophilic interaction liquid chromatography (HILIC) were explored for the separation of proteins and peptides. EFLC is a separation mode that uses a mobile phase made of conventional solvents combined with liquid carbon dioxide (CO 2 ) in subcritical conditions. The addition of liquid CO 2 enhances diffusivity and decreases viscosity while maintaining mixture polarity, which typically results in reduced time of analysis. TFA additive and elevated temperature were leveraged as key factors in the separation of a 13-analyte intact protein mixture in under 5min. Under these conditions EFLC showed modest improvement in terms of peak asymmetry and analysis time over the competing ACN/H 2 O separation. Protein analytes detected by electrospray ionization - quadrupole time of flight, were shown to be unaffected by the addition of CO 2 in the mobile phase. Herein, the feasibility of separating hydrophilic proteins up to 80kDa (with transferrin) is demonstrated for CO 2 -containing mobile phases. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Comprehensive two-dimensional liquid chromatography and hyphenated liquid chromatography to study the degradation of poly(bisphenol A)carbonate

    NARCIS (Netherlands)

    Coulier, L.; Kaal, E.R.; Hankemeier, T.

    2005-01-01

    Size exclusion chromatography (SEC), gradient polymer elution chromatography (GPEC) and liquid chromatography at critical conditions (LC-CC) have been developed and applied to observe chemical changes in poly(bisphenol A)carbonate (PC) due to hydrolytic degradation. Especially LC-CC appeared to be

  20. Csaba Horváth and preparative liquid chromatography.

    Science.gov (United States)

    Guiochon, Georges

    2005-06-24

    Few chromatographers have been interested in furthering preparative liquid chromatography. The pioneers, Tswett, Kuhn and Lederer, A.J.P. Martin, Tiselius, isolated fractions but as an intermediate step in the analysis of their samples. The progress in electronics and sensors, and in their miniaturization has lead to the paradoxical situation that the analysts never see the transient pure fractions that their detector quantitates. Yet, over the last 25 years, preparative liquid chromatography has become an important industrial process for the separation, the extraction, and/or the purification of many pharmaceuticals or pharmaceutical intermediates, including pure enantiomers, purified peptides and proteins, compounds that are manufactured at the relatively large industrial scale of a few kilograms to several hundred tons per year. This development that has strongly affected the modem pharmaceutical industry is mainly due to the pioneering work of Csaba Horváth. His work in preparative HPLC was critical at both the practical and the theoretical levels. He was the first scientist in modem times to pay serious attention to the relationships between the curvature of the equilibrium isotherms, the competitive nature of nonlinear isotherms, and the chromatographic band profiles of complex mixtures. The thermodynamics of multi-component phase equilibria and mass transfer kinetics in chromatography attracted his interest and were the focus of ground-breaking contributions. He investigated displacement chromatography, an old method invented by Tiselius that Csaba was first to implement in HPLC. This choice was explained by the essential characteristic of displacement chromatography, in that it delivers fractions that can be far more concentrated than the feed. Remarkably, once the basics of nonlinear chromatography had been mastered in his group, most of the applications that were studied by his coworkers dealt with peptides of various sizes and with proteins. Thus, all

  1. Electro-optical switching of liquid crystals of graphene oxide

    Science.gov (United States)

    Song, Jang-Kun

    Electric field effects on aqueous graphene-oxide (GO) dispersions are reviewed in this chapter. In isotropic and biphasic regimes of GO dispersions, in which the inter-particle friction is low, GO particles sensitively respond to the application of electric field, producing field-induced optical birefringence. The electro-optical sensitivity dramatically decreases as the phase transits to the nematic phase; the increasing inter-particle friction hinders the rotational switching of GO particles. The corresponding Kerr coefficient reaches the maximum near the isotropic to biphasic transition concentration, at which the Kerr coefficient is found be c.a. 1:8 · 10-5 mV-2, the highest value ever reported in all Kerr materials. The exceptionally large Kerr effect arises from the Maxwell- Wagner polarization of GO particles with an extremely large aspect ratio and a thick electrical double layer (EDL). The polarization sensitively depends on the ratio of surface and bulk conductivities in dispersions. As a result, low ion concentration in bulk solvent is highly required to achieve a quality electro-optical switching in GO dispersions. Spontaneous vinylogous carboxylic reaction in GO particles produces H+ ions, resulting in spontaneous degradation of electro-optical response with time, hence the removal of residual ions by using a centrifuge cleaning process significantly improves the electro-optical sensitivity. GO particle size is another important parameter for the Kerr coefficient and the response time. The best performance is observed in a GO dispersion with c.a. 0.5 μm mean size. Dielectrophoretic migration of GO particles can be also used to manipulate GO particles in solution. Using these unique features of GO dispersions, one can fabricate GO liquid crystal devices similar to conventional liquid crystal displays; the large Kerr effect allows fabricating a low power device working at extremely low electric fields.

  2. Nanomaterials as stationary phases and supports in liquid chromatography.

    Science.gov (United States)

    Beeram, Sandya R; Rodriguez, Elliott; Doddavenkatanna, Suresh; Li, Zhao; Pekarek, Allegra; Peev, Darin; Goerl, Kathryn; Trovato, Gianfranco; Hofmann, Tino; Hage, David S

    2017-10-01

    The development of various nanomaterials over the last few decades has led to many applications for these materials in liquid chromatography (LC). This review will look at the types of nanomaterials that have been incorporated into LC systems and the applications that have been explored for such systems. A number of carbon-based nanomaterials and inorganic nanomaterials have been considered for use in LC, ranging from carbon nanotubes, fullerenes and nanodiamonds to metal nanoparticles and nanostructures based on silica, alumina, zirconia and titanium dioxide. Many ways have been described for incorporating these nanomaterials into LC systems. These methods have included covalent immobilization, adsorption, entrapment, and the synthesis or direct development of nanomaterials as part of a chromatographic support. Nanomaterials have been used in many types of LC. These applications have included the reversed-phase, normal-phase, ion-exchange, and affinity modes of LC, as well as related methods such as chiral separations, ion-pair chromatography and hydrophilic interaction liquid chromatography. Both small and large analytes (e.g., dyes, drugs, amino acids, peptides and proteins) have been used to evaluate possible applications for these nanomaterial-based methods. The use of nanomaterials in columns, capillaries and planar chromatography has been considered as part of these efforts. Potential advantages of nanomaterials in these applications have included their good chemical and physical stabilities, the variety of interactions many nanomaterials can have with analytes, and their unique retention properties in some separation formats. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. VIII All-Russian symposium on molecular liquid chromatography and capillary electrophoresis. Program. Summary of reports

    International Nuclear Information System (INIS)

    2001-01-01

    Program and summary of reports of the VIII All-Russian symposium on molecular liquid chromatography and capillary electrophoresis are performed. The meeting took place 15-19 October, 2001 in Moscow. Many problems of liquid and ion exchange chromatography, capillary electrophoresis, thin-layer chromatography have been discussed extensively. Reports covering properties of sorbents and devices for chromatography are incorporated in the collection [ru

  4. Screening of drugs and toxic compounds with liquid chromatography-linear ion trap tandem mass spectrometry.

    Science.gov (United States)

    Sauvage, François-Ludovic; Saint-Marcoux, Franck; Duretz, Bénédicte; Deporte, Didier; Lachatre, Gérard; Marquet, Pierre

    2006-09-01

    In clinical and forensic toxicology, general unknown screening is used to detect and identify exogenous compounds. In this study, we aimed to develop a comprehensive general unknown screening method based on liquid chromatography coupled with a hybrid triple-quadrupole linear ion trap mass spectrometer. After solid-phase extraction, separation was performed using gradient reversed-phase chromatography. The mass spectrometer was operated in the information-dependent acquisition mode, switching between a survey scan acquired in the Enhanced Mass Spectrometry mode with dynamic subtraction of background noise and a dependent scan obtained in the enhanced product ion scan mode. The complete cycle time was 1.36 s. A library of 1000 enhanced product ion-tandem mass spectrometry spectra in positive mode and 250 in negative mode, generated using 3 alternated collision tensions during each scan, was created by injecting pure solutions of drugs and toxic compounds. Comparison with HPLC-diode array detection and gas chromatography-mass spectrometry for the analysis of 36 clinical samples showed that linear ion trap tandem mass spectrometry could identify most of the compounds (94% of the total). Some compounds were detected only by 1 of the other 2 techniques. Specific clinical cases highlighted the advantages and limitations of the method. A unique combination of new operating modes provided by hybrid triple-quadrupole linear ion trap mass spectrometers and new software features allowed development of a comprehensive and efficient method for the general unknown screening of drugs and toxic compounds in blood or urine.

  5. Protein Mobility Shifts Contribute to Gel Electrophoresis Liquid Chromatography Analysis.

    Science.gov (United States)

    Carruthers, Nicholas J; Parker, Graham C; Gratsch, Theresa; Caruso, Joseph A; Stemmer, Paul M

    2015-09-01

    Profiling of cellular and subcellular proteomes by liquid chromatography with tandem mass spectrometry (MS) after fractionation by SDS-PAGE is referred to as GeLC (gel electrophoresis liquid chromatography)-MS. The GeLC approach decreases complexity within individual MS analyses by size fractionation with SDS-PAGE. SDS-PAGE is considered an excellent fractionation technique for intact proteins because of good resolution for proteins of all sizes, isoelectric points, and hydrophobicities. Additional information derived from the mobility of the intact proteins is available after an SDS-PAGE fractionation, but that information is usually not incorporated into the proteomic analysis. Any chemical or proteolytic modification of a protein that changes the mobility of that protein in the gel can be detected. The ability of SDS-PAGE to resolve proteins with chemical modifications has not been widely utilized within profiling experiments. In this work, we examined the ability of the GeLC-MS approach to help identify proteins that were modified after a small hairpin RNA-dependent knockdown in an experiment using stable isotope labeling by amino acids in cell culture-based quantitation.

  6. Comparison of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography for the separation of synthetic cathinones.

    Science.gov (United States)

    Carnes, Stephanie; O'Brien, Stacey; Szewczak, Angelica; Tremeau-Cayel, Lauriane; Rowe, Walter F; McCord, Bruce; Lurie, Ira S

    2017-09-01

    A comparison of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography for the separation of synthetic cathinones has been conducted. Nine different mixtures of bath salts were analyzed in this study. The three different chromatographic techniques were examined using a general set of controlled synthetic cathinones as well as a variety of other synthetic cathinones that exist as positional isomers. Overall 35 different synthetic cathinones were analyzed. A variety of column types and chromatographic modes were examined for developing each separation. For the ultra high performance supercritical fluid chromatography separations, analyses were performed using a series of Torus and Trefoil columns with either ammonium formate or ammonium hydroxide as additives, and methanol, ethanol or isopropanol organic solvents as modifiers. Ultra high performance liquid chromatographic separations were performed in both reversed phase and hydrophilic interaction chromatographic modes using SPP C18 and SPP HILIC columns. Gas chromatography separations were performed using an Elite-5MS capillary column. The orthogonality of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography was examined using principal component analysis. For the best overall separation of synthetic cathinones, the use of ultra high performance supercritical fluid chromatography in combination with gas chromatography is recommended. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Purification of flavonoids from licorice using an off-line preparative two-dimensional normal-phase liquid chromatography/reversed-phase liquid chromatography method.

    Science.gov (United States)

    Fan, Yunpeng; Fu, Yanhui; Fu, Qing; Cai, Jianfeng; Xin, Huaxia; Dai, Mei; Jin, Yu

    2016-07-01

    An orthogonal (71.9%) off-line preparative two-dimensional normal-phase liquid chromatography/reversed-phase liquid chromatography method coupled with effective sample pretreatment was developed for separation and purification of flavonoids from licorice. Most of the nonflavonoids were firstly removed using a self-made Click TE-Cys (60 μm) solid-phase extraction. In the first dimension, an industrial grade preparative chromatography was employed to purify the crude flavonoids. Click TE-Cys (10 μm) was selected as the stationary phase that provided an excellent separation with high reproducibility. Ethyl acetate/ethanol was selected as the mobile phase owing to their excellent solubility for flavonoids. Flavonoids co-eluted in the first dimension were selected for further purification using reversed-phase liquid chromatography. Multiple compounds could be isolated from one normal-phase fraction and some compounds with bad resolution in one-dimensional liquid chromatography could be prepared in this two-dimensional system owing to the orthogonal separation. Moreover, this two-dimensional liquid chromatography method was beneficial for the preparation of relatively trace flavonoid compounds, which were enriched in the first dimension and further purified in the second dimension. Totally, 24 flavonoid compounds with high purity were obtained. The results demonstrated that the off-line two-dimensional liquid chromatography method was effective for the preparative separation and purification of flavonoids from licorice. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Simultaneous determination of triple therapy for Helicobacter pylori in human plasma by reversed phase chromatography with online wavelength switching

    Science.gov (United States)

    Ahmed, Sameh; Atia, Noha N.

    2015-02-01

    The infection of gastric mucosa by Helicobacter pylori (HP) is an essential cofactor in the aetiology of gastroduodenal ulcer and gastric carcinoma. Because of the bacterial resistance, combination therapy containing omeprazole (OME), tinidazole (TNZ) and clarithromycin (CLA) is commonly used for eradication of HP. However, the simultaneous determination of the triple therapy in human plasma was not reported. A simple, reproducible, and selective HPLC method was developed for the simultaneous determination of the triple therapy mixture used for management of HP infections in human plasma. An HPLC procedure based on a liquid-liquid extraction, enrichment of the analytes and subsequent reversed-phase chromatography with UV detection was used. To enable sensitive and selective detection, the method involved the use of online wavelength switching detection, with two different detection wavelengths; 280 nm for detection of OME and TNZ and 210 nm for detection of CLA. Separations were performed on C18 analytical column with acetonitrile-10 mM phosphate buffer of pH = 3.0 at flow rate of 1.0 mL min-1. The linear ranges in human plasma were 0.05-10 μg mL-1 with correlation coefficients >0.9990. The detection limits in human plasma were 0.02-0.07 μg mL-1. Validation parameters were assessed in compliance with US-FDA guidelines. The method proved to be valuable for the therapeutic drug monitoring after oral administration of triple therapy tablets.

  9. (Vapour + liquid) equilibria of ternary systems with ionic liquids using headspace gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Mokhtarani, Babak [Chemistry and Chemical Engineering Research Center of Iran, P.O. Box 14335-186, Tehran (Iran, Islamic Republic of); Gmehling, Juergen, E-mail: gmehling@tech.chem.uni-oldenburg.d [Carl von Ossietzky Universitaet Oldenburg, Technische Chemie, D-26111 Oldenburg (Germany)

    2010-08-15

    (Vapour + liquid) equilibrium (VLE) data for the ternary systems (hexane + benzene), (hexane + cyclohexane), (benzene + cyclohexane), and (ethanol + water) with an ionic liquid as entrainer for extractive distillation were measured by headspace gas chromatography. As ionic liquids, 1-hexyl-3-methyl-imidazolium bis (trifluoromethyl-sulfonyl) imide [HMIM][BTI], 1-octyl-3-methyl-imidazolium bis (trifluoromethyl-sulfonyl) imide [OMIM][BTI], 1-octyl-3-methyl-imidazolium trifluoro-methanesulfonate [OMIM][OTF], and 1-butyl-3-methyl-imidazolium trifluoro-methanesulfonate [BMIM][OTF] were used. The experimental data show that the ionic liquids investigated have a great influence on the separation factors of the systems (hexane + benzene), (hexane + cyclohexane), and (benzene + cyclohexane). The experimental data were compared with the predicted results using mod. UNIFAC (Do). The predicted results are in good agreement with the experimental data.

  10. Reduction of silanophilic interactions in liquid chromatography with the use of ionic liquids

    International Nuclear Information System (INIS)

    MarszaII, MichaI Piotr; Baczek, Tomasz; Kaliszan, Roman

    2005-01-01

    A suppression of silanophilic interactions by the selected ionic liquids added to the mobile phase in thin-layer chromatography (TLC) and high-performance liquid chromatography (HPLC) is reported. Acetonitrile was used as the eluent, alone or with various concentrations of water and phosphoric buffer pH 3. Selectivity of the normal (NP) and the reversed (RP) stationary phase material was examined using a series of proton-acceptor basic drugs analytes. The ionic liquids studied appeared to significantly affect analyte retention in NP-TLC, RP-TLC and RP-HPLC systems tested. Consequently, the increased separation selectivity was attained. Due to ionic liquid additives to eluent even analytes could be chromatographed, which were not eluted from the silica-based stationary phase materials with 100% of acetonitrile in the mobile phase. Addition of ionic liquid already in very small concentration (0.5%, v/v) could reduce the amount of acetonitrile used during the optimization of basic analytes separations in TLC and HPLC systems. Moreover, the influence of temperature on the separation of basic analytes was demonstrated and considered in practical HPLC method development

  11. Reduction of silanophilic interactions in liquid chromatography with the use of ionic liquids

    Energy Technology Data Exchange (ETDEWEB)

    MarszaII, MichaI Piotr [Department of Biopharmaceutics and Pharmacodynamics, Medical University of Gdansk, Gen. J. Hallera 107, 80-416 Gdansk (Poland); Baczek, Tomasz [Department of Biopharmaceutics and Pharmacodynamics, Medical University of Gdansk, Gen. J. Hallera 107, 80-416 Gdansk (Poland); Kaliszan, Roman [Department of Biopharmaceutics and Pharmacodynamics, Medical University of Gdansk, Gen. J. Hallera 107, 80-416 Gdansk (Poland)]. E-mail: roman.kaliszan@amg.gda.pl

    2005-08-22

    A suppression of silanophilic interactions by the selected ionic liquids added to the mobile phase in thin-layer chromatography (TLC) and high-performance liquid chromatography (HPLC) is reported. Acetonitrile was used as the eluent, alone or with various concentrations of water and phosphoric buffer pH 3. Selectivity of the normal (NP) and the reversed (RP) stationary phase material was examined using a series of proton-acceptor basic drugs analytes. The ionic liquids studied appeared to significantly affect analyte retention in NP-TLC, RP-TLC and RP-HPLC systems tested. Consequently, the increased separation selectivity was attained. Due to ionic liquid additives to eluent even analytes could be chromatographed, which were not eluted from the silica-based stationary phase materials with 100% of acetonitrile in the mobile phase. Addition of ionic liquid already in very small concentration (0.5%, v/v) could reduce the amount of acetonitrile used during the optimization of basic analytes separations in TLC and HPLC systems. Moreover, the influence of temperature on the separation of basic analytes was demonstrated and considered in practical HPLC method development.

  12. Determination of sulfonamides in butter samples by ionic liquid magnetic bar liquid-phase microextraction high-performance liquid chromatography.

    Science.gov (United States)

    Wu, Lijie; Song, Ying; Hu, Mingzhu; Xu, Xu; Zhang, Hanqi; Yu, Aimin; Ma, Qiang; Wang, Ziming

    2015-01-01

    A novel, simple, and environmentally friendly pretreatment method, ionic liquid magnetic bar liquid-phase microextraction, was developed for the determination of sulfonamides in butter samples by high-performance liquid chromatography. The ionic liquid magnetic bar was prepared by inserting a stainless steel wire into the hollow of a hollow fiber and immobilizing ionic liquid in the micropores of the hollow fiber. In the extraction process, the ionic liquid magnetic bars were used to stir the mixture of sample and extraction solvent and enrich the sulfonamides in the mixture. After extraction, the analyte-adsorbed ionic liquid magnetic bars were readily isolated with a magnet from the extraction system. It is notable that the present method was environmentally friendly since water and only several microliters of ionic liquid were used in the whole extraction process. Several parameters affecting the extraction efficiency were investigated and optimized, including the type of ionic liquid, sample-to-extraction solvent ratio, the number of ionic liquid magnetic bars, extraction temperature, extraction time, salt concentration, stirring speed, pH of the extraction solvent, and desorption conditions. The recoveries were in the range of 73.25-103.85 % and the relative standard deviations were lower than 6.84 %. The experiment results indicated that the present method was effective for the extraction of sulfonamides in high-fat content samples.

  13. Determination of Rocuronium bromide by hydrophilic interaction liquid chromatography (HILIC

    Directory of Open Access Journals (Sweden)

    Natalija Nakov

    2012-01-01

    Full Text Available A new method involving hydrophilic interaction liquid chromatography (HILIC has been developed for determination of rocuronium bromide in presents of its main impurities (impurity A and impurity C, which are also its main degradation products, in solution for injection. The influence of the critical chromatographic parameters such as content of acetonitrile in the mobile phase, ionic strength and pH value of the buffer used in the mobile phase were investigated using the Design of experiments approach (DoE. The mechanism of retention of rocuronium bromide on bare silica column was also investigated. Optimal chromatographic conditions were obtained using mixture of acetonitrile and ammonium formate (107.5mM, pH 7.0 in ratio 90:10 as a mobile phase. The validation results have shown that the method is suitable for determination of rocuronium bromid in solution for injection.

  14. Alcoholic fermentation process control by high-performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Morawski, J.; Dincer, A.K.; Ivie, K.

    1983-02-01

    In large-scale fermentation for energy production high-performance liquid chromatography (HPLC) provides an accurate method of monitoring the original oligosaccharides and polysaccharides, as well as their hydrolysis to fermentable monosaccharides. Also measuring the saccharide and alcohol content of the fermentation vat allows overseeing of the process, providing the capability of allowing the fermentation to proceed to the most economical level prior to distillation. Another application for HPLC in a large-scale fermentation for energy is to analyze the stillage for its ethanol content during distillation, in order to observe the efficiency of the still. HPLC can separate and detect very low levels, (i.e., 100 parts per million), of ethanol to yield information concerning the distillation process. These capabilities indicate that HPLC is an extremely useful efficient instrument to the fermentation industries. (Refs. 2).

  15. A rapid liquid chromatography determination of free formaldehyde in cod.

    Science.gov (United States)

    Storey, Joseph M; Andersen, Wendy C; Heise, Andrea; Turnipseed, Sherri B; Lohne, Jack; Thomas, Terri; Madson, Mark

    2015-01-01

    A rapid method for the determination of free formaldehyde in cod is described. It uses a simple water extraction of formaldehyde which is then derivatised with 2,4-dinitrophenylhydrazine (DNPH) to form a sensitive and specific chromophore for high-performance liquid chromatography (HPLC) detection. Although this formaldehyde derivative has been widely used in past tissue analysis, this paper describes an improved derivatisation procedure. The formation of the DNPH formaldehyde derivative has been shortened to 2 min and a stabilising buffer has been added to the derivative to increase its stability. The average recovery of free formaldehyde in spiked cod was 63% with an RSD of 15% over the range of 25-200 mg kg(-1) (n = 48). The HPLC procedure described here was also compared to a commercial qualitative procedure - a swab test for the determination of free formaldehyde in fish. Several positive samples were compared by both methods.

  16. Micro parallel liquid chromatography: enabling technology for discovery analytical chemistry.

    Science.gov (United States)

    Lemmo, Anthony V; Hobbs, Steve; Patel, Paren

    2004-08-01

    Since the introduction of combinatorial chemistry, compound libraries have undergone a significant increase in size and diversity. The ensuing expansion and diversification of compound libraries have resulted in increased demand for analytical throughput. Following the evolution of new technologies for generating lead compounds and targets and the desire to increase research and development productivity, analytical chemistry is now gaining attention as a bottleneck that would benefit from advances in instrumentation for increased analytical throughput. The commercial introduction of the Veloce trade mark micro parallel liquid chromatography system from Nanostream offers discovery analytical chemists the capability to analyze 24 samples in parallel with as little as 0.5 microl of sample. The system offers a scalable analytical approach to address bottlenecks in historically underserved areas, such as compound library purity screening, as well as higher value-added applications, such as log P determination and aqueous solubility assessment. This article describes the Veloce system and presents representative data from several discovery analytical applications.

  17. Liquid chromatography mass spectrometry for analysis of microbial metabolites

    DEFF Research Database (Denmark)

    Klitgaard, Andreas

    are still to be discovered. The main analytical technique used to investigate production of products from these diverse organisms is liquid-chromatography coupled to mass spectrometry (LC-MS). With the development of new and improved analytical instrumentation for chemical analysis, the time needed...... the recorded LC-MS data and annotate known compounds, a process we have named aggressive dereplication. By overlaying automatically generated extracted-ion chromatograms from detected compounds on the base peak chromatogram, all major potentially novel peaks can be visualized, allowing for fast dereplication...... and methodologies developed during these studies have shown to be very effective and applicable to metabolite analysis of a wide range of microorganisms, and not restricted to fungi. The developed methods have revealed new insights into microbial SMs, and it is clear that even more discoveries can be made using...

  18. Gradient design for liquid chromatography using multi-scale optimization.

    Science.gov (United States)

    López-Ureña, S; Torres-Lapasió, J R; Donat, R; García-Alvarez-Coque, M C

    2018-01-26

    In reversed phase-liquid chromatography, the usual solution to the "general elution problem" is the application of gradient elution with programmed changes of organic solvent (or other properties). A correct quantification of chromatographic peaks in liquid chromatography requires well resolved signals in a proper analysis time. When the complexity of the sample is high, the gradient program should be accommodated to the local resolution needs of each analyte. This makes the optimization of such situations rather troublesome, since enhancing the resolution for a given analyte may imply a collateral worsening of the resolution of other analytes. The aim of this work is to design multi-linear gradients that maximize the resolution, while fulfilling some restrictions: all peaks should be eluted before a given maximal time, the gradient should be flat or increasing, and sudden changes close to eluting peaks are penalized. Consequently, an equilibrated baseline resolution for all compounds is sought. This goal is achieved by splitting the optimization problem in a multi-scale framework. In each scale κ, an optimization problem is solved with N κ  ≈ 2 κ variables that are used to build the gradients. The N κ variables define cubic splines written in terms of a B-spline basis. This allows expressing gradients as polygonals of M points approximating the splines. The cubic splines are built using subdivision schemes, a technique of fast generation of smooth curves, compatible with the multi-scale framework. Owing to the nature of the problem and the presence of multiple local maxima, the algorithm used in the optimization problem of each scale κ should be "global", such as the pattern-search algorithm. The multi-scale optimization approach is successfully applied to find the best multi-linear gradient for resolving a mixture of amino acid derivatives. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Towards Chip Scale Liquid Chromatography and High Throughput Immunosensing

    Energy Technology Data Exchange (ETDEWEB)

    Ni, Jing [Iowa State Univ., Ames, IA (United States)

    2000-09-21

    This work describes several research projects aimed towards developing new instruments and novel methods for high throughput chemical and biological analysis. Approaches are taken in two directions. The first direction takes advantage of well-established semiconductor fabrication techniques and applies them to miniaturize instruments that are workhorses in analytical laboratories. Specifically, the first part of this work focused on the development of micropumps and microvalves for controlled fluid delivery. The mechanism of these micropumps and microvalves relies on the electrochemically-induced surface tension change at a mercury/electrolyte interface. A miniaturized flow injection analysis device was integrated and flow injection analyses were demonstrated. In the second part of this work, microfluidic chips were also designed, fabricated, and tested. Separations of two fluorescent dyes were demonstrated in microfabricated channels, based on an open-tubular liquid chromatography (OT LC) or an electrochemically-modulated liquid chromatography (EMLC) format. A reduction in instrument size can potentially increase analysis speed, and allow exceedingly small amounts of sample to be analyzed under diverse separation conditions. The second direction explores the surface enhanced Raman spectroscopy (SERS) as a signal transduction method for immunoassay analysis. It takes advantage of the improved detection sensitivity as a result of surface enhancement on colloidal gold, the narrow width of Raman band, and the stability of Raman scattering signals to distinguish several different species simultaneously without exploiting spatially-separated addresses on a biochip. By labeling gold nanoparticles with different Raman reporters in conjunction with different detection antibodies, a simultaneous detection of a dual-analyte immunoassay was demonstrated. Using this scheme for quantitative analysis was also studied and preliminary dose-response curves from an immunoassay of a

  20. Recent advances in ultra-high performance liquid chromatography for the analysis of traditional chinese medicine

    Science.gov (United States)

    Traditional Chinese medicines (TCMs) have been widely used for the prevention and treatment of various diseases for thousands of years in China. Ultra Performance Liquid Chromatography (UHPLC) is a relatively new technique offering new possibilities in liquid chromatography. This paper reviews recen...

  1. Investigating the Retention Mechanisms of Liquid Chromatography Using Solid-Phase Extraction Cartridges

    Science.gov (United States)

    O'Donnell, Mary E.; Musial, Beata A.; Bretz, Stacey Lowery; Danielson, Neil D.; Ca, Diep

    2009-01-01

    Liquid chromatography (LC) experiments for the undergraduate analytical laboratory course often illustrate the application of reversed-phase LC to solve a separation problem, but rarely compare LC retention mechanisms. In addition, a high-performance liquid chromatography instrument may be beyond what some small colleges can purchase. Solid-phase…

  2. Analytical method for high resolution liquid chromatography for quality control French Macaw

    International Nuclear Information System (INIS)

    Garcia Penna, Caridad M; Torres Amaro, Leonid; Menendez Castillo, Rosa; Sanchez, Esther; Martinez Espinosa, Vivian; Gonzalez, Maria Lidia; Rodriguez, Carlos

    2007-01-01

    Was developed and validated an analytical method for high resolution liquid chromatography applicable to quality control of drugs dry French Macaw (Senna alata L. Roxb.) With ultraviolet detection at 340 nm. The method for high resolution liquid chromatography used to quantify the sennosides A and B, main components, was validated and proved to be specific, linear, precise and accurate. (Author)

  3. Pressurized liquid extraction followed by liquid chromatography with tandem mass spectrometry to determine pharmaceuticals in mussels.

    Science.gov (United States)

    Núñez, Mireia; Borrull, Francesc; Pocurull, Eva; Fontanals, Núria

    2016-02-01

    An analytical method based on pressurized liquid extraction and solid-phase extraction with a mixed-mode Oasis(®) MAX sorbent as cleanup, followed by liquid chromatography with electrospray ionization and tandem mass spectrometry was developed and validated for the determination of seven widely used pharmaceuticals in mussel species. The optimization of the pressurized liquid extraction and the solid-phase extraction parameters is described. The method provided extraction recoveries ranging from 61 to 90%, and limits of detection ranging from 2 to 50 ng/g (dry weight). The repeatability and reproducibility of the method, expressed as relative standard deviation, were lower than 15 and 19%, respectively. The method was successfully applied to the analysis of mussel samples from different locations. The analyses showed that salicylic acid was present in mussels at concentrations up to 177 ng/g (dry weight). © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. A new A431/cell membrane chromatography and online high performance liquid chromatography/mass spectrometry method for screening epidermal growth factor receptor antagonists from Radix sophorae flavescentis.

    Science.gov (United States)

    Wang, Sicen; Sun, Meng; Zhang, Yanmin; Du, Hui; He, Langchong

    2010-08-06

    The intracellular kinase domains of epidermal growth factor receptor (EGFR) in some tumor cells such as human epidermal squamous cells (A(431) cells) are an important target for drug discovery. We have developed a new A(431)/cell membrane chromatography (A(431)/CMC)-online-high performance liquid chromatography/mass spectrometry (HPLC/MS) method for screening EGFR antagonists from medicinal herbs such as traditional Chinese medicines (TCMs). In this study, A(431) cells with high EGFR expression levels were used to prepare cell membrane stationary phase (CMSP) in an A(431)/CMC model. The retention fractions eluted from the CMSP column were enriched onto an ODS pre-column and then switched into an HPLC/MS system by combining a 10 port columns switching valve. The screening results found that oxymatrine and matrine from Radix sophorae flavescentis (RSF) were the targeted components which could act on EGFR in similar manner of gefitinib as a control drug. There was a good relationship of their inhibiting effects on EGFR secretion and A(431) cell growth in vitro. This new A(431)/CMC-online-HPLC/MS method can be applied for screening EGFR antagonists from TCMs such as RSF. It will be a useful method for drug discovery with natural medicinal herbs as a leading compound resource. Copyright 2010 Elsevier B.V. All rights reserved.

  5. Phytochemical Profile of Erythrina variegata by Using High-Performance Liquid Chromatography and Gas Chromatography-Mass Spectroscopy Analyses

    OpenAIRE

    Suriyavathana Muthukrishnan; Subha Palanisamy; Senthilkumar Subramanian; Sumathi Selvaraj; Kavitha Rani Mari; Ramalingam Kuppulingam

    2016-01-01

    Natural products derived from plant sources have been utilized to treat patients with numerous diseases. The phytochemical constituents present in ethanolic leaf extract of Erythrina variegata (ELEV) were identified by using high-performance liquid chromatography (HPLC) and gas chromatography-mass spectroscopy (GC-MS) analyses. Shade dried leaves were powdered and extracted with ethanol for analyses through HPLC to identify selected flavonoids and through GC-MS to identify other molecules. Th...

  6. Review of online coupling of sample preparation techniques with liquid chromatography.

    Science.gov (United States)

    Pan, Jialiang; Zhang, Chengjiang; Zhang, Zhuomin; Li, Gongke

    2014-03-07

    Sample preparation is still considered as the bottleneck of the whole analytical procedure, and efforts has been conducted towards the automation, improvement of sensitivity and accuracy, and low comsuption of organic solvents. Development of online sample preparation techniques (SP) coupled with liquid chromatography (LC) is a promising way to achieve these goals, which has attracted great attention. This article reviews the recent advances on the online SP-LC techniques. Various online SP techniques have been described and summarized, including solid-phase-based extraction, liquid-phase-based extraction assisted with membrane, microwave assisted extraction, ultrasonic assisted extraction, accelerated solvent extraction and supercritical fluids extraction. Specially, the coupling approaches of online SP-LC systems and the corresponding interfaces have been discussed and reviewed in detail, such as online injector, autosampler combined with transport unit, desorption chamber and column switching. Typical applications of the online SP-LC techniques have been summarized. Then the problems and expected trends in this field are attempted to be discussed and proposed in order to encourage the further development of online SP-LC techniques. Copyright © 2014 Elsevier B.V. All rights reserved.

  7. Determination of Organic Pollutants in Small Samples of Groundwaters by Liquid-Liquid Extraction and Capillary Gas Chromatography

    DEFF Research Database (Denmark)

    Harrison, I.; Leader, R.U.; Higgo, J.J.W.

    1994-01-01

    A method is presented for the determination of 22 organic compounds in polluted groundwaters. The method includes liquid-liquid extraction of the base/neutral organics from small, alkaline groundwater samples, followed by derivatisation and liquid-liquid extraction of phenolic compounds after...... neutralisation. The extracts were analysed by capillary gas chromatography. Dual detection by flame Ionisation and electron capture was used to reduce analysis time....

  8. Liquid chromatography-mass spectrometry in forensic toxicology.

    Science.gov (United States)

    Van Bocxlaer, J F; Clauwaert, K M; Lambert, W E; Deforce, D L; Van den Eeckhout, E G; De Leenheer, A P

    2000-01-01

    Liquid chromatography-mass spectrometry has evolved from a topic of mainly research interest into a routinely usable tool in various application fields. With the advent of new ionization approaches, especially atmospheric pressure, the technique has established itself firmly in many areas of research. Although many applications prove that LC-MS is a valuable complementary analytical tool to GC-MS and has the potential to largely extend the application field of mass spectrometry to hitherto "MS-phobic" molecules, we must recognize that the use of LC-MS in forensic toxicology remains relatively rare. This rarity is all the more surprising because forensic toxicologists find themselves often confronted with the daunting task of actually searching for evidence materials on a scientific basis without any indication of the direction in which to search. Through the years, mass spectrometry, mainly in the GC-MS form, has gained a leading role in the way such quandaries are tackled. The advent of robust, bioanalytically compatible combinations of liquid chromatographic separation with mass spectrometric detection really opens new perspectives in terms of mass spectrometric identification of difficult molecules (e.g., polar metabolites) or biopolymers with toxicological relevance, high throughput, and versatility. Of course, analytical toxicologists are generally mass spectrometry users rather than mass spectrometrists, and this difference certainly explains the slow start of LC-MS in this field. Nevertheless, some valuable applications have been published, and it seems that the introduction of the more universal atmospheric pressure ionization interfaces really has boosted interests. This review presents an overview of what has been realized in forensic toxicological LC-MS. After a short introduction into LC-MS interfacing operational characteristics (or limitations), it covers applications that range from illicit drugs to often abused prescription medicines and some

  9. Confirmatory analysis of acetylgestagens in plasma using liquid chromatography-tandem mass spectrometry

    DEFF Research Database (Denmark)

    Mortensen, Sarah Kelly; Pedersen, Mikael

    2007-01-01

    -assisted liquid-liquid extraction (LLE) on Extrelut NT columns followed by C18 solid-phase extraction (SPE). Analytes were analysed using liquid chromatography-tandem mass spectrometry (I-C-MS/MS), and quantification was performed using matrix-matched calibration standards in combination with deuterated internal...

  10. Investigation of Symphytum cordatum alkaloids by liquid-liquid partitioning, thin-layer chromatography and liquid chromatography-ion-trap mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mroczek, Tomasz [Department of Pharmacognosy with Medicinal Plants Laboratory, Medical University, 1 Chodzki St., 20-093 Lublin (Poland)]. E-mail: tmroczek@pharmacognosy.org; Ndjoko-Ioset, Karine [Laboratoire de Pharmacognosie et Phytochimie, Ecole de Pharmacie Geneve-Lausanne, Universite de Geneve, Quai Ernest-Ansermet 30, CH-1211 Geneva 4 (Switzerland); Glowniak, Kazimierz [Department of Pharmacognosy with Medicinal Plants Laboratory, Medical University, 1 Chodzki St., 20-093 Lublin (Poland); Mietkiewicz-Capala, Agnieszka [Department of Pharmacognosy with Medicinal Plants Laboratory, Medical University, 1 Chodzki St., 20-093 Lublin (Poland); Hostettmann, Kurt [Laboratoire de Pharmacognosie et Phytochimie, Ecole de Pharmacie Geneve-Lausanne, Universite de Geneve, Quai Ernest-Ansermet 30, CH-1211 Geneva 4 (Switzerland)

    2006-05-04

    From the alkalised crude extract of Symphytum cordatum (L.) W.K. roots, pyrrolizidine alkaloids (PAs) were extracted as free tertiary bases and polar N-oxides in a merely one-step liquid-liquid partitioning (LLP) in separation funnel and subsequently pre-fractionated by preparative multiple-development (MD) thin-layer chromatography (TLC) on silica gel plates. In this way three alkaloid fractions of different polarities and retention on silica gel plates were obtained as: the most polar N-oxides of the highest retention, the tertiary bases of medium retention, and diesterified N-oxides of the lowest retention. The former fraction was reduced into free bases by sodium hydrosulfite and purified by LLP on Extrelut-NT3 cartridge. It was further analysed together with the two other fractions by high-performance liquid chromatography (HPLC)-ion-trap mass spectrometry with atmospheric pressure chemical ionization (APCI) interface on XTerra C{sub 18} column using a gradient elution. Based on MS {sup n} spectra, 18 various alkaloids have been tentatively determined for the first time in this plant as the following types of structure: echimidine-N-oxide (three diasteroisomers), 7-sarracinyl-9-viridiflorylretronecine (two diasteroisomers), echimidine (two diasteroisomers), lycopsamine (two diasteroisomers), dihydroechinatine-N-oxide, dihydroheliospathuline-N-oxide, lycopsamine-N-oxide (three diasteroisomers), 7-acetyllycopsamine-N-oxide, symphytine-N-oxide (two diasteroisomers) and 2'',3''-epoxyechiumine-N-oxide.

  11. Investigation of Symphytum cordatum alkaloids by liquid-liquid partitioning, thin-layer chromatography and liquid chromatography-ion-trap mass spectrometry

    International Nuclear Information System (INIS)

    Mroczek, Tomasz; Ndjoko-Ioset, Karine; Glowniak, Kazimierz; Mietkiewicz-Capala, Agnieszka; Hostettmann, Kurt

    2006-01-01

    From the alkalised crude extract of Symphytum cordatum (L.) W.K. roots, pyrrolizidine alkaloids (PAs) were extracted as free tertiary bases and polar N-oxides in a merely one-step liquid-liquid partitioning (LLP) in separation funnel and subsequently pre-fractionated by preparative multiple-development (MD) thin-layer chromatography (TLC) on silica gel plates. In this way three alkaloid fractions of different polarities and retention on silica gel plates were obtained as: the most polar N-oxides of the highest retention, the tertiary bases of medium retention, and diesterified N-oxides of the lowest retention. The former fraction was reduced into free bases by sodium hydrosulfite and purified by LLP on Extrelut-NT3 cartridge. It was further analysed together with the two other fractions by high-performance liquid chromatography (HPLC)-ion-trap mass spectrometry with atmospheric pressure chemical ionization (APCI) interface on XTerra C 18 column using a gradient elution. Based on MS n spectra, 18 various alkaloids have been tentatively determined for the first time in this plant as the following types of structure: echimidine-N-oxide (three diasteroisomers), 7-sarracinyl-9-viridiflorylretronecine (two diasteroisomers), echimidine (two diasteroisomers), lycopsamine (two diasteroisomers), dihydroechinatine-N-oxide, dihydroheliospathuline-N-oxide, lycopsamine-N-oxide (three diasteroisomers), 7-acetyllycopsamine-N-oxide, symphytine-N-oxide (two diasteroisomers) and 2'',3''-epoxyechiumine-N-oxide

  12. Liquid-liquid extraction and liquid chromatography-mass spectrometry detection of curcuminoids from bacterial culture medium.

    Science.gov (United States)

    Tan, Suryani; Rupasinghe, Thusitha W T; Tull, Dedreia L; Augustin, Mary Ann; Gras, Sally L

    2015-04-15

    Liquid chromatography-mass spectrometry (LC-MS) has been used to detect polyphenolic curcuminoids found in turmeric but studies of metabolism by bacterial and mammalian cells in vitro are compromised by poor recovery from the culture medium. We report a liquid-liquid extraction procedure with ethyl acetate and use LC-MS to quantify extracted curcuminoids. Ethyl acetate allows recoveries of ∼ 80-86% of curcuminoids from the bacterial growth medium, bacterial cell lysate and combined bacterial cell and growth medium matrices; a clear improvement over acetonitrile where recoveries were ∼ 25-66%. This optimised method will enable studies of curcuminoid metabolism and may be applicable to other hydrophobic polyphenolic compounds. Copyright © 2015 Elsevier B.V. All rights reserved.

  13. Simultaneous analysis for water- and fat-soluble vitamins by a novel single chromatography technique unifying supercritical fluid chromatography and liquid chromatography.

    Science.gov (United States)

    Taguchi, Kaori; Fukusaki, Eiichiro; Bamba, Takeshi

    2014-10-03

    Chromatography techniques usually use a single state in the mobile phase, such as liquid, gas, or supercritical fluid. Chromatographers manage one of these techniques for their purpose but are sometimes required to use multiple methods, or even worse, multiple techniques when the target compounds have a wide range of chemical properties. To overcome this challenge, we developed a single method covering a diverse compound range by means of a "unified" chromatography which completely bridges supercritical fluid chromatography and liquid chromatography. In our method, the phase state was continuously changed in the following order; supercritical, subcritical and liquid. Moreover, the gradient of the mobile phase starting at almost 100% CO2 was replaced with 100% methanol at the end completely. As a result, this approach achieved further extension of the polarity range of the mobile phase in a single run, and successfully enabled the simultaneous analysis of fat- and water-soluble vitamins with a wide logP range of -2.11 to 10.12. Furthermore, the 17 vitamins were exceptionally separated in 4min. Our results indicated that the use of dense CO2 and the replacement of CO2 by methanol are practical approaches in unified chromatography covering diverse compounds. Additionally, this is a first report to apply the novel approach to unified chromatography, and can open another door for diverse compound analysis in a single chromatographic technique with single injection, single column and single system. Copyright © 2014. Published by Elsevier B.V.

  14. Electrochemically modulated liquid chromatography: Theoretical investigations and applications from the perspectives of chromatography and interfacial electrochemistry

    Energy Technology Data Exchange (ETDEWEB)

    Keller, David W. [Iowa State Univ., Ames, IA (United States)

    2005-01-01

    Electrochemically modulated liquid chromatography (EMLC) employs a conductive material as both a stationary phase for chromatographic separations and as a working electrode for performing electrochemistry experiments. This dual functionality gives EMLC the capacity to manipulate chromatographic separations by changing the potential applied (Eapp) to the stationary phase with respect to an external reference. The ability to monitor retention as a function of Eapp provides a means to chromatographically monitor electrosorption processes at solid-liquid interfaces. In this dissertation, the retention mechanism for EMLC is examined from the perspective of electrical double layer theory and interfacial thermodynamics. From the chromatographic data, it is possible to determine the interfacial excess (Λ) of a solute and changes in interfacial tension (dγ) as a function of both Eapp and the supporting electrolyte concentration. Taken together, these two experimentally manipulated parameters can be examined within the context of the Gibbs adsorption equation to delineate the contribution of a variety of interfacial properties, including the charge of solute on the stationary phase and the potential of zero charge (PZC), to the mechanism behind EMLC-based retention. The chromatographic probing of interfacial phenomena is complemented by electroanalytical experiments that exploit the ability to monitor the electronic current flowing through an EMLC column. Cyclic voltammetry and chronoamperometry of an EMLC column are used to determine the electronic performance characteristics of an EMLC column. An electrochemical flow injection analysis of a column is provided in which the current required to maintain a constant Eapp is monitored and provides a way to examine the influence that acetonitrile and supporting electrolyte composition, flow rate, column backpressure, and ionic strength have on the structure of electrified interfaces.

  15. Determination of triazine herbicides in juice samples by microwave-assisted ionic liquid/ionic liquid dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography.

    Science.gov (United States)

    Su, Rui; Li, Dan; Wu, Lijie; Han, Jing; Lian, Wenhui; Wang, Keren; Yang, Hongmei

    2017-07-01

    A novel microextraction method, termed microwave-assisted ionic liquid/ionic liquid dispersive liquid-liquid microextraction, has been developed for the rapid enrichment and analysis of triazine herbicides in fruit juice samples by high-performance liquid chromatography. Instead of using hazardous organic solvents, two kinds of ionic liquids, a hydrophobic ionic liquid (1-hexyl-3-methylimidazolium hexafluorophosphate) and a hydrophilic ionic liquid (1-butyl-3-methylimidazolium tetrafluoroborate), were used as the extraction solvent and dispersion agent, respectively, in this method. The extraction procedure was induced by the formation of cloudy solution, which was composed of fine drops of 1-hexyl-3-methylimidazolium hexafluorophosphate dispersed entirely into sample solution with the help of 1-butyl-3-methylimidazolium tetrafluoroborate. In addition, an ion-pairing agent (NH 4 PF 6 ) was introduced to improve recoveries of the ionic liquid phase. Several experimental parameters that might affect the extraction efficiency were investigated. Under the optimum experimental conditions, the linearity for determining the analytes was in the range of 5.00-250.00 μg/L, with the correlation coefficients of 0.9982-0.9997. The practical application of this effective and green method is demonstrated by the successful analysis of triazine herbicides in four juice samples, with satisfactory recoveries (76.7-105.7%) and relative standard deviations (lower than 6.6%). In general, this method is fast, effective, and robust to determine triazine herbicides in juice samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Column liquid chromatography-ultraviolet and column liquid chromatography/mass spectrometry evaluation of stress degradation behavior of escitalopram oxalate.

    Science.gov (United States)

    Dhaneshwar, Sunil R; Mahadik, Mahadeo V; Kulkarni, Mahesh J

    2009-01-01

    The objective of this work was to study the degradation behavior of escitalopram oxalate under different International Conference on Harmonization (ICH)-recommended stress conditions by column liquid chromatography (LC)-UV and LC/mass spectrometry (LC/MS) and to establish a validated stability-indicating LC assay method. Escitalopram oxalate was subjected to stress conditions of hydrolysis, oxidation, photolysis, and thermal decomposition. Extensive degradation was found to occur in alkaline medium. Mild degradation was observed in acidic and oxidative conditions. Escitalopram oxalate was stable to neutral, photolytic, and thermal stress. Successful separation of the drug from degradation products formed under stress conditions was achieved on a PerfectSil-100 ODS-3 column [C18 (5 microm, 25 cm x 4.6 mm id)] using methanol-0.01 M acetate buffer pH 3.8 adjusted with acetic acid (45 + 55) as the mobile phase. The flow rate was 1 ml/min, and the detection wavelength was 239 nm. The method was validated according to ICH guidelines. Major degradation products formed in hydrolysis and oxidative conditions were isolated, and structural elucidation of degradation products was done by LCIMS and infrared spectrometry studies. The major hydrolysis degradation product was confirmed as 1-(3-dimethylaminopropyl)-1-(4-fluoro- phenyl)-1,3dihydroisobenzofuran-5-carboxylic acid, and the major oxidative degradation product was confirmed as 1-{[3-dimethylamino(oxide)- propyl]-1-(4-fluro-phenyl)}-1,3-dihydro-isobenzofuran- 5-carbonitrile.

  17. Liquid chromatography-fluorescence and liquid chromatography-mass spectrometry detection of tryptophan degradation products of a recombinant monoclonal antibody.

    Science.gov (United States)

    Nowak, Christine; Ponniah, Gomathinayagam; Cheng, Guilong; Kita, Adriana; Neill, Alyssa; Kori, Yekaterina; Liu, Hongcheng

    2016-03-01

    Light exposure is one of several conditions used to study the degradation pathways of recombinant monoclonal antibodies. Tryptophan is of particular interest among the 20 amino acids because it is the most photosensitive. Tryptophan degradation forms several products, including an even stronger photosensitizer and several reactive oxygen species. The current study reports a specific peptide mapping procedure to monitor tryptophan degradation. Instead of monitoring peptides using UV 214 nm, fluorescence detection with an excitation wavelength of 295 nm and an emission wavelength of 350 nm was used to enable specific detection of tryptophan-containing peptides. Peaks that decreased in area over time are likely to contain susceptible tryptophan residues. This observation can allow further liquid chromatography-mass spectrometry (LC-MS) analysis to focus only on those peaks to confirm tryptophan degradation products. After confirmation of tryptophan degradation, susceptibility of tryptophan residues can be compared based on the peak area decrease. Copyright © 2015 Elsevier Inc. All rights reserved.

  18. Viewing angle switching of liquid crystal display using fringe-field switching to control off-axis phase retardation

    International Nuclear Information System (INIS)

    Lim, Young Jin; Kim, Jin Ho; Her, Jung Hwa; Lee, Seung Hee; Park, Kyoung Ho; Lee, Joun Ho; Kim, Byeong Koo; Kang, Wan-Seok; Lee, Gi-Dong

    2010-01-01

    A viewing angle switchable liquid crystal display associated with fringe-field switching mode is proposed. In the device, one pixel is composed of a main pixel and a sub-pixel, in which both pixels are formed to generate a fringe electric field. However, the field directions are different from each other so that in the main pixel, the fringe field rotates the liquid crystal for displaying the main image, whereas it controls only the tilt angle of the liquid crystal without rotating in the sub-pixel region. In this way, phase retardation to cause leakage of light at the off-normal axis can be generated in the sub-pixel, and by utilizing the light, the main displayed image in the normal direction can be blocked in the oblique viewing direction.

  19. Viewing angle switching of liquid crystal display using fringe-field switching to control off-axis phase retardation

    Energy Technology Data Exchange (ETDEWEB)

    Lim, Young Jin; Kim, Jin Ho; Her, Jung Hwa; Lee, Seung Hee [Polymer BIN Fusion Research Center, Department of Polymer Nano-Science and Technology, Chonbuk National University, Chonju, Chonbuk 561-756 (Korea, Republic of); Park, Kyoung Ho; Lee, Joun Ho; Kim, Byeong Koo [Mobile Product Development Department, LG Display Company, Ltd, Gumi, Gyungbuk 730-350 (Korea, Republic of); Kang, Wan-Seok; Lee, Gi-Dong, E-mail: gdlee@dau.ac.k, E-mail: lsh1@chonbuk.ac.k [Department of Electronics Engineering, Dong-A University, Pusan 604-714 (Korea, Republic of)

    2010-03-03

    A viewing angle switchable liquid crystal display associated with fringe-field switching mode is proposed. In the device, one pixel is composed of a main pixel and a sub-pixel, in which both pixels are formed to generate a fringe electric field. However, the field directions are different from each other so that in the main pixel, the fringe field rotates the liquid crystal for displaying the main image, whereas it controls only the tilt angle of the liquid crystal without rotating in the sub-pixel region. In this way, phase retardation to cause leakage of light at the off-normal axis can be generated in the sub-pixel, and by utilizing the light, the main displayed image in the normal direction can be blocked in the oblique viewing direction.

  20. Determination of maduramicin in feedingstuffs and premixtures by liquid chromatography : development, validation and interlaboratory study

    NARCIS (Netherlands)

    Jong, de J.; Stoisser, B.; Wagner, K.; Tomassen, M.J.H.; Driessen, J.J.M.; Hofman, P.; Putzka, H.A.

    2004-01-01

    A reversed-phase liquid chromatography method for determination of maduramicin in feedingstuffs and premixtures was developed, validated, and interlaboratory studied. The extraction solvent was methanol. Maduramicin was detected at 520 nm after postcolumn derivatization with vanillin. Recovery was

  1. Determination of Aspartame, Caffeine, Saccharin, and Benzoic Acid in Beverages by High Performance Liquid Chromatography.

    Science.gov (United States)

    Delaney, Michael F.; And Others

    1985-01-01

    Describes a simple and reliable new quantitative analysis experiment using liquid chromatography for the determinaiton of caffeine, saccharin, and sodium benzoate in beverages. Background information, procedures used, and typical results obtained are provided. (JN)

  2. Assay for dihydroorotase using high-performance liquid chromatography with radioactivity detection

    International Nuclear Information System (INIS)

    Mehdi, S.; Wiseman, J.S.

    1989-01-01

    An assay for measuring dihydroorotase activity was devised. Radiolabeled substrate and product were separated by high-performance liquid chromatography using a reverse-phase column with ion-pairing, and the radioactivity was quantitated by flow detection

  3. Qualitative and quantitative determination of ubiquinones by the method of high-efficiency liquid chromatography

    International Nuclear Information System (INIS)

    Yanotovskii, M.T.; Mogilevskaya, M.P.; Obol'nikova, E.A.; Kogan, L.M.; Samokhvalov, G.I.

    1986-01-01

    A method has been developed for the qualitative and quantitative determination of ubiquinones CoQ 6 -CoQ 10 , using high-efficiency reversed-phase liquid chromatography. Tocopherol acetate was used as the internal standard

  4. Liquid chromatography-mass spectrometry coupling by the intermediary of a liquid micro chromatography-electro spray interface; Couplage chromatographie liquide-spectrometrie de masse par l`intermediaire d`une interface electrospray-microchromatographie liquide

    Energy Technology Data Exchange (ETDEWEB)

    Gillard Factor, C.

    1996-12-06

    The objective of this work is to realize a liquid chromatography- mass spectrometry coupling by the intermediary of an electro spray interface and the evaluation of performances of tis analytical tool to study pollutants in water, and more particularly pesticides whom maximum admissible concentration in a table water is 0.1{mu}g/l. This study has allowed to bring to the fore the interest of the ionization mode by electro spray in a LC/MS coupling to identify and quantify pesticides in the state of traces without treating the sample. Then, it was demonstrated the usefulness of this analytical tool to detect high molecular masses molecules. (N.C.)

  5. Tryptophan and kynurenine determination in human hair by liquid chromatography.

    Science.gov (United States)

    Dario, Michelli F; Freire, Thamires Batello; Pinto, Claudinéia Aparecida Sales de Oliveira; Prado, María Segunda Aurora; Baby, André R; Velasco, Maria Valéria R

    2017-10-15

    Tryptophan, an amino acid found in hair proteinaceous structure is used as a marker of hair photodegradation. Also, protein loss caused by several chemical/physical treatments can be inferred by tryptophan quantification. Kynurenine is a photo-oxidation product of tryptophan, expected to be detected when hair is exposed mainly to UVB (290-320nm) radiation range. Tryptophan from hair is usually quantified directly as a solid or after alkaline hydrolysis, spectrofluorimetrically. However, these types of measure are not sufficiently specific and present several interfering substances. Thus, this work aimed to propose a quantification method for both tryptophan and kynurenine in hair samples, after alkali hydrolysis process, by using high-performance liquid chromatography (HPLC) with fluorimetric and UV detection. The tryptophan and kynurenine quantification method was developed and validated. Black, white, bleached and dyed (blond and auburn) hair tresses were used in this study. Tryptophan and kynurenine were separated within ∼9min by HPLC. Both black and white virgin hair samples presented similar concentrations of tryptophan, while bleaching caused a reduction in the tryptophan content as well as dyeing process. Unexpectedly, UV/vis radiation did not promote significantly the conversion of tryptophan into its photo-oxidation product and consequently, kynurenine was not detected. Thus, this works presented an acceptable method for quantification of tryptophan and its photooxidation metabolite kynurenine in hair samples. Also, the results indicated that bleaching and dyeing processes promoted protein/amino acids loss but tryptophan is not extensively degraded in human hair by solar radiation. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. An efficient hydrophilic interaction liquid chromatography separation of 7 phospholipid classes based on a diol column

    NARCIS (Netherlands)

    Zhu, C.; Dane, A.; Spijksma, G.; Wang, M.; Greef, J. van der; Luo, G.; Hankemeier, T.; Vreeken, R.J.

    2012-01-01

    A hydrophilic interaction liquid chromatography (HILIC) - ion trap mass spectrometry method was developed for separation of a wide range of phospholipids. A diol column which is often used with normal phase chromatography was adapted to separate different phospholipid classes in HILIC mode using a

  7. Surface-enhanced resonance Raman spectroscopy as an identification tool in column liquid chromatography

    NARCIS (Netherlands)

    Seifar, R.M.; Altelaar, M.A.F.; Dijkstra, R.J.; Ariese, F.; Brinkman, U.A.T.; Gooijer, C.

    2000-01-01

    The compatibility of ion-pair reversed-phase column liquid chromatography and surface-enhanced resonance Raman spectroscopy (SERRS) for separation and identification of anionic dyes has been investigated, with emphasis on the at-line coupling via a thin-layer chromatography (TLC) plate. SERR spectra

  8. Study of high performance liquid chromatography fingerprint for traditional chinese medicine yigongningxue oral liquid

    International Nuclear Information System (INIS)

    Feng, C.; Ruan, J.L.

    2010-01-01

    A simple, reliable and accurate fingerprinting method has been developed for quality control of YiGongNingXue oral liquid. The separation was done by reverse phase chromatography using Zorbax eclipse XDB C/sub 18/ column (250mmx4.6mmi. d. with 5.0 micro m particle size) and detection at 246nm. Methanol (5-95 % in 70 min)-buffer solution (water-phosphorica cid, pH 3.0, 95-0 percent in 70 min) as mobile phase for linear gradient elution. The flow rate was 1.0 mLmin/sup 1/ and the column temperature was at 25 deg. C. The similarity of 20 batches of YGNX oral liquid was more than 90 %. Also 15 common peaks of chromatogram have been detected, ten of them were identified by comparing fingerprint chromatogram with reference substances The HPLC fingerprint can be used to control the quality of YiGongNingXue oral liquid. (author)

  9. Chromatography.

    Science.gov (United States)

    Brantley, L. Reed, Sr.; Demanche, Edna L.; Klemm, E. Barbara; Kyselka, Will; Phillips, Edwin A.; Pottenger, Francis M.; Yamamoto, Karen N.; Young, Donald B.

    This booklet presents some activities on chromatography. Directions for preparing leaf pigment extracts using alcohol are given, and paper chromatography and thin-layer chromatography are described as modifications of the basic principles of chromatography. (KHR)

  10. Development of an on-line mixed-mode gel liquid chromatography×reversed phase liquid chromatography method for separation of water extract from Flos Carthami.

    Science.gov (United States)

    Wang, Yu-Qing; Tang, Xu; Li, Jia-Fu; Wu, Yun-Long; Sun, Yu-Ying; Fang, Mei-Juan; Wu, Zhen; Wang, Xiu-Min; Qiu, Ying-Kun

    2017-10-13

    A novel on-line comprehensive two-dimensional liquid chromatography (2D-LC) method by coupling mixed-mode gel liquid chromatography (MMG-LC) with reversed phase liquid chromatography (RPLC) was developed. A mixture of 17 reference compounds was used to study the separation mechanism. A crude water extract of Flos Carthami was applied to evaluate the performance of the novel 2D-LC system. In the first dimension, the extract was eluted with a gradient of water/methanol over a cross-linked dextran gel Sephadex LH-20 column. Meanwhile, the advantages of size exclusion, reversed phase partition and adsorption separation mechanism were exploited before further on-line reversed phase purification on the second dimension. This novel on-line mixed-mode Sephadex LH-20×RPLC method provided higher peak resolution, sample processing ability (2.5mg) and better orthogonality (72.9%) versus RPLC×RPLC and hydrophilic interaction liquid chromatography (HILIC)×RPLC. To the best of our knowledge, this is the first report of a mixed-mode Sephadex LH-20×RPLC separation method with successful applications in on-line mode, which might be beneficial for harvesting targets from complicated medicinal plants. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Evaluation of a silicon oxynitride hydrophilic interaction liquid chromatography column in saccharide and glycoside separations.

    Science.gov (United States)

    Wan, Huihui; Sheng, Qianying; Zhong, Hongmin; Guo, Xiujie; Fu, Qing; Liu, Yanfang; Xue, Xingya; Liang, Xinmiao

    2015-05-01

    The retention characteristics of a silicon oxynitride stationary phase for carbohydrate separation were studied in hydrophilic interaction chromatography mode. Four saccharides including mono-, di-, and trisaccharides were employed to investigate the effects of water content and buffer concentration in the mobile phase on hydrophilic interaction liquid chromatography retention. For the tested saccharides, the silicon oxynitride column demonstrated excellent performance in terms of separation efficiency, hydrophilicity, and interesting separation selectivity for carbohydrates compared to the bare silica stationary phase. Finally, the silicon oxynitride hydrophilic interaction liquid chromatography column was employed in the separation of complex samples of fructooligosaccharides, saponins, and steviol glycoside from natural products. The resulting chromatograms demonstrated good separation efficiency and longer retention compared with silica, which further confirmed the advantages and potential application of silicon oxynitride stationary phase for hydrophilic interaction liquid chromatography separation. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Characterization of synthetic dyes by comprehensive two-dimensional liquid chromatography combining ion-exchange chromatography and fast ion-pair reversed-phase chromatography.

    Science.gov (United States)

    Pirok, Bob W J; Knip, Jitske; van Bommel, Maarten R; Schoenmakers, Peter J

    2016-03-04

    In the late 19th century, newly invented synthetic dyes rapidly replaced the natural dyes on the market. The characterization of mixtures of these so-called early synthetic dyes is complicated through the occurrence of many impurities and degradation products. Conventional one-dimensional liquid chromatography does not suffice to obtain fingerprints with sufficient resolution and baseline integrity. Comprehensive two-dimensional liquid chromatography (LC×LC) is employed in this study, with ion-exchange chromatography in the first dimension and fast ion-pair liquid chromatography in the second. Retention in the first dimension is largely determined by the number of charges, while the selection of a small ion-pair reagent (tetramethylammonium hydroxide) in the second dimension causes retention to be largely determined by the molecular structure of the dye. As a result, there is a high degree of orthogonality of the two dimensions, similar to the values typically encountered in GC×GC. The proposed LC×LC method shows a theroretical peak capacity of about 2000 in an analysis time of about three hours. Clear, informative fingerprints are obtained that open a way to a more efficient characterization of dyes used in objects of cultural heritage. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Preparation and evaluation of surface-bonded tricationic ionic liquid silica as stationary phases for high-performance liquid chromatography.

    Science.gov (United States)

    Qiao, Lizhen; Shi, Xianzhe; Lu, Xin; Xu, Guowang

    2015-05-29

    Two tricationic ionic liquids were prepared and then bonded onto the surface of supporting silica materials through "thiol-ene" click chemistry as new stationary phases for high-performance liquid chromatography. The obtained columns of tricationic ionic liquids were evaluated respectively in the reversed-phase liquid chromatography (RPLC) mode and hydrophilic interaction liquid chromatography (HILIC) mode, and possess ideal column efficiency of 80,000 plates/m in the RPLC mode with naphthalene as the test solute. The tricationic ionic liquid stationary phases exhibit good hydrophobic and shape selectivity to hydrophobic compounds, and RPLC retention behavior with multiple interactions. In the HILIC mode, the retention and selectivity were evaluated through the efficient separation of nucleosides and bases as well as flavonoids, and the typical HILIC retention behavior was demonstrated by investigating retention changes of hydrophilic solutes with water volume fraction in mobile phase. The results show that the tricationic ionic liquid columns possess great prospect for applications in analysis of hydrophobic and hydrophilic samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. Graphitized carbon in gas-liquid-solid chromatography and gas chromatography/mass spectrometric analysis of high boiling hydrocarbon mixtures

    International Nuclear Information System (INIS)

    Ciccioli, P.; Hayes, J.M.; Rinaldi, G.; Denson, K.B.; Meinschein, W.G.

    1979-01-01

    Gas--liquid--solid chromatography (GLSC) employing a poly(phenyl ether) (PPE 20) liquid phase on graphitized carbon black (GCB) is applicable to the analyses of crude oils and distillates of sedimentary rocks. The elution of C 4 to C 40 hydrocarbons which consist of n-alkanes, isoprenoid-type alkanes, steranes, olefins, and aromatic hydrocarbons can be handled in a single GC run. A GLSC column in tandem with a mass spectrometer provides an excellent means for the identification of geochemically significant organic compounds in complex natural mixtures. 8 figures, 4 tables

  15. Analysis of chlorpheniramine in human urine samples using dispersive liquid-liquid microextraction combined with high-performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Mehdi Maham

    2014-09-01

    Full Text Available A simple and environmentally friendly microextraction technique was used for determination of chlorpheniramine (CPM, an antihistamine drug, in human urine samples using dispersive liquid-liquid microextraction (DLLME followed by high performance liquid chromatography with diode array detection (HPLC-DAD. In this extraction technique, an appropriate mixture of acetonitrile (disperser solvent and carbon tetrachloride (extraction solvent was rapidly injected into the urine sample containing the target analyte. Tiny droplets of extractant were formed and dispersed into the sample solution and then sedimented at the bottom of the conical test tube by centrifugation. Under optimal conditions, the calibration curve was linear in the range of 0.055-5.5 µg mL-1, with a detection limit of 16.5 ng mL-1. This proposed method was successfully applied to the analysis of real urine samples. Low consumption of toxic organic solvents, simplicity of operation, low cost and acceptable figures of merit are the main advantages of the proposed technique.

  16. High-performance liquid chromatography analysis methods developed for quantifying enzymatic esterification of flavonoids in ionic liquids

    DEFF Research Database (Denmark)

    Lue, Bena-Marie; Guo, Zheng; Xu, X.B.

    2008-01-01

    Methods using reversed-phase high-performance liquid chromatography (RP-HPLC) with ELSD were investigated to quantify enzymatic reactions of flavonoids with fatty acids in the presence of diverse room temperature ionic liquids (RTILs). A buffered salt (preferably triethylamine-acetate) was found ...... developed was successfully applied for primary screening of RTILs (> 20), with in depth evaluation of substrates in 10 RTILs, for their evaluation as reaction media....

  17. Light-driven chiral molecular switches or motors in liquid crystals.

    Science.gov (United States)

    Wang, Yan; Li, Quan

    2012-04-17

    The ability to tune molecular self-organization with an external stimulus is a main driving force in the bottom-up nanofabrication of molecular devices. Light-driven chiral molecular switches or motors in liquid crystals that are capable of self-organizing into optically tunable helical superstructures undoubtedly represent a striking example, owing to their unique property of selective light reflection and which may lead to applications in the future. In this review, we focus on different classes of light-driven chiral molecular switches or motors in liquid crystal media for the induction and manipulation of photoresponsive cholesteric liquid crystal systems and their consequent applications. Moreover, the change of helical twisting powers of chiral dopants and their capability of helix inversion in the induced cholesteric phases are highlighted and discussed in the light of their molecular geometric changes. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Frequency-dependent dielectric contribution of flexoelectricity allowing control of state switching in helicoidal liquid crystals.

    Science.gov (United States)

    Outram, B I; Elston, S J

    2013-07-01

    The contribution of flexoelectric polarization to the dielectric susceptibility in helicoidal liquid crystals is formulated for the static equilibrium case, and further in the case of a time-varying field. A dispersion of the dielectric permittivity due to the frequency response of flexoelectric switching is described. The special case of a negative dielectric-anisotropy nematic material is considered and experimentally shown to agree with the analytical theory. It is further demonstrated how relaxation of the flexoelectric contribution to the dielectric tensor in this special case can be exploited to switch between states in cholesteric liquid crystal structures by altering the applied time-dependent field amplitude, if Δε-Δεε(0). Consequentially, a versatile mechanism for driving between states in liquid crystal systems has been demonstrated and its implications for technology are suggested, and include dual-mode, bistable, and transflective displays.

  19. Frequency-dependent dielectric contribution of flexoelectricity allowing control of state switching in helicoidal liquid crystals

    Science.gov (United States)

    Outram, B. I.; Elston, S. J.

    2013-07-01

    The contribution of flexoelectric polarization to the dielectric susceptibility in helicoidal liquid crystals is formulated for the static equilibrium case, and further in the case of a time-varying field. A dispersion of the dielectric permittivity due to the frequency response of flexoelectric switching is described. The special case of a negative dielectric-anisotropy nematic material is considered and experimentally shown to agree with the analytical theory. It is further demonstrated how relaxation of the flexoelectric contribution to the dielectric tensor in this special case can be exploited to switch between states in cholesteric liquid crystal structures by altering the applied time-dependent field amplitude, if Δɛ-Δɛɛ0. Consequentially, a versatile mechanism for driving between states in liquid crystal systems has been demonstrated and its implications for technology are suggested, and include dual-mode, bistable, and transflective displays.

  20. Comprehensive two-dimensional liquid chromatography for polyphenol analysis in foodstuffs.

    Science.gov (United States)

    Cacciola, Francesco; Farnetti, Sara; Dugo, Paola; Marriott, Philip John; Mondello, Luigi

    2017-01-01

    Polyphenols are a class of plant secondary metabolites that are recently drawing a special interest because of their broad spectrum of pharmacological effects. As they are characterized by an enormous structural variability, the identification of these molecules in food samples is a difficult task, and sometimes having only a limited number of commercially available reference materials is not of great help. One-dimensional liquid chromatography is the most widely applied analytical approach for their analysis. In particular, the hyphenation of liquid chromatography to mass spectrometry has come to play an influential role by allowing relatively fast tentative identification and accurate quantification of polyphenolic compounds at trace levels in vegetable media. However, when dealing with very complex real-world food samples, a single separation system often does not provide sufficient resolving power for attaining rewarding results. Comprehensive two-dimensional liquid chromatography is a technique of great analytical impact, since it offers much higher peak capacities than separations in a single dimension. In the present review, we describe applications in the field of comprehensive two-dimensional liquid chromatography for polyphenol analysis in real-world food samples. Comprehensive two-dimensional liquid chromatography applications to nonfood matrices fall outside the scope of the current report and will not be discussed. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Isolation and purification of six iridoid glycosides from gardenia jasminoides fruit by medium-pressure liquid chromatography combined with macroporous resin chromatography.

    Science.gov (United States)

    Wang, Yun; Liu, Hui; Shen, Lifeng; Yao, Lan; Ma, Yinlian; Yu, Dingrong; Chen, Jianhong; Li, Puling; Chen, Ying; Zhang, Cun

    2015-12-01

    Gardeniae fructus is one of the most frequently used herbs in traditional Chinese medicine. In the present study, a process for the enrichment of six iridoid glycosides from Gardeniae fructus was developed using medium-pressure liquid chromatography combined with macroporous resin and reversed-phase chromatography. The purities of different fractions from Gardeniae fructus were assessed using quantitative high-performance liquid chromatography. After fractionation using HPD-100 column chromatography, a 30% ethanol fraction was selected based on high-performance liquid chromatography and liquid chromatography with mass spectrometry qualitative analysis to separate and purify. Based on the orientation analysis results, six compounds-deacetyl asperulosidic acid methyl ester, gardenoside, ixoroside, scandoside methyl ester, genipin-1-O-β-d-gentiobioside, and geniposide-were successfully isolated and purified in three to four combined steps from Gardeniae fructus. The purities of these compounds were found by high-performance liquid chromatography analysis to be 97.9, 98.1, 95.5, 96.3, 97.1, and 98.7%, respectively. Moreover, their structures were elucidated by NMR spectroscopy and liquid chromatography with tandem mass spectrometry. The separation process was highly efficient, rapid, and accurate, making it a potential approach for the large-scale production of iridoids in the laboratory and providing several marker compounds for quality control. This procedure may be meaningful for the purification of other natural products used in traditional Chinese medicine. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. New Highly-Sensitive Ultra-Performance Liquid Chromatography ...

    African Journals Online (AJOL)

    chromatography mass spectrometry method for the quantification of the angiotensin II receptor antagonist, telmisartan (TEL), in human ... spectrometry with positive ion mode. The ion transitions recorded in multiple reaction monitoring mode ..... application of UPLC in pharmaceutical analysis. Talanta 2006; 68(3): 908-918.

  3. Screening and quantitative determination of twelve acidic and neutral pharmaceuticals in whole blood by liquid-liquid extraction and liquid chromatography-tandem mass spectrometry

    DEFF Research Database (Denmark)

    Simonsen, Kirsten Wiese; Steentoft, Anni; Buck, Maike

    2010-01-01

    . The method was fully validated for salicylic acid, paracetamol, phenobarbital, carisoprodol, meprobamate, topiramate, etodolac, chlorzoxazone, furosemide, ibuprofen, warfarin, and salicylamide. The method also tentatively includes thiopental, theophylline, piroxicam, naproxen, diclophenac, and modafinil......We describe a multi-method for simultaneous identification and quantification of 12 acidic and neutral compounds in whole blood. The method involves a simple liquid-liquid extraction, and the identification and quantification are performed using liquid chromatography-tandem mass spectrometry...

  4. Application of liquid column chromatography to preconcentration, separation and determination of platinum metals

    International Nuclear Information System (INIS)

    Alimarin, I.P.; Basova, E.M.; Bol'shova, T.A.; Ivanov, V.M.

    1986-01-01

    Separation and determination of platimum metals using the methods of adsorption, ion-pair, ion-exchange, distributing and sieve chromatography are discussed in the review of literature in 1971-1984. Separation and determination of metals as chelates using the method of adsorption and ion-pair chromatograpy are noted to be most perspective directions of developing highly effective liquid chromatography of inorganic systems

  5. Immunoaffinity chromatography of abscisic acid combined with electrospray liquid chromatography–mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Hradecká, Veronika; Novák, Ondřej; Havlíček, Libor; Strnad, Miroslav

    2007-01-01

    Roč. 847, č. 2 (2007), s. 162-173 ISSN 1570-0232 R&D Projects: GA MŠk(CZ) LC06034; GA AV ČR IBS5038351 Institutional research plan: CEZ:AV0Z50380511 Source of funding: V - iné verejné zdroje ; V - iné verejné zdroje Keywords : abscisic acid * immunoaffinity chromatography * liquid chromatography-mass spectrometry Subject RIV: ED - Physiology Impact factor: 2.935, year: 2007

  6. Characterization of natural organic colorants in historical and art objects by high-performance liquid chromatography.

    Science.gov (United States)

    Pauk, Volodymyr; Barták, Petr; Lemr, Karel

    2014-12-01

    High-performance liquid chromatography plays an important role in analysis of historical organic colorants. A number of papers have been published in this field over the last 30 years. Classification of the most commonly used natural dyes and an overview of high-performance liquid chromatography methods with main focus on recent works (2008 to the beginning of 2014) are provided. The review deals with an entire analytical protocol covering sample preparation, chromatographic separation, and suitable detection (UV/visible and fluorescent spectroscopy and mass spectrometric techniques). High-performance liquid chromatography has been successfully used in the complete characterization of some organic dyestuffs present in historical and art objects. The possibilities and difficulties for identification of natural sources of historical colorants are also discussed. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Voltage-Controlled Switching of Strong Light-Matter Interactions using Liquid Crystals.

    Science.gov (United States)

    Hertzog, Manuel; Rudquist, Per; Hutchison, James A; George, Jino; Ebbesen, Thomas W; Börjesson, Karl

    2017-12-22

    We experimentally demonstrate a fine control over the coupling strength of vibrational light-matter hybrid states by controlling the orientation of a nematic liquid crystal. Through an external voltage, the liquid crystal is seamlessly switched between two orthogonal directions. Using these features, for the first time, we demonstrate electrical switching and increased Rabi splitting through transition dipole moment alignment. The C-N str vibration on the liquid crystal molecule is coupled to a cavity mode, and FT-IR is used to probe the formed vibropolaritonic states. A switching ratio of the Rabi splitting of 1.78 is demonstrated between the parallel and the perpendicular orientation. Furthermore, the orientational order increases the Rabi splitting by 41 % as compared to an isotropic liquid. Finally, by examining the influence of molecular alignment on the Rabi splitting, the scalar product used in theoretical modeling between light and matter in the strong coupling regime is verified. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Preparation and chromatographic evaluation of a newly designed steviol glycoside modified-silica stationary phase in hydrophilic interaction liquid chromatography and reversed phase liquid chromatography.

    Science.gov (United States)

    Liang, Tu; Fu, Qing; Shen, Aijin; Wang, Hui; Jin, Yu; Xin, Huaxia; Ke, Yanxiong; Guo, Zhimou; Liang, Xinmiao

    2015-04-03

    A diterpene glycoside compound, rebaudioside A (commonly abbreviated as RA), was immobilized onto porous silica surface through "thiol-ene" click chemistry strategy. The successful immobilization of the RA on the silica support was confirmed by FT-IR and elemental analysis. Chromatographic characteristics of the new stationary phase, named Click TE-RA, were evaluated by a set of diverse analytes such as carbohydrates, nucleosides, and organic acids in hydrophilic interaction liquid chromatography (HILIC) mode. The effects of water content, buffer pH and concentration were investigated and a typical HILIC retention feature of Click TE-RA was observed at high organic modifier content. The Click TE-RA stationary phase was further studied by a series of glycoside compounds. Tunable retention mechanisms from hydrophilic to hydrophobic interactions were observed. Separation of very polar compounds including oligosaccharides, nucleic acid bases and nucleosides using Click TE-RA in HILIC mode was successfully accomplished. In addition, separation of saponins both in HILIC and reversed-phase liquid chromatography (RPLC) modes was performed, demonstrating the presence of orthogonality between two different modes on Click TE-RA column. The multiple interactions induced by polar sugar group and hydrophobic aglycone group allowed this Click TE-RA to serve as a multi-mode stationary phase in two-dimensional liquid chromatography. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. Redox-switched amphiphilic ionic liquid behavior in aqueous solution.

    Science.gov (United States)

    Chamiot, Bénédicte; Rizzi, Cécile; Gaillon, Laurent; Sirieix-Plénet, Juliette; Lelièvre, Joël

    2009-02-03

    A new redox amphiphilic ionic liquid (AIL) containing ferrocene as a redox-active group was synthesized, 1-(11-ferrocenylundecyl)-3-methylimidazolium bromide (Fc11MIm+). Adsorption and aggregation of both reduced and oxidized forms of this ferrocenated AIL in aqueous solution were studied by surface tension measurements. The micellization was favored for the reduced ferrocenated AIL (Fc11MIm+) as compared with the oxidized ferrocenated AIL (Fc+11MIm+). Minimum areas at the air/aqueous solution interface were identical whereas limiting surface tensions were slightly different. This corroborated the formation of an expanded monolayer of redox active AIL at the interface. The electrochemical behavior of redox active AIL was investigated. The electrochemical responses of Fc11MIm+ aqueous solution interestingly differed, depending on its concentration. Below the cmc, the electrochemical reaction was dominated by ferrocenated AIL adsorbed onto the electrode surface; then above the cmc, it was controlled by the Fc11MIm+ diffusing to the electrode. For the latter, the electrochemical mechanism was suggested to couple with the disruption reaction of the reduced form micelles.

  10. Lidar Electro-Optic Beam Switch with a Liquid Crystal Variable Retarder

    Science.gov (United States)

    Baer, James

    2012-01-01

    A document discusses a liquid crystal variable retarder, an electro-optic element that changes the polarization of an optical beam in response to a low-voltage electronic signal. This device can be fabricated so that the element creates, among other states, a half-wave of retardance that can be reduced to a very small retardance. When aligned to a polarized source, this can act to rotate the polarization by 90 in one state, but generate no rotation in the other state. If the beam is then incident on a polarization beam splitter, it will efficiently switch from one path to the other when the voltage is applied. The laser beam switching system has no moving parts, improving reliability over mechanical switching. It is low cost, tolerant of high laser power density, and needs only simple drive electronics, minimizing the required system resources.

  11. Determination of statin drugs in hospital effluent with dispersive liquid-liquid microextraction and quantification by liquid chromatography.

    Science.gov (United States)

    Martins, Ayrton F; Frank, Carla da S; Altissimo, Joseline; de Oliveira, Júlia A; da Silva, Daiane S; Reichert, Jaqueline F; Souza, Darliana M

    2017-08-24

    Statins are classified as being amongst the most prescribed agents for treating hypercholesterolaemia and preventing vascular diseases. In this study, a rapid and effective liquid chromatography method, assisted by diode array detection, was designed and validated for the simultaneous quantification of atorvastatin (ATO) and simvastatin (SIM) in hospital effluent samples. The solid phase extraction (SPE) of the analytes was optimized regarding sorbent material and pH, and the dispersive liquid-liquid microextraction (DLLME), in terms of pH, ionic strength, type and volume of extractor/dispersor solvents. The performance of both extraction procedures was evaluated in terms of linearity, quantification limits, accuracy (recovery %), precision and matrix effects for each analyte. The methods proved to be linear in the concentration range considered; the quantification limits were 0.45 µg L -1 for ATO and 0.75 µg L -1 for SIM; the matrix effect was almost absent in both methods and the average recoveries remained between 81.5-90.0%; and the RSD values were <20%. The validated methods were applied to the quantification of the statins in real samples of hospital effluent; the concentrations ranged from 18.8 µg L -1 to 35.3 µg L -1 for ATO, and from 30.3 µg L -1 to 38.5 µg L -1 for SIM. Since the calculated risk quotient was ≤192, the occurrence of ATO and SIM in hospital effluent poses a potential serious risk to human health and the aquatic ecosystem.

  12. Comprehensive Profiling of Phytohormones in Honey by Sequential Liquid-Liquid Extraction Coupled with Liquid Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Wang, Qing; Cai, Wen-Jing; Yu, Lei; Ding, Jun; Feng, Yu-Qi

    2017-01-25

    Honey exhibits various nutritional and medicinal functions, which are highly related to the active components; thus, the exploration of new compounds in honey is of great importance. Because honey is a byproduct of flower nectar, which is rich in phytohormones, the existence of phytohormones in honey is anticipated. In this research, a method for comprehensive profiling of 49 phytohormones in honey was developed by sequential liquid-liquid extraction (LLE) coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS). Good linearities for 49 phytohormones were obtained with correlation coefficients (R) larger than 0.9913. The limits of detection (LODs) were in the range of 0.2-628.2 pg/mL. Satisfied reproducibility and reliability were achieved by evaluation of the intra- and interday precisions with relative standard deviations (RSDs) less than 15.8% and relative recoveries ranging from 80.4 to 123.7%. The method was further applied to analyze the phytohormones in 14 monofloral raw honey samples and 3 commercial honey samples. The existence of 34 phytohormones was confirmed, including 14 cytokinins (CKs), 8 gibberellins (GAs), 5 brassinosteroids (BRs), indole-3-acetic acid (IAA), indole-3-butyric acid (IBA), abscisic acid (ABA), salicylic acid (SA), jasmonic acid (JA), jasmonoyl-leucine (JA-Leu), and jasmonoyl-phenylalanine (JA-Phe). In addition, the content and species of phytohormones varies in different kinds of honey. The study is beneficial to fully illustrate the phytohormone profile of honey and contributive to elucidate the mechanism of its nutritional and medicinal functions.

  13. Analysis of drugs of abuse in human plasma by dispersive liquid-liquid microextraction and high-performance liquid chromatography.

    Science.gov (United States)

    Fernández, P; Regenjo, M; Bermejo, A M; Fernández, A M; Lorenzo, R A; Carro, A M

    2015-04-01

    Opioids and cocaine are widely used at present, both for recreational purposes and as drugs of abuse. This raises the need to develop new analytical methods specifically designed for the simultaneous detection of several drugs of abuse in biological samples. In this work, dispersive liquid-liquid microextraction (DLLME) was assessed as a new sample treatment for the simultaneous extraction of morphine (MOR), 6-acetylmorphine (6AM), cocaine (COC), benzoylecgonine (BZE) and methadone (MET) from human plasma. Preliminary assays were done before developing an experimental design based on a Uniform Network Doehlert which allowed the optimum extraction conditions to be identified, namely: a volume of extractant solvent (chloroform) and dispersant solvent (acetonitrile) of 220 µl and 3.2 ml, respectively; 0.2 g of NaCl as a salting-out additive; pH 10.6 and ultrasound stirring for 3.5 min. The resulting extracts were analyzed by high-performance liquid chromatography with photodiode array detection (HPLC-PDA), using an XBridge® RP18 column (250 × 4.6 mm i.d., 5 µm particle size). Calibration graphs were linear over the concentration range 0.1-10 µg ml⁻¹, and detection limits ranged from 13.9 to 28.5 ng ml⁻¹. Precision calculated at three different concentration levels in plasma was included in the range 0.1-6.8% RSD. Recoveries of the five drugs were all higher than 84% on average. Finally the proposed method was successfully applied to 22 plasma samples from heroin, cocaine and/or methadone users, and the most frequently detected drug was benzoylecgonine, followed by methadone, cocaine and morphine. Copyright © 2014 John Wiley & Sons, Ltd.

  14. Bacterial Cell Wall Precursor Phosphatase Assays Using Thin-layer Chromatography (TLC) and High Pressure Liquid Chromatography (HPLC).

    Science.gov (United States)

    Pazos, Manuel; Otten, Christian; Vollmer, Waldemar

    2018-03-20

    Peptidoglycan encases the bacterial cytoplasmic membrane to protect the cell from lysis due to the turgor. The final steps of peptidoglycan synthesis require a membrane-anchored substrate called lipid II, in which the peptidoglycan subunit is linked to the carrier lipid undecaprenol via a pyrophosphate moiety. Lipid II is the target of glycopeptide antibiotics and several antimicrobial peptides, and is degraded by 'attacking' enzymes involved in bacterial competition to induce lysis. Here we describe two protocols using thin-layer chromatography (TLC) and high pressure liquid chromatography (HPLC), respectively, to assay the digestion of lipid II by phosphatases such as Colicin M or the LXG toxin protein TelC from Streptococcus intermedius . The TLC method can also monitor the digestion of undecaprenyl (pyro)phosphate, whereas the HPLC method allows to separate the di-, mono- or unphosphorylated disaccharide pentapeptide products of lipid II.

  15. Time-resolved sign-dependent switching in a hybrid aligned nematic liquid crystal cell

    International Nuclear Information System (INIS)

    Taphouse, T S; Cornford, S L; Birkett, J E; Sambles, J R

    2008-01-01

    An optical waveguide technique is used to determine the director tilt profile across a hybrid aligned nematic (HAN) liquid crystal cell, in which the optical response is dependent on the sign of the applied voltage. Two physical models are shown that fit the equilibrium experimental data, but with alternative explanations for this sign dependence. Models with either a flexoelectric coefficient of 2.25x10 -11 C m -1 or a bound surface charge of 12.2 μC m -2 are shown that fit this equilibrium data. In an attempt to resolve this degeneracy sign-dependent switching data are analysed. However, neither model can explain these switching data, which are affected by slow transients of ∼100 ms which are believed to be due to the motion of free ions in the liquid crystal. From the form of these slow transients, it is suggested that the equilibrium position of the ions is next to a cell substrate

  16. Lipidomic analysis of biological samples: Comparison of liquid chromatography, supercritical fluid chromatography and direct infusion mass spectrometry methods.

    Science.gov (United States)

    Lísa, Miroslav; Cífková, Eva; Khalikova, Maria; Ovčačíková, Magdaléna; Holčapek, Michal

    2017-11-24

    Lipidomic analysis of biological samples in a clinical research represents challenging task for analytical methods given by the large number of samples and their extreme complexity. In this work, we compare direct infusion (DI) and chromatography - mass spectrometry (MS) lipidomic approaches represented by three analytical methods in terms of comprehensiveness, sample throughput, and validation results for the lipidomic analysis of biological samples represented by tumor tissue, surrounding normal tissue, plasma, and erythrocytes of kidney cancer patients. Methods are compared in one laboratory using the identical analytical protocol to ensure comparable conditions. Ultrahigh-performance liquid chromatography/MS (UHPLC/MS) method in hydrophilic interaction liquid chromatography mode and DI-MS method are used for this comparison as the most widely used methods for the lipidomic analysis together with ultrahigh-performance supercritical fluid chromatography/MS (UHPSFC/MS) method showing promising results in metabolomics analyses. The nontargeted analysis of pooled samples is performed using all tested methods and 610 lipid species within 23 lipid classes are identified. DI method provides the most comprehensive results due to identification of some polar lipid classes, which are not identified by UHPLC and UHPSFC methods. On the other hand, UHPSFC method provides an excellent sensitivity for less polar lipid classes and the highest sample throughput within 10min method time. The sample consumption of DI method is 125 times higher than for other methods, while only 40μL of organic solvent is used for one sample analysis compared to 3.5mL and 4.9mL in case of UHPLC and UHPSFC methods, respectively. Methods are validated for the quantitative lipidomic analysis of plasma samples with one internal standard for each lipid class. Results show applicability of all tested methods for the lipidomic analysis of biological samples depending on the analysis requirements

  17. Experimental study on (vapor + liquid) equilibria of ternary systems of hydrocarbons/ionic liquid using headspace gas chromatography

    International Nuclear Information System (INIS)

    Mokhtarani, Babak; Valialahi, Leila; Heidar, Kurosh Tabar; Mortaheb, Hamid Reza; Sharifi, Ali; Mirzaei, Mojtaba

    2012-01-01

    Highlights: ► The ionic liquid [Omim][SCN] is considered as an appropriate entrainer for separation of five binary hydrocarbon systems. ► VLE data for the ternary systems consisting [Omim][SCN] and hydrocarbons were measured using headspace gas chromatography. ► The experimental VLE data are correlated using the thermodynamic model of NRTL with a good accuracy. ► The experimental results are compared with the VLE data using other ionic liquids as the entrainer. ► [Omim][SCN] can significantly improve the separation factors of these systems. - Abstract: (Vapor + liquid) equilibrium (VLE) data for ternary systems of (hexane + benzene), (hexane + cyclohexane), (benzene + cyclohexane), (1-hexene + cyclohexane), and (1-hexene + benzene) with an ionic liquid were measured by headspace gas chromatography. The applied ionic liquid 1-methyl 3-octylimidazolium thiocyanate, [Omim][SCN], acts as an entrainer. The comparison of the measured VLE data with the equilibrium data for the binary mixtures without ionic liquid show that [Omim][SCN] significantly improves the separation factor of these systems. The NRTL thermodynamic model is applied for correlating the experimental data. The modeling results show the NRTL model can correlate the experimental data with a good accuracy.

  18. Buffer-Free High Performance Liquid Chromatography Method for ...

    African Journals Online (AJOL)

    Purpose: To develop and validate a simple, economical and reproducible high performance liquid chromatographic (HPLC) method for the determination of theophylline in pharmaceutical dosage forms. Method: Caffeine was used as the internal standard and reversed phase C-18 column was used to elute the drug and ...

  19. Application in pesticide analysis: Liquid chromatography - A review of the state of science for biomarker discovery and identification

    Science.gov (United States)

    Book Chapter 18, titled Application in pesticide analysis: Liquid chromatography - A review of the state of science for biomarker discovery and identification, will be published in the book titled High Performance Liquid Chromatography in Pesticide Residue Analysis (Part of the C...

  20. Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

    NARCIS (Netherlands)

    Moerdijk-Poortvliet, T.C.W.; Schierbeek, H.; Houtekamer, M.; van Engeland, T.; Derrien, D.; Stal, L.J.; Boschker, H.T.S.

    2015-01-01

    Rationale: We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of δ13C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence,

  1. Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

    NARCIS (Netherlands)

    Moerdijk-Poortvliet, T.C.W.; Schierbeek, H.; Houtekamer, M.; van Engeland, T.; Derrien, D.; Stal, L.J.; Boschker, H.T.S.

    2015-01-01

    We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of d13C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence, although

  2. Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

    NARCIS (Netherlands)

    Moerdijk-Poortvliet, Tanja C. W.; Schierbeek, Henk; Houtekamer, Marco; van Engeland, Tom; Derrien, Delphine; Stal, Lucas J.; Boschker, Henricus T. S.

    2015-01-01

    We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of δ(13)C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence, although

  3. The analysis of aqueous mixtures using liquid chromatography-electrospray mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Johnson, Steven [Iowa State Univ., Ames, IA (United States)

    1999-02-12

    The focus of this dissertation is the use of chromatographic methods coupled with electrospray mass spectrometry (ES-MS) for the determination of both organic and inorganic compounds in aqueous solutions. The combination of liquid chromatography (LC) methods and ES-MS offers one of the foremost methods for determining compounds in complex aqueous solutions. In this work, LC-ES-MS methods are devised using ion exclusion chromatography, reversed phase chromatography, and ion exchange chromatography, as well as capillary electrophoresis (CE). For an aqueous sample, these LC-ES-MS and CE-ES-MS techniques require no sample preparation or analyte derivatization, which makes it possible to observe a wide variety of analytes as they exist in solution. The majority of this work focuses on the use of LC-ES-MS for the determination of unknown products and intermediates formed during electrochemical incineration (ECI), an experimental waste remediation process. This report contains a general introduction to the project and the general conclusions. Four chapters have been removed for separate processing. Titles are: Chapter 2: Determination of small carboxylic acids by ion exclusion chromatography with electrospray mass spectrometry; Chapter 3: Electrochemical incineration of benzoquinone in aqueous media using a quaternary metal oxide electrode in the absence of a soluble supporting electrolyte; Chapter 4: The determination of electrochemical incineration products of 4-chlorophenol by liquid chromatography-electrospray mass spectrometry; and Chapter 5: Determination of small carboxylic acids by capillary electrophoresis with electrospray mass spectrometry.

  4. Hydrophilic Interaction Liquid Chromatography: ESI–MS/MS of Plasmalogen Phospholipids from Pectinatus Bacterium

    Czech Academy of Sciences Publication Activity Database

    Řezanka, Tomáš; Siřišťová, L.; Matoulková, D.; Sigler, Karel

    2011-01-01

    Roč. 46, č. 8 (2011), 765-780 ISSN 0024-4201 R&D Projects: GA MŠk 1M0570 Institutional research plan: CEZ:AV0Z50200510 Keywords : Plasmalogens * Pectinatus * Liquid chromatography-electrospray tandem mass spectrometry Subject RIV: EE - Microbiology, Virology Impact factor: 2.129, year: 2011

  5. Quantification and validation of ertapenem using a liquid chromatography-tandem mass spectrometry method

    NARCIS (Netherlands)

    van Rijn, S.P.; Wessels, A.M.A.; Greijdanus, B.; Touw, D.J.; Alffenaar, J.W.C.

    Ertapenem, a carbapenem, relies on time-dependent killing. Therapeutic drug monitoring (TDM) should be considered, when ertapenem is used in specific populations, to achieve optimal bactericidal activity and optimize drug-dosing regimens. No validated liquid chromatography-tandem mass spectrometry

  6. Determination of Bedaquiline in Human Serum Using Liquid Chromatography-Tandem Mass Spectrometry

    NARCIS (Netherlands)

    Alffenaar, Jan-Willem C.; Bolhuis, Mathieu; van Hateren, Kai; Sturkenboom, Marieke; Akkerman, Onno; de Lange, Wiel; Greijdanus, Ben; van der Werf, Tjip; Touw, Daan

    Bedaquiline, a diarylquinoline for the treatment of multidrug-resistant tuberculosis (TB), relies on exposure-dependent killing. As data on drug exposure in specific populations are scarce, pharmacokinetic studies may be of interest. No simple and robust validated liquid chromatography-tandem mass

  7. Alternative sample-introduction technique to avoid breakthrough in gradient-elution liquid chromatography of polymers

    NARCIS (Netherlands)

    Reingruber, E.; Bedani, F.; Buchberger, W.; Schoenmakers, P.

    2010-01-01

    Gradient-elution liquid chromatography (GELC) is a powerful tool for the characterization of synthetic polymers. However, gradient-elution chromatograms often suffer from breakthrough phenomena. Breakthrough can be averted by using a sample solvent as weak as the mobile phase. However, this approach

  8. Deformation and degradation of polymers in ultra-high-pressure liquid chromatography

    NARCIS (Netherlands)

    Uliyanchenko, E.; van der Wal, S.; Schoenmakers, P.J.

    2011-01-01

    Ultra-high-pressure liquid chromatography (UHPLC) using columns packed with sub-2 μm particles has great potential for separations of many types of complex samples, including polymers. However, the application of UHPLC for the analysis of polymers meets some fundamental obstacles. Small particles

  9. Determination of Peroxide-Based Explosives Using Liquid Chromatography with On-Line Infrared Detection

    NARCIS (Netherlands)

    Schulte-Ladbeck, Rasmus; Edelmann, Andrea; Quintas, Guillermo; Lendl, Bernhard; Karst, U.

    2006-01-01

    A nondestructive analytical method for peroxide-based explosives determination in solid samples is described. Reversed-phase high-performance liquid chromatography in combination with on-line Fourier transform infrared (FT-IR) detection is used for the analysis of triacetonetriperoxide (TATP) and

  10. Arsenic speciation by liquid chromatography coupled with ionspray tandem mass spectrometry

    DEFF Research Database (Denmark)

    Corr, J. J.; Larsen, Erik Huusfeldt

    1996-01-01

    Ionspray mass spectrometry, a well established organic analysis technique, has been coupled to high-performance liquid chromatography for speciation of organic arsenic compounds, The ionspray source and differentially pumped interface of the mass spectrometer were operated in dual modes for eleme...

  11. Characterization of typical chemical background interferences in atmospheric pressure ionization liquid chromatography-mass spectrometry

    NARCIS (Netherlands)

    Guo, Xinghua; Bruins, Andries P.; Covey, Thomas R.

    2006-01-01

    The structures and origins of typical chemical background noise ions in positive atmospheric pressure ionization liquid chromatography/mass spectrometry (API LC/MS) are investigated and summarized in this study. This was done by classifying chemical background ions using precursor and product ion

  12. Separation of enzymically active bovine cytochrome c oxidase monomers and dimers by high performance liquid chromatography

    NARCIS (Netherlands)

    Hakvoort, T. B.; Sinjorgo, K. M.; van Gelder, B. F.; Muijsers, A. O.

    1985-01-01

    The aggregation state of two types of bovine heart cytochrome c oxidase preparations in the presence of laurylmaltoside was investigated by high performance liquid chromatography in two buffers of ionic strengths of 388 mM and 45 mM, respectively. At high ionic strength, it was found that the Fowler

  13. High-performance liquid chromatography determination of dapsone, monoacetyldapsone, and pyrimethamine in filter paper blood spots

    DEFF Research Database (Denmark)

    Rønn, A M; Lemnge, M M; Angelo, H R

    1995-01-01

    A high-performance liquid chromatography method for the simultaneous analysis of dapsone (DDS), the major metabolite of DDS, monoacetyldapsone (MADDS), and pyrimethamine (PYR) was modified for capillary blood samples obtained by finger prick and dried on filter paper. Limit of quantitation using...

  14. Benzoin Condensation: Monitoring a Chemical Reaction by High-Pressure Liquid Chromatography

    Science.gov (United States)

    Bhattacharya, Apurba; Purohit, Vikram C.; Bellar, Nicholas R.

    2004-01-01

    High-pressure liquid chromatography (HPLC) is the preferred method of separating a variety of materials in complex mixtures such as pharmaceuticals, polymers, soils, food products and biological fluids and is also considered to be a powerful analytical tool in both academia and industry. The use of HPLC analysis as a means of monitoring and…

  15. Determination of organophosphorus acids by thermo-spray liquid chromatography-mass spectrometry

    NARCIS (Netherlands)

    Wils, E.R.J.; Hulst, A.G.

    1988-01-01

    The determination of thirteen organophosphorus acids, hydrolysis products of nerve agents and pesticides, by a combination of ion-pair liquid chromatography on a reversed-phase C18 column and thermospray mass spectrometry was investigated. Ammonium acetate and three tetraalkylammonium salts with

  16. Extraction and Purification of Glucoraphanin by Preparative High-Performance Liquid Chromatography (HPLC)

    Science.gov (United States)

    Lee, Iris; Boyce, Mary C.

    2011-01-01

    A student activity that focuses on the isolation of glucoraphanin from broccoli using preparative high-performance liquid chromatography (HPLC) is presented here. Glucoraphanin is a glucosinolate, whose byproducts are known to possess anticancer properties. It is present naturally at high levels in broccoli and other "Brassica" vegetables. This…

  17. A liquid chromatography-mass spectrometry-based metabolome database for tomato

    NARCIS (Netherlands)

    Moco, S.I.A.; Bino, R.J.; Vorst, O.F.J.; Verhoeven, H.A.; Groot, de J.C.W.; Beek, van T.A.; Vervoort, J.J.M.; Vos, de C.H.

    2006-01-01

    For the description of the metabolome of an organism, the development of common metabolite databases is of utmost importance. Here we present the Metabolome Tomato Database (MoTo DB), a metabolite database dedicated to liquid chromatography-mass spectrometry (LC-MS)- based metabolomics of tomato

  18. High resolution full scan liquid chromatography mass spectrometry comprehensive screening in sports antidoping urine analysis

    NARCIS (Netherlands)

    Abushareeda, Wadha; Vonaparti, Ariadni; Saad, Khadija Al; Almansoori, Moneera; Meloug, Mbarka; Saleh, Amal; Aguilera, Rodrigo; Angelis, Yiannis; Horvatovich, Peter L.; Lommen, Arjen; Alsayrafi, Mohammed; Georgakopoulos, Costas

    2018-01-01

    The aim of this paper is to present the development and validation of a high-resolution full scan (HR-FS) electrospray ionization (ESI) liquid chromatography coupled to quadrupole Orbitrap mass spectrometer (LC/Q/Orbitrap MS) platform for the screening of prohibited substances in human urine

  19. Determination for Synthesis and Content of Tetrahydropalmatine Based on High Performance Liquid Chromatography

    OpenAIRE

    Yuanming Zhang

    2014-01-01

    Tetrahydropalmatine is a kind of food additive with useful medicine value (dietary supplement), the tetrahydropalmatine synthetic process by using high performance liquid chromatography method was researched in the study, the experiments show that the dissolution rate of active ingredients in the tetrahydropalmatine water extract synthesized by this method has increased and the amount of active ingredient has greatly improved.

  20. Column liquid chromatography- mass spectrometry: selected techniques in environmental applications for polar pesticides and related compounds.

    NARCIS (Netherlands)

    Slobodnik, J.; van Baar, B.L.M.; Brinkman, U.A.T.

    1995-01-01

    A review covering the field of environmental applications of liquid chromatography-mass spectrometry (LC-MS) is presented. Recent developments and advances are discussed with emphasis on the presently popular thermospray, particle beam and atmospheric pressure ionisation interfaces. Each interface

  1. Improving Separation Performance and Detection Capabilities in Liquid Chromatography Using Active Flow Technology: A Review

    NARCIS (Netherlands)

    Camenzuli, M.; Shalliker, R.A.

    2015-01-01

    The development of sub-2-mu m particles, core shell particles, and monolithic columns has improved separation performance in liquid chromatography (LC) over the past 20 years. However, a key limitation that still prevents LC columns from reaching their full potential is the heterogeneity in the flow

  2. Simultaneous quantitative analysis of metabolites using ion-pair liquid chromatography-electrospray ionization mass spectrometry

    NARCIS (Netherlands)

    Coulier, L.; Bas, R.; Jespersen, S.; Verheij, E.; Werf, M.J. van der; Hankemeier, T.

    2006-01-01

    We have developed an analytical method, consisting of ion-pair liquid chromatography coupled to electrospray ionization mass spectrometry (IP-LC-ESI-MS), for the simultaneous quantitative analysis of several key classes of polar metabolites, like nucleotides, coenzyme A esters, sugar nucleotides,

  3. A Laboratory Experiment in Pharmaceutical Analysis: Analysis of Diazepam Tablets by High Pressure Liquid Chromatography

    Science.gov (United States)

    Bailey, Leonard

    1978-01-01

    The experiment described was developed for the third-year course in inorganic and analytical pharmaceutical chemistry to provide students with "hands-on" experience with high pressure liquid chromatography. Assay procedures are given along with experimental parameters and student results. (LBH)

  4. An on-line high performance liquid chromatography-crocin bleaching assay for detection of antioxidants

    NARCIS (Netherlands)

    Bountagkidou, O.; Klift, van der E.J.C.; Tsimidou, M.Z.; Ordoudi, S.A.; Beek, van T.A.

    2012-01-01

    An on-line HPLC (high performance liquid chromatography) method for the rapid screening of individual antioxidants in mixtures was developed using crocin as a substrate (i.e. oxidation probe) and 2,2'-azobis(2-amidinopropane dihydrochloride (AAPH)) in phosphate buffer (pH 7.5) as a radical

  5. High-Performance Liquid Chromatography in the Undergraduate Chemical Engineering Laboratory

    Science.gov (United States)

    Frey, Douglas D.; Guo, Hui; Karnik, Nikhila

    2013-01-01

    This article describes the assembly of a simple, low-cost, high-performance liquid chromatography (HPLC) system and its use in the undergraduate chemical engineering laboratory course to perform simple experiments. By interpreting the results from these experiments students are able to gain significant experience in the general method of…

  6. Simulated Moving Bed Chromatography: Separation and Recovery of Sugars and Ionic Liquid from Biomass Hydrolysates

    Science.gov (United States)

    Caes, Benjamin R.; Van Oosbree, Thomas R.; Lu, Fachuang; Ralph, John; Maravelias, Christos T.

    2015-01-01

    Simulated moving bed chromatography, a continuous separation method, enables the nearly quantitative recovery of sugar products and ionic liquid solvent from chemical hydrolysates of biomass. The ensuing sugars support microbial growth, and the residual lignin from the process is intact. PMID:23939991

  7. Novel approach to determine ghrelin analogs by liquid chromatography with mass spectrometry using a monolithic column

    Czech Academy of Sciences Publication Activity Database

    Zemenová, Jana; Sýkora, D.; Adámková, H.; Maletínská, Lenka; Elbert, Tomáš; Marek, Aleš; Blechová, Miroslava

    2017-01-01

    Roč. 40, č. 5 (2017), s. 1032-1039 ISSN 1615-9306 Institutional support: RVO:61388963 Keywords : enzyme-linked immunosorbent assay * ghrelin * lipopeptides * liquid chromatography mass spectrometry * monolithic columns Subject RIV: CB - Analytical Chemistry, Separation OBOR OECD: Analytical chemistry Impact factor: 2.557, year: 2016

  8. Analysis of 2-methylthio-derivatives of isoprenoid cytokinins by liquid chromatography-tandem mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Tarkowski, Petr; Václavíková, Kateřina; Novák, Ondřej; Pertry, I.; Hanuš, Jan; Whenham, R.; Vereecke, D.; Šebela, M.; Strnad, Miroslav

    2010-01-01

    Roč. 680, 1-2 (2010), s. 86-91 ISSN 0003-2670 R&D Projects: GA ČR GA301/08/1649 Institutional research plan: CEZ:AV0Z50380511 Keywords : Cytokinins * Rhodococcus fascians * High-performance liquid chromatography Subject RIV: CE - Biochemistry Impact factor: 4.310, year: 2010

  9. Monoliths in capillary electrochromatography and capillary liquid chromatography in conjunction with mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Moravcová, Dana; Rantamäki, A. H.; Duša, Filip; Wiedmer, S. K.

    2016-01-01

    Roč. 37, 7-8 (2016), s. 880-912 ISSN 0173-0835 Institutional support: RVO:68081715 Keywords : capillary electrochromatography * capillary liquid chromatography * mass spec- trometry * monolithic columns Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.744, year: 2016

  10. Simultaneous and consecutive two-photon excited fluorescence detection in conventional-size liquid chromatography.

    NARCIS (Netherlands)

    Gooijer, C.; Brinkman, U.A.T.; Velthorst, N.H.; van de Nesse, R.J.; van der Wegen, R.J.

    1995-01-01

    The applicability of two-photon excitation (TPE) for fluorescence detection in flow dynamic systems was explored. Emphasis was on conventional-size liquid chromatography (LC) and a direct comparison was made with one-photon excitation (OPE) by the use of standard laser- and lamp excitation.

  11. Measurement of H2S in Crude Oil and Crude Oil Headspace Using Multidimensional Gas Chromatography, Deans Switching and Sulfur-selective Detection.

    Science.gov (United States)

    Heshka, Nicole E; Hager, Darcy B

    2015-12-10

    A method for the analysis of dissolved hydrogen sulfide in crude oil samples is demonstrated using gas chromatography. In order to effectively eliminate interferences, a two dimensional column configuration is used, with a Deans switch employed to transfer hydrogen sulfide from the first to the second column (heart-cutting). Liquid crude samples are first separated on a dimethylpolysiloxane column, and light gases are heart-cut and further separated on a bonded porous layer open tubular (PLOT) column that is able to separate hydrogen sulfide from other light sulfur species. Hydrogen sulfide is then detected with a sulfur chemiluminescence detector, adding an additional layer of selectivity. Following separation and detection of hydrogen sulfide, the system is backflushed to remove the high-boiling hydrocarbons present in the crude samples and to preserve chromatographic integrity. Dissolved hydrogen sulfide has been quantified in liquid samples from 1.1 to 500 ppm, demonstrating wide applicability to a range of samples. The method has also been successfully applied for the analysis of gas samples from crude oil headspace and process gas bags, with measurement from 0.7 to 9,700 ppm hydrogen sulfide.

  12. Separation of carbohydrates using hydrophilic interaction liquid chromatography.

    Science.gov (United States)

    Fu, Qing; Liang, Tu; Li, Zhenyu; Xu, Xiaoyong; Ke, Yanxiong; Jin, Yu; Liang, Xinmiao

    2013-09-20

    A strategy was developed to rapidly evaluate chromatographic properties of hydrophilic interaction chromatography (HILIC) columns for separating carbohydrates. Seven HILIC columns (Silica, Diol, TSK Amide-80, XAmide, Click Maltose, Click β-CD, and Click TE-Cys columns) were evaluated by using three monosaccharide and seven disaccharides as probes. The influence of column temperature on the peak shape and tautomerization of carbohydrates, as well as column selectivity were investigated. The influence of surface charge property on the retention was also studied by using glucose, glucuronic acid, and glucosamine, which indicated that buffer salt concentration and pH value in mobile phase was necessary to control the ionic interactions between ionic carbohydrates and HILIC columns. According to evaluation results, the XAmide column was selected as an example to establish experimental schemes for separation of complex mixtures of oligosaccharide. Copyright © 2013 Elsevier Ltd. All rights reserved.

  13. Ionic liquid-based air-assisted liquid-liquid microextraction followed by high performance liquid chromatography for the determination of five fungicides in juice samples.

    Science.gov (United States)

    You, Xiangwei; Chen, Xiaochu; Liu, Fengmao; Hou, Fan; Li, Yiqiang

    2018-01-15

    A novel and simple ionic liquid-based air-assisted liquid-liquid microextraction technique combined with high performance liquid chromatography was developed to analyze five fungicides in juice samples. In this method, ionic liquid was used instead of a volatile organic solvent as the extraction solvent. The emulsion was formed by pulling in and pushing out the mixture of aqueous sample solution and extraction solvent repeatedly using a 10mL glass syringe. No organic dispersive solvent was required. Under the optimized conditions, the limits of detection (LODs) were 0.4-1.8μgL -1 at a signal-to-noise ratio of 3. The limits of quantification (LOQs) set as the lowest spiking levels with acceptable recovery in juices were 10μgL -1 , except for fludioxonil whose LOQ was 20μgL -1 . The proposed method was applied to determine the target fungicides in juice samples, and acceptable recoveries ranging from 74.9% to 115.4% were achieved. Copyright © 2017. Published by Elsevier Ltd.

  14. Determination of synthetic hormones in animal urine by high-performance liquid chromatography/mass spectrometry.

    Science.gov (United States)

    Rúbies, Antoni; Cabrera, Albert; Centrich, Francesc

    2007-01-01

    A method was developed for the extraction of stanozolol, taleranol, zeranol, hexestrol, dienestrol, ethynylestradiol, diethylstilbestrol, and trenbolone from animal urine. The analytes were extracted from the matrix by enzymatic hydrolysis, solid-phase extraction, and liquid-liquid extraction. Detection and quantitation were performed on a high-performance liquid chromatography system coupled to a triple quadrupole mass spectrometer. The identification criteria met the European Union regulations. Validation of this method established a decision limit between 0.2 and 0.9 microg/L and a detection capability between 0.3 and 1.0 microg/L, depending on the analyte.

  15. Ultrasound-assisted ionic liquid-based homogeneous liquid-liquid microextraction high-performance liquid chromatography for determination of tanshinones in Salvia miltiorrhiza Bge. root.

    Science.gov (United States)

    Wang, Zhibing; Cao, Bocheng; Yu, Aimin; Zhang, Hanqi; Qiu, Fangping

    2015-02-01

    The ultrasound-assisted ionic liquid-based homogeneous liquid-liquid microextraction has been developed and applied to the extraction of four tanshinones, including dihydrotanshinone, tanshinone I, cryptotanshinone and tanshinone IIA in Salvia miltiorrhiza Bge. root. High performance liquid chromatography was applied to the separation and determination of the analytes. The ionic liquid was used as extraction solvent and target analytes were extracted with help of ultrasound. Then, ion-pairing agent was added into the sample solution, which resulted in the formation of water-insoluble ionic liquid in the solution. The phase separation was performed by centrifugation. The extraction, concentration and purification of target analytes were performed simultaneously. The experimental parameters, including type and volume of ionic liquid, sample amount, the size of sample particle, pH value of extraction medium, extraction temperature, extraction time, amount of ion-pairing agent and centrifuging time, were investigated and optimized. The calibration curves showed good linear relationship (r>0.9997). The limits of detection and quantification were in the range of 0.052-0.093 and 0.17-0.31 μg mL(-1), respectively. The recoveries were between 70.45% and 94.23% with relative standard deviations lower than 5.31%. The present method is free of volatile organic solvents, and represents lower expenditures of sample, extraction time and solvent, compared with UAE and HRE. There was no obvious difference in the extraction yields of active constitutions obtained by the three extraction methods. Copyright © 2014 Elsevier B.V. All rights reserved.

  16. Heterogeneous catalysis on solids of gases diffusing through a liquid layer, studied by inverse gas chromatography.

    Science.gov (United States)

    Kapolos, John; Katsanos, Nicholas A

    2002-11-15

    Physicochemical parameters for heterogeneous catalytic reactions when the catalytic bed was under a liquid phase have been determined, using a non-linear adsorption isotherm by the reversed-flow version of inverse gas chromatography (RF-GC). The mathematical analysis developed in heterogeneous catalysis, mass transfer across gas-liquid boundaries, and diffusion coefficients of gases in liquids was associated with a non-linear adsorption isotherm to find the relevant equations pertaining to the problem. These equations were then used to calculate the adsorption/desorption rate constant, the rate constant for the first-order catalytic reaction and the equilibrium constant for the non-linear adsorption isotherm. The diffusion coefficients of the reactant in the liquid and gaseous phases and the partition coefficients for the distribution of the reactant between the gaseous and liquid phase were also determined.

  17. Comprehensive lipidomic analysis of human plasma using multidimensional liquid- and gas-phase separations: Two-dimensional liquid chromatography-mass spectrometry vs. liquid chromatography-trapped-ion-mobility-mass spectrometry.

    Science.gov (United States)

    Baglai, Anna; Gargano, Andrea F G; Jordens, Jan; Mengerink, Ynze; Honing, Maarten; van der Wal, Sjoerd; Schoenmakers, Peter J

    2017-12-29

    Recent advancements in separation science have resulted in the commercialization of multidimensional separation systems that provide higher peak capacities and, hence, enable a more-detailed characterization of complex mixtures. In particular, two powerful analytical tools are increasingly used by analytical scientists, namely online comprehensive two-dimensional liquid chromatography (LC×LC, having a second-dimension separation in the liquid phase) and liquid chromatography-ion mobility-spectrometry (LC-IMS, second dimension separation in the gas phase). The goal of the current study was a general assessment of the liquid-chromatography-trapped-ion-mobility-mass spectrometry (LC-TIMS-MS) and comprehensive two-dimensional liquid chromatography-mass spectrometry (LC×LC-MS) platforms for untargeted lipid mapping in human plasma. For the first time trapped-ion-mobility spectrometry (TIMS) was employed for the separation of the major lipid classes and ion-mobility-derived collision-cross-section values were determined for a number of lipid standards. The general effects of a number of influencing parameters have been inspected and possible directions for improvements are discussed. We aimed to provide a general indication and practical guidelines for the analyst to choose an efficient multidimensional separation platform according to the particular requirements of the application. Analysis time, orthogonality, peak capacity, and an indicative measure for the resolving power are discussed as main characteristics for multidimensional separation systems. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Two-dimensional liquid chromatography analysis of polystyrene/polybutadiene block copolymers.

    Science.gov (United States)

    Lee, Sanghoon; Choi, Heejae; Chang, Taihyun; Staal, Bastiaan B P

    2018-04-20

    A detailed characterization of a commercial polystyrene/polybutadiene block copolymer material (StyroluxTM) was carried out using two-dimensional liquid chromatography (2D-LC). The Styrolux is prepared by statistical linking reaction of two different polystyrene-block-polybutadienyl anion precursors with a multivalent linking agent. Therefore, it is a mixture of a number of branched block copolymers different in molecular weight, composition and chain architecture. While individual LC analysis including size exclusion chromatography, interaction chromatography or liquid chromatography at critical condition is not good enough to resolve all the polymer species, 2D-LC separations coupling two chromatography methods were able to resolve all polymer species present in the sample; at least 13 block copolymer species and a homo-polystyrene blended. Four different 2D-LC analyses combining a different pair of two LC methods provide their characteristic separation results. The separation characteristics of the 2D-LC separations are compared to elucidate the elution characteristics of the block copolymer species.

  19. Determination of pyrazinamide in human by high performance liquid chromatography.

    Directory of Open Access Journals (Sweden)

    Revankar S

    1994-01-01

    Full Text Available A facile and sensitive high performance liquid chromatographic (HPLC technique has been developed for the determination pyrazinamide (PZA in human plasma. Nicotinamide(NIA is used as internal standard(IS. Plasma is deproteinized with 0.7 M perchloric acid; clear supernatant is neutralized with 1M NaOH and injected onto HPLC. The separation of pyrazinamide and the internal standard is carried out on a Supelco LC-18 (DB column with a basic mobile phase. Pyrazinoic acid, the major metabolite, other anti-tuberculous drugs and endogenous components do not interfere with measurement of pyrazinamide. The limit of detection of pyrazinamide with this method is 0.2 mg/0.2 ml plasma (CV 8.2%.

  20. Determination of patulin in apple juice by single-drop liquid-liquid-liquid microextraction coupled with liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Li, Xianjiang; Li, Hongmei; Ma, Wen; Guo, Zhen; Li, Xiaomin; Li, Xiuqin; Zhang, Qinghe

    2018-08-15

    Quick and simple analytical methodology has been developed for the measurement of patulin in apple juice by combining single-drop liquid-liquid-liquid microextraction with isotope dilution ultra-high performance liquid chromatography-mass spectrometry. After systematic parameters optimization, the whole sample pretreatment only consisted of single extraction that consumed 1.5 mL ethyl acetate. While, other methods usually needed complicated pretreatment, including extraction, purification, evaporation and redissolution. This sample pretreatment method could greatly lower the interferences from sugar-rich matrix, and the limit of detection was 0.5 μg/L and limit of quantification was 2 μg/L in apple juice. Moreover, linear range covered three orders of magnitude from 2 to 2000 μg/L. The proposed method is promising for patulin extraction and detection in apple juice, which will opens a new perspective in the enrichment of trace contaminations in high sugar complex matrix. Copyright © 2018. Published by Elsevier Ltd.

  1. Ionic liquid-dispersive liquid-liquid microextraction for the simultaneous determination of pesticides and metabolites in soils using high-performance liquid chromatography and fluorescence detection.

    Science.gov (United States)

    Asensio-Ramos, María; Hernández-Borges, Javier; Borges-Miquel, Teresa M; Rodríguez-Delgado, Miguel Ángel

    2011-07-29

    In this work, an ionic liquid-dispersive liquid-liquid microextraction (IL-DLLME) procedure was developed for the extraction of a group of pesticides (carbendazim/benomyl, thiabendazole, fuberidazole, carbaryl and triazophos) and some of their key metabolites in soils (2-aminobenzimidazole, metabolite of carbendazim and 1-naphthol, metabolite of carbaryl) from aqueous soil extracts, using high performance liquid chromatography (HPLC) with fluorescence detection (FD). Analytes were previously extracted from four soils with different physicochemical properties (forestal, ornamental, garden and lapilli soils) by ultrasound-assisted extraction (USE). The IL 1-hexyl-3-methylimidazolium hexafluorophosphate ([HMIm][PF(6)]) and methanol (MeOH) were used as extraction and dispersion solvent, respectively, for the DLLME procedure. Factors affecting IL-DLLME (sample pH, IL amount, volume of dispersion solvent and sodium chloride percentage) were optimized by means of an experimental design, obtaining the most favorable results when using 117.5 mg of IL and 418 μL of MeOH to extract the compounds from the aqueous soil extracts at pH 5.20 containing 30% (w/v) NaCl. Calibration of the USE-IL-DLLME-HPLC-FD method was carried out for every type of soil and accuracy and precision studies were developed at two levels of concentration, finding that no significant differences existed between real and spiked concentrations (Student's t test). LODs achieved were in the low ng/g range. Copyright © 2010 Elsevier B.V. All rights reserved.

  2. Silica hydride based phases for small molecule separations using automated liquid chromatography-mass spectrometry method development.

    Science.gov (United States)

    Appulage, Dananjaya K; Schug, Kevin A

    2017-07-21

    Silica hydride, or Type C silica, has been developed as an alternative chromatographic support material for liquid chromatography. There are various bonded phases available with this new support. For four such phases (Cholesterol, Bidentate C18, Diamond Hydride, and Diol), retention and selectivity behavior were investigated using liquid chromatography coupled with triple quadrupole mass spectrometry. A set of small molecules from several chemical classes of interest, and varying in their physicochemical properties, were chromatographed under both reversed-phase and aqueous normal phase modes. To screen the columns, column switching was performed using an automated platform controlled by associated software and an additional valve. A typical scouting gradient was implemented. The separation conditions were not further optimized since the goal was simply to evaluate the variable retention behavior of the phases and selectivity under generic conditions. Further, retention of the analytes were evaluated under isocratic conditions with varying percentages of organic phase to visualize the potential for dual retention modes on the same column for certain analytes. Four analytes (fentanyl, hydrocodone, hydromorphone, and matrine) showed dual mode retention behavior with all four phases. Especially, fentanyl exhibited dramatic "U-shaped" retention profiles on Cholesterol and Bidentate C18 phases. Overall, changes in the retention order between reversed phase and aqueous normal phases emphasized the potential for altered selectivity. Results showed that the Cholesterol phase provided the highest retention for most analytes compared to the other phases. The more polar Diol phase still provided good retention in reversed phase mode. Retention and selectivity were all highly reproducible. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. Determination of 1-hydroxypyrene in human urine by high-performance liquid chromatography

    DEFF Research Database (Denmark)

    Hansen, Åse Marie; Poulsen, O M; Christensen, J M

    1993-01-01

    of chromatography was 10 min using isocratic elution (acetonitrile-water, 70:30), and the retention time for 1-hydroxypyrene was 3.5 min. The short run time in combination with the low limit detection (1.37 nmol/L) makes the method potentially applicable for surveillance of pyrene exposure in work environments......A high-performance liquid chromatography (HPLC)/fluorescence method for quantitative analysis of 1-hydroxypyrene in urine was developed. The method validation analysis showed the method to be in analytical control. No significant systematical errors could be demonstrated. The entire run time...

  4. Characterization of Extracellular Vesicles by Size-Exclusion High-Performance Liquid Chromatography (HPLC).

    Science.gov (United States)

    Huang, Tao; He, Jiang

    2017-01-01

    Extracellular vesicles (EVs) have recently attracted substantial attention due to the potential diagnostic and therapeutic relevance. Although a variety of techniques have been used to isolate and analyze EVs, it is still far away from satisfaction. Size-exclusion chromatography (SEC), which separates subjects by size, has been widely applied in protein purification and analysis. The purpose of this chapter is to show the applications of size-exclusion high-performance liquid chromatography (HPLC) as methods for EV characterization of impurities or contaminants of small size, and thus for quality assay for the purity of the samples of EVs.

  5. Determination of 1-hydroxypyrene in human urine by high-performance liquid chromatography

    DEFF Research Database (Denmark)

    Hansen, Åse Marie; Poulsen, O M; Christensen, J M

    1993-01-01

    A high-performance liquid chromatography (HPLC)/fluorescence method for quantitative analysis of 1-hydroxypyrene in urine was developed. The method validation analysis showed the method to be in analytical control. No significant systematical errors could be demonstrated. The entire run time...... of chromatography was 10 min using isocratic elution (acetonitrile-water, 70:30), and the retention time for 1-hydroxypyrene was 3.5 min. The short run time in combination with the low limit detection (1.37 nmol/L) makes the method potentially applicable for surveillance of pyrene exposure in work environments...

  6. Determination of methylphenidate in Calliphorid larvae by liquid-liquid extraction and liquid chromatography mass spectrometry - Forensic entomotoxicology using an in vivo rat brain model

    DEFF Research Database (Denmark)

    Bushby, Sarah K.; Thomas, Nicky; Priemel, Petra A.

    2012-01-01

    and Calliphorid larvae) by liquid-liquid extraction with recovery of >80%, and quantified using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The LC-MS/MS assay was validated for entomotoxicological use and initially applied to male Sprague-Dawley rats (n=6) that were dosed with MPH (20mg/kg) ante......The aim of this study was to examine the potential forensic utilisation of blowfly larvae (Diptera: Calliphoridae) as an alternative toxicological specimen for the detection of the psychotropic model drug methylphenidate (MPH). MPH was extracted from biological matrices (rat brain, serum...

  7. Quantitative analysis of multiple components based on liquid chromatography with mass spectrometry in full scan mode.

    Science.gov (United States)

    Xu, Min Li; Li, Bao Qiong; Wang, Xue; Chen, Jing; Zhai, Hong Lin

    2016-08-01

    Although liquid chromatography with mass spectrometry in full scan mode can obtain all the signals simultaneously in a large range and low cost, it is rarely used in quantitative analysis due to several problems such as chromatographic drifts and peak overlap. In this paper, we propose a Tchebichef moment method for the simultaneous quantitative analysis of three active compounds in Qingrejiedu oral liquid based on three-dimensional spectra in full scan mode of liquid chromatography with mass spectrometry. After the Tchebichef moments were calculated directly from the spectra, the quantitative linear models for three active compounds were established by stepwise regression. All the correlation coefficients were more than 0.9978. The limits of detection and limits of quantitation were less than 0.11 and 0.49 μg/mL, respectively. The intra- and interday precisions were less than 6.54 and 9.47%, while the recovery ranged from 102.56 to 112.15%. Owing to the advantages of multi-resolution and inherent invariance properties, Tchebichef moments could provide favorable results even in the situation of peaks shifting and overlapping, unknown interferences and noise signals, so it could be applied to the analysis of three-dimensional spectra in full scan mode of liquid chromatography with mass spectrometry. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Combined use of liquid chromatography-hybrid quadrupole time-of-flight mass spectrometry (LC-QTOF-MS) and high performance liquid chromatography with photodiode array detector (HPLC-DAD) in systematic toxicological analysis.

    Science.gov (United States)

    Broecker, Sebastian; Pragst, Fritz; Bakdash, Abdulsallam; Herre, Sieglinde; Tsokos, Michael

    2011-10-10

    Time of flight mass spectrometry provides new possibilities of substance identification by determination of the molecular formula from accurate molecular mass and isotope pattern. However, the huge number of possible isomers requires additional evidence. As a suitable way for routine performance of systematic toxicological analysis, a method for combined use of liquid chromatography-hybrid quadrupole time-of-flight mass spectrometry (LC-QTOF-MS) and high performance liquid chromatography with diode array detector (HPLC-DAD) was developed and applied to blood samples from 77 death cases. The blood samples were prepared by extraction with CH(2)Cl(2) and by protein precipitation with acetonitrile (1:4 (v/v)). The evaporated extracts were reconstituted in 35% acetonitril/0.1% formic acid/H(2)O and aliquots were injected for analysis by LC-QTOF-MS (Agilent 6530) and HPLC-DAD (Agilent 1200). A valve switching system enabled simultaneous operation of both separated chromatographic lines under their respective optimal conditions using the same autosampler. The ESI-QTOF-MS instrument was run in data dependent acquisition mode with switching between MS and MS/MS (cycle time 1.1s) and measuring the full mass spectra and the collision induced dissociation (CID) fragment spectra of all essential [M+H](+) ions. Libraries of accurate mass CID spectra (~2500 substances) and of DAD-UV spectra (~3300 substances) of the authors were used for substance identification. The application of this procedure is demonstrated in detail at four examples with multiple drug intake or administration. In the 77 cases altogether 198 substances were identified (87 by DAD and 195 by QTOF-MS) with a frequency between 1 and 20. In practical application, the sample preparation proved to be suitable for both techniques and for a wide variety of substances with different polarity. The automatic performance of the measurements was efficient and robust. Mutual confirmation, decrease of false positive and

  9. Analyses of Indole Compounds in Sugar Cane (Saccharum officinarum L. Juice by High Performance Liquid Chromatography and Liquid Chromatography-Mass Spectrometry after Solid-Phase Extraction

    Directory of Open Access Journals (Sweden)

    Jean Wan Hong Yong

    2017-03-01

    Full Text Available Simultaneous quantitative analysis of 10 indole compounds, including indole-3-acetic acid (IAA, one of the most important naturally occurring auxins and some of its metabolites, by high performance liquid chromatography (HPLC and liquid chromatography-mass spectrometry (LC-MS after solid-phase extraction (SPE was reported for the first time. The analysis was carried out using a reverse phase HPLC gradient elution, with an aqueous mobile phase (containing 0.1% formic acid modified by methanol. Furthermore, a novel SPE procedure was developed for the pre-concentration and purification of indole compounds using C18 SPE cartridges. The combination of SPE, HPLC, and LC-MS was applied to screen for the indole compounds present in sugar cane (Saccharum officinarum L. juice, a refreshing beverage with various health benefits. Finally, four indole compounds were successfully detected and quantified in sugar cane juice by HPLC, which were further unequivocally confirmed by LC-MS/MS experiments operating in the multiple reaction monitoring (MRM mode.

  10. Rational approach to solvent system selection for liquid-liquid extraction-assisted sample pretreatment in counter-current chromatography.

    Science.gov (United States)

    Wang, Jiajia; Gu, Dongyu; Wang, Miao; Guo, Xinfeng; Li, Haoquan; Dong, Yue; Guo, Hong; Wang, Yi; Fan, Mengqi; Yang, Yi

    2017-05-15

    A rational liquid-liquid extraction approach was established to pre-treat samples for high-speed counter-current chromatography (HSCCC). n-Hexane-ethyl acetate-methanol-water (4:5:4:5, v/v) and (1:5:1:5, v/v) were selected as solvent systems for liquid-liquid extraction by systematically screening K of target compounds to remove low- and high-polarity impurities in the sample, respectively. After liquid-liquid extraction was performed, 1.4g of crude sample II was obtained from 18.5g of crude sample I which was extracted from the flowers of Robinia pseudoacacia L., and then separated with HSCCC by using a solvent system composed of n-hexane-ethyl acetate-methanol-water (1:2:1:2, v/v). As a result, 31mg of robinin and 37mg of kaempferol 7-O-α-l-rhamnopyranoside were isolated from 200mg of crude sample II in a single run of HSCCC. A scale-up separation was also performed, and 160mg of robinin with 95% purity and 188mg of kaempferol 7-O-α-l-rhamnopyranoside with 97% purity were produced from 1.2g of crude sample II. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Determination of thyroid hormones in mouse tissues by isotope-dilution microflow liquid chromatography-mass spectrometry method

    DEFF Research Database (Denmark)

    De Angelis, Meri; Giesert, Florian; Finan, Brian

    2016-01-01

    selectivity. In the last decade, several analytical methods using liquid chromatography-mass spectrometry (LC-MS) and tandem mass spectrometry (LC-MS/MS) have been developed to measure THs. These new techniques proved to be more accurate than the IA analysis and they were widely used for the determination......, (13)C6-T3, (13)C6-rT3, (13)C6-T2) dilution liquid chromatography-mass spectrometry. The major difference with previously described methods lies in the utilization of a nano-UPLC (Ultra Performance Liquid Chromatography) system in micro configuration. This approach leads to a reduction compared...

  12. Determination of Niacinamide in Lotions and Creams Using Liquid-Liquid Extraction and High-Performance Liquid Chromatography

    Science.gov (United States)

    Usher, Karyn M.; Simmons, Carolyn R.; Keating, Daniel W.; Rossi, Henry F., III

    2015-01-01

    Chemical separations are an important part of an undergraduate chemistry curriculum. Sophomore students often get experience with liquid-liquid extraction in organic chemistry classes, but liquid-liquid extraction is not as often introduced as a quantitative sample preparation method in honors general chemistry or quantitative analysis classes.…

  13. Online coupling of hydrophilic interaction/strong cation exchange/reversed-phase liquid chromatography with porous graphitic carbon liquid chromatography for simultaneous proteomics and N-glycomics analysis.

    Science.gov (United States)

    Zhao, Yun; Law, Henry C H; Zhang, Zaijun; Lam, Herman C; Quan, Quan; Li, Guohui; Chu, Ivan K

    2015-10-09

    In this study we developed a fully automated three-dimensional (3D) liquid chromatography methodology-comprising hydrophilic interaction separation as the first dimension, strong cation exchange fractionation as the second dimension, and low-pH reversed-phase (RP) separation as the third dimension-in conjunction downstream with additional complementary porous graphitic carbon separation, to capture non-retained hydrophilic analytes, for both shotgun proteomics and N-glycomics analyses. The performance of the 3D system alone was benchmarked through the analysis of the total lysate of Saccharomyces cerevisiae, leading to improved hydrophilic peptide coverage, from which we identified 19% and 24% more proteins and peptides, respectively, relative to those identified from a two-dimensional hydrophilic interaction liquid chromatography and low-pH RP chromatography (HILIC-RP) system over the same mass spectrometric acquisition time; consequently, the 3D platform also provided enhanced proteome and protein coverage. When we applied the integrated technology to analyses of the total lysate of primary cerebellar granule neurons, we characterized a total of 2201 proteins and 16,937 unique peptides for this primary cell line, providing one of its most comprehensive datasets. Our new integrated technology also exhibited excellent performance in the first N-glycomics analysis of cynomolgus monkey plasma; we successfully identified 122 proposed N-glycans and 135 N-glycosylation sites from 122 N-glycoproteins, and confirmed the presence of 38 N-glycolylneuraminic acid-containing N-glycans, a rare occurrence in human plasma, through tandem mass spectrometry for the first time. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. High-throughput determination of cortisol, cortisone, and melatonin in oral fluid by on-line turbulent flow liquid chromatography interfaced with liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Fustinoni, Silvia; Polledri, Elisa; Mercadante, Rosa

    2013-07-15

    Cortisol, cortisone, and melatonin (CORTol, CORTone, and MELA, respectively) are hormones related to stress and sleep disorders. Their detection is relevant to epidemiological studies aimed at investigating the effects of circadian cycle disruption. The aim of this study was to develop and evaluate a high-throughput assay for the detection of CORTol, CORTone, and MELA concentrations in non-invasively collected oral fluid samples. A liquid chromatography/tandem mass spectrometry (LC/MS/MS) method to measure levels of CORTol, CORTone, and MELA in oral fluid samples in the presence of deuterated analogs was optimized and validated. A 50 μL aliquot of oral fluid sample, obtained by centrifugation of a chewed swab, was purified using on-line turbulent flow liquid chromatography. Analytes were then separated using C18 reversed-phase chromatography, subjected to positive ionization using an electrospray source, then quantitated using a triple quadrupole mass detector in the selected reaction monitoring mode. Limits of quantification and linear dynamic ranges were found to be 0.55 nmol/L, 5.5 nmol/L, and 0.004 nmol/L, and up to 28 nmol/L, 277 nmol/L, and 0.43 nmol/L for CORTol, CORTone, and MELA, respectively. Inter- and intra-run precisions as relative standard deviation values were <5%, and accuracies were within 95-106% of theoretical concentrations. An evaluation of matrix effects showed that the use of deuterated analogs controlled sources of bias. Furthermore, the total analysis time per sample was 13 min, resulting in a throughput of approximately 100 samples/day. To our knowledge, this is the first automated, high-throughput assay for the simultaneous quantification of CORTol, CORTone, and MELA in oral fluid specimens. Copyright © 2013 John Wiley & Sons, Ltd.

  15. Determination of oxyfluorfen herbicide and oxyfluorfen amine residues in garbanzo beans by liquid chromatography.

    Science.gov (United States)

    Zhou, M; Miles, C J

    1991-01-01

    Oxyfluorfen and oxyfluorfen amine were determined by liquid chromatography (LC) with ultraviolet (UV) and photoconductivity detection (PCD). A simple extraction procedure acceptably recovered both analytes from garbanzo beans over a wide range of fortifications (0.05 to 20 ppm) (83 +/- 4 for oxyfluorfen; 85 +/- 4 for oxyfluorfen amine). Percent recoveries decreased slightly as the fortification level decreased. Both analytes could be determined simultaneously at a concentration greater than 0.2 ppm in garbanzo beans. Detection limits were 3 ng for oxyfluorfen and 100 ng for oxyfluorfen amine using LC/UV, and 12 ng for both oxyfluorfen and oxyfluorfen amine with LC/PCD. Different knitted reaction coils and photoreactors were evaluated. Photoproduct yields and identification were determined by ion chromatography. The LC/PCD method measures oxyfluorfen and oxyfluorfen amine separately and has a shorter analysis time, while the standard method using gas chromatography measures total residues and is more sensitive.

  16. Simultaneous determination of several phytohormones in natural coconut juice by hollow fiber-based liquid-liquid-liquid microextraction-high performance liquid chromatography.

    Science.gov (United States)

    Wu, Yunli; Hu, Bin

    2009-11-06

    A simple, selective, sensitive and inexpensive method of hollow fiber-based liquid-liquid-liquid microextraction (HF-LLLME) combined with high performance liquid chromatography (HPLC)-ultraviolet (UV) detection was developed for the determination of four acidic phytohormones (salicylic acid (SA), indole-3-acetic acid (IAA), (+/-) abscisic acid (ABA) and (+/-) jasmonic acid (JA)) in natural coconut juice. To the best of our knowledge, this is the first report on the use of liquid phase microextraction (LPME) as a sample pretreatment technique for the simultaneous analysis of several phytohormones. Using phenetole to fill the pores of hollow fiber as the organic phase, 0.1molL(-1) NaOH solution in the lumen of hollow fiber as the acceptor phase and 1molL(-1) HCl as the donor phase, a simultaneous preconcentration of four target phytohormones was realized. The acceptor phase was finally withdrawn into the microsyringe and directly injected into HPLC for the separation and quantification of the target phytohormones. The factors affecting the extraction efficiency of four phytohormones by HF-LLLME were optimized with orthogonal design experiment, and the data was analyzed by Statistical Product and Service Solutions (SPSS) software. Under the optimized conditions, the enrichment factors for SA, IAA, ABA and JA were 243, 215, 52 and 48, with the detection limits (S/N=3) of 4.6, 1.3, 0.9ngmL(-1) and 8.8 microg mL(-1), respectively. The relative standard deviations (RSDs, n=7) were 7.9, 4.9, 6.8% at 50ngmL(-1) level for SA, IAA, ABA and 8.4% at 500 microg mL(-1) for JA, respectively. To evaluate the accuracy of the method, the developed method was applied for the simultaneous analysis of several phytohormones in five natural coconut juice samples, and the recoveries for the spiked samples were in the range of 88.3-119.1%.

  17. Phytochemical Profile of Erythrina variegata by Using High-Performance Liquid Chromatography and Gas Chromatography-Mass Spectroscopy Analyses.

    Science.gov (United States)

    Muthukrishnan, Suriyavathana; Palanisamy, Subha; Subramanian, Senthilkumar; Selvaraj, Sumathi; Mari, Kavitha Rani; Kuppulingam, Ramalingam

    2016-08-01

    Natural products derived from plant sources have been utilized to treat patients with numerous diseases. The phytochemical constituents present in ethanolic leaf extract of Erythrina variegata (ELEV) were identified by using high-performance liquid chromatography (HPLC) and gas chromatography-mass spectroscopy (GC-MS) analyses. Shade dried leaves were powdered and extracted with ethanol for analyses through HPLC to identify selected flavonoids and through GC-MS to identify other molecules. The HPLC analysis of ELEV showed the presence of gallic and caffeic acids as the major components at concentrations of 2.0 ppm and 0.1 ppm, respectively, as well as other components. GC-MS analysis revealed the presence of 3-eicosyne; 3,7,11,15-tetramethyl-2-hexadecen-1-ol; butanoic acid, 3-methyl-3,7-dimethyl-6-octenyl ester; phytol; 1,2-benzenedicarboxylic acid, diundecyl ester; 1-octanol, 2-butyl-; squalene; and 2H-pyran, 2-(7-heptadecynyloxy) tetrahydro-derivative. Because pharmacopuncture is a new evolving natural mode that uses herbal extracts for treating patients with various ailments with minimum pain and maximum effect, the results of this study are particularly important and show that ELEV possesses a wide range of phytochemical constituents, as indicated above, as effective active principle molecules that can be used individually or in combination to treat patients with various diseases. Copyright © 2016. Published by Elsevier B.V.

  18. Elucidation of urinary metabolites of fluoxymesterone by liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Pozo, Oscar J; Van Thuyne, Wim; Deventer, Koen; Van Eenoo, Peter; Delbeke, Frans T

    2008-03-01

    The suitability of liquid chromatography tandem mass spectrometry (LC-MS/MS) and gas chromatography mass spectrometry (GC-MS) for the elucidation of fluoxymesterone metabolism has been evaluated. Electrospray ionization (ESI) and collision induced dissociation (CID) fragmentation in LC-MS/MS and electron impact spectra (EI) in GC-MS have been studied for fluoxymesterone and two commercially available metabolites. MS(n) experiments and accurate mass measurements performed by an ion-trap analyser and a QTOF instrument respectively have been used for the elucidation of the fragmentation pathway. The neutral loss scan of 20 Da (loss of HF) in LC-MS/MS has been applied for the selective detection of fluoxymesterone metabolites. In a positive fluoxymesterone doping control sample, 9 different analytes have been detected including the parent compound. Seven of these metabolites were also confirmed by GC-MS including 5 previously unreported metabolites. On the basis of the ionization, the CID fragmentation, the accurate mass of the product ions and the EI spectra of these analytes, a tentative elucidation as well as a proposal for the metabolic pathway of fluoxymesterone has been suggested. The presence of these compounds has also been confirmed by the analysis of five other positive fluoxymesterone urine samples. Copyright (c) 2008 John Wiley & Sons, Ltd.

  19. Phytochemical Profile of Erythrina variegata by Using High-Performance Liquid Chromatography and Gas Chromatography-Mass Spectroscopy Analyses

    Directory of Open Access Journals (Sweden)

    Suriyavathana Muthukrishnan

    2016-08-01

    Full Text Available Natural products derived from plant sources have been utilized to treat patients with numerous diseases. The phytochemical constituents present in ethanolic leaf extract of Erythrina variegata (ELEV were identified by using high-performance liquid chromatography (HPLC and gas chromatography-mass spectroscopy (GC-MS analyses. Shade dried leaves were powdered and extracted with ethanol for analyses through HPLC to identify selected flavonoids and through GC-MS to identify other molecules. The HPLC analysis of ELEV showed the presence of gallic and caffeic acids as the major components at concentrations of 2.0 ppm and 0.1 ppm, respectively, as well as other components. GC-MS analysis revealed the presence of 3-eicosyne; 3,7,11,15-tetramethyl-2-hexadecen-1-ol; butanoic acid, 3-methyl-3,7-dimethyl-6-octenyl ester; phytol; 1,2-benzenedicarboxylic acid, diundecyl ester; 1-octanol, 2-butyl-; squalene; and 2H-pyran, 2-(7-heptadecynyloxy tetrahydro-derivative. Because pharmacopuncture is a new evolving natural mode that uses herbal extracts for treating patients with various ailments with minimum pain and maximum effect, the results of this study are particularly important and show that ELEV possesses a wide range of phytochemical constituents, as indicated above, as effective active principle molecules that can be used individually or in combination to treat patients with various diseases.

  20. Gas chromatography-mass spectrometry and high-performance liquid chromatography-diode array detection for dating of paper ink.

    Science.gov (United States)

    Díaz-Santana, Oscar; Vega-Moreno, Daura; Conde-Hardisson, Francisco

    2017-09-15

    An extraction and determination method is shown for the analysis of dyes and solvents present in two types of ballpoint pen inks that are deposited onto paper. Ink extracts are analysed using a combination of gas chromatography with mass spectrometry (GC-MS), and high-pressure liquid chromatography with photodiode array detection (HPLC-DAD), within a single sample extraction procedure. Seventeen solvents and thirteen dyes contained in two Montblanc ® inks (black and blue) were monitored for 45 months at monthly intervals, in order to determine variations in the concentrations of the compounds over time. We also studied the relative variations between different compounds and the generation of degradation products such as phenol. The concentration data obtained from these compounds during their exposure have been analysed and a multiple regression model is developed for each ink type that allows an estimate of the exposure time of the ink on paper with a maximum error of between 4 and 7 months. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Use, history, and liquid chromatography/mass spectrometry chemical analysis of Aconitum

    Directory of Open Access Journals (Sweden)

    Mohamed El-Shazly

    2016-01-01

    Full Text Available Aconitum and its products have been used in Asia for centuries to treat various ailments, including arthritis, gout, cancer, and inflammation. In general, their preparations and dispensing have been restricted to qualified folk medicine healers due to their low safety index and reported toxicity. In the past few decades, official guidelines have been introduced in Asian pharmacopeias to control Aconitum herbal products. However, these guidelines were based on primitive analytical techniques for the determination of the whole Aconitum alkaloids and were unable to distinguish between toxic and nontoxic components. Recent advances in analytical techniques, especially high performance liquid chromatography (HPLC and electrophoresis coupled with highly sensitive detectors, allowed rapid and accurate determination of Aconitum secondary metabolites. Reports focusing on liquid chromatography/mass spectrometry analysis of Aconitum and its herbal products are discussed in the current review. This review can be used by the health regulatory authorities for updating pharmacopeial guidelines of Aconitum and its herbal products.

  2. Tools to discover anionic and nonionic polyfluorinated alkyl surfactants by liquid chromatography electrospray ionisation mass spectrometry

    DEFF Research Database (Denmark)

    Trier, Xenia; Granby, Kit; Christensen, Jan H.

    2011-01-01

    A tiered approach is proposed for the discovery of unknown anionic and nonionic polyfluorinated alkyl surfactants (PFASs) by reversed phase ultra high performance liquid chromatography (UHPLC) – negative electrospray ionisation – quadrupole time of flight mass spectrometry (UHPLC–ESI−–QTOF–MS). T......A tiered approach is proposed for the discovery of unknown anionic and nonionic polyfluorinated alkyl surfactants (PFASs) by reversed phase ultra high performance liquid chromatography (UHPLC) – negative electrospray ionisation – quadrupole time of flight mass spectrometry (UHPLC...... such as [M−H+solvent]− and [(M−H)(M−H+Na)n]− were used to confirm the identity of the precursor ions. In relation to quantification of PFASs, we discuss how their surfactancy influence the ESI processes, challenge their handling in solution and choices of precursor-to-product ions for MSMS of e...

  3. High-pressure liquid chromatography with direct injection of gas sample.

    Science.gov (United States)

    Astanin, Anton I; Baram, Grigory I

    2017-06-09

    The conventional method of using liquid chromatography to determine the composition of a gaseous mixture entails dissolving vapors in a suitable solvent, then obtaining a chromatograph of the resulting solution. We studied the direct introduction of a gaseous sample into a C18 reversed-phase column, followed by separation of the components by HPLC with UV detection. Since the chromatography was performed at high pressure, vapors readily dissolved in the eluent and the substances separated in the column as effectively as in liquid samples. Samples were injected into the column in two ways: a) through the valve without a flow stop; b) after stopping the flow and relieving all pressure. We showed that an injectable gas volume could reach 70% of column dead volume. When an injected gaseous sample volume was less than 10% of the column dead volume, the resulting peaks were symmetrical and the column efficiency was high. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Clinical applications of fast liquid chromatography: a review on the analysis of cardiovascular drugs and their metabolites.

    Science.gov (United States)

    Baranowska, Irena; Magiera, Sylwia; Baranowski, Jacek

    2013-05-15

    One of the major challenges facing the medicine today is developing new therapies that enhance human health. To help address these challenges the utilization of analytical technologies and high-throughput automated platforms has been employed; in order to perform more experiments in a shorter time frame with increased data quality. In the last decade various analytical strategies have been established to enhance separation speed and efficiency in liquid chromatography applications. Liquid chromatography is an increasingly important tool for monitoring drugs and their metabolites. Furthermore, liquid chromatography has played an important role in pharmacokinetics and metabolism studies at these drug development stages since its introduction. This paper provides an overview of current trends in fast chromatography for the analysis of cardiovascular drugs and their metabolites in clinical applications. Current trends in fast liquid chromatographic separations involve monolith technologies, fused-core columns, high-temperature liquid chromatography (HTLC) and ultra-high performance liquid chromatography (UHPLC). The high specificity in combination with high sensitivity makes it an attractive complementary method to traditional methodology used for routine applications. The practical aspects of, recent developments in and the present status of fast chromatography for the analysis of biological fluids for therapeutic drug and metabolite monitoring, pharmacokinetic studies and bioequivalence studies are presented. Copyright © 2013 Elsevier B.V. All rights reserved.

  5. DETECTION AND QUANTIFICATION OF PHYTOCHEMICAL MARKERS OF Ilex paraguariensis BY LIQUID CHROMATOGRAPHY

    OpenAIRE

    Pinto,Rodrigo M. C.; Lemes,Bruna M.; Zielinski,Acácio A. F.; Klein,Traudi; Paula,Fernado de; Kist,Airton; Marques,Anna S. F.; Nogueira,Alessandro; Demiate,Ivo M.; Beltrame,Flávio L.

    2015-01-01

    Ilex paraguariensis (yerba-mate) is used as a beverage, and its extract requires adequate quality control methods in order to guarantee quality and safe use. Strategies to develop and optimize a chromatographic method to quantify theobromine, caffeine, and chlorogenic acid in I. paraguariensis extracts were evaluated by applying a quality by design (QbD) model and ultra high-performance liquid chromatography (UHPLC). The presence of these three phytochemical markers in the extracts was evalua...

  6. Quantitative analysis of cytokinins in plants by liquid chromatography single-quadrupole mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Novák, Ondřej; Tarkowski, Petr; Tarkowská, Danuše; Doležal, Karel; Lenobel, René; Strnad, Miroslav

    2003-01-01

    Roč. 480, č. 2 (2003), s. 207ů218 ISSN 0003-2670 R&D Projects: GA ČR GA522/01/0275 Grant - others: Volkswagen Stiftung(DE) I/76 865 Institutional research plan: CEZ:AV0Z5038910; CEZ:MSM 153100008 Keywords : Liquid chromatography mass spectrometry * Cytokinins Subject RIV: EB - Genetics ; Molecular Biology Impact factor: 2.210, year: 2003

  7. In Vivo Neurochemical Monitoring using Benzoyl Chloride Derivatization and Liquid Chromatography – Mass Spectrometry

    OpenAIRE

    Song, Peng; Mabrouk, Omar S.; Hershey, Neil D.; Kennedy, Robert T.

    2011-01-01

    In vivo neurochemical monitoring using microdialysis sampling is important in neuroscience because it allows correlation of neurotransmission with behavior, disease state, and drug concentrations in the intact brain. A significant limitation of current practice is that different assays are utilized for measuring each class of neurotransmitter. We present a high performance liquid chromatography (HPLC) - tandem mass spectrometry method that utilizes benzoyl chloride for determination of the mo...

  8. Separation of PCBs by liquid chromatography on reversed phase sub-2-micron particle columns

    Czech Academy of Sciences Publication Activity Database

    Olšovská, Jana; Křesinová, Zdena; Flieger, Miroslav; Cajthaml, Tomáš

    2010-01-01

    Roč. 80, č. 5 (2010), s. 1849-1855 ISSN 0039-9140 R&D Projects: GA MŠk 2B06156; GA ČR GA525/09/1058 Institutional research plan: CEZ:AV0Z50200510 Keywords : Ultra high-performance liquid chromatography * PCB * Congener analysis Subject RIV: EE - Microbiology, Virology Impact factor: 3.722, year: 2010

  9. Micromethod for measuring hexachlorophene in whole blood by gas-liquid chromatography.

    Science.gov (United States)

    Dodson, W E; Tyrala, E E; Hillman, R E

    1977-06-01

    We describe a micromethod for measuring hexachlorophene by use of gas-liquid chromatography with a 63Ni electron capture detector. The procedure requires 100 micronl of blood for extractions of hexachlorophene, and dichlorophene is added as an internal standard. CV is 3.4% over the concentration range of 500 to 1300 microng of hexachlorophene per liter of whole blood. This procedure permits repeated measurements of hexachlorophene in newborns who are being washed with soap containing hexachlorophene.

  10. Toxic Compounds Analysis With High Performance Liquid Chromatography Detected By Electro Chemical Detector (Ecd)

    OpenAIRE

    Hideharu Shintaniq

    2014-01-01

    The principal area of application of high performance liquid chromatography-electrochemical detector (HPLC-ECD) has been in the analysis of naturally-occurring analytes, such as catecholamines, and pharmaceuticals in biological samples, HPLC-ECD has also applied to the analysis of pesticides and other analytes of interest to the toxicologist. In this paper, toxic area is described. In these, ammatoxins, aromatic amine, nitro-compounds, algal toxins, fungal toxins, pesticides, veterinary drug ...

  11. Determination of Decabrominated Diphenyl Ether in Soils by Soxhlet Extraction and High Performance Liquid Chromatography

    OpenAIRE

    Xing-Jian Yang; Zhi Dang; Fang-Li Zhang; Zhao-Ying Lin; Meng-Yao Zou; Xue-Qin Tao; Gui-Ning Lu

    2013-01-01

    This study described the development of a method based on soxhlet extraction combining high performance liquid chromatography (soxhlet-HPLC) for the accurate detection of BDE-209 in soils. The solvent effect of working standard solutions in HPLC was discussed. Results showed that 1?:?1 of methanol and acetone was the optimal condition which could totally dissolve the BDE-209 in environmental samples and avoid the decrease of the peak area and the peak deformation difference of BDE-209 in HPLC...

  12. An analytical study by gas liquid chromatography and radiochromatography of tritium labelled lebaycid

    International Nuclear Information System (INIS)

    Perez Garcia, M. M.

    1969-01-01

    The stability and purity of the syntheses products of Lebaycid: 0,0 dime thylfosfochlorothionate and 4 methyl-thio-m-cresol were investigated by gas liquid chromatography. The study on (CH 3 O) 2 PSC1 was made in a column of Silicone SE-30, Reoplex 400 using a thermal conductivity detector. The 99,4% pure product obtained from the preparative gas chromatograph was found to be stable within the duration of the experiment: seven months. (Author) 23 refs

  13. Simple and rapid determination of zaltoprofen in human plasma by manual-shaking-assisted dispersive liquid-liquid microextraction followed by liquid chromatography with ultraviolet detection.

    Science.gov (United States)

    Han, Se Young; Jeong, Kyung Min; Yoo, Da Eun; Jin, Yan; Kim, Eun Mi; Kim, Su Hyun; Lee, Seok-Yong; Kim, Se-Hyung; Zhao, Jing; Lee, Jeongmi

    2017-10-01

    A readily applicable method was developed to determine the concentration level of zaltoprofen, a non-steroidal antiinflammatory drug from the propionic acid family, in human plasma. This method is based on manual-shaking-assisted dispersive liquid-liquid microextraction coupled with liquid chromatography with ultraviolet detection. Factors affecting the extraction efficiency were screened and optimized by experimental design using fractional factorial and central composite designs, respectively. Optimal conditions were: 220 μL of C 2 H 4 Cl 2 (extraction solvent), 5 mL of 3.75% w/v NaCl aqueous solution at pH 2.0, and manual shaking for 13 s (65 times). The resulting extraction method yielded a reasonable enrichment factor of 18.0 (±0.6, n = 3) and extraction recovery of 86.0% (±3.3%, n = 3). The established method was validated for selectivity, linearity, precision, accuracy, matrix effect, recovery, dilution integrity, and stability, and it met the acceptable criteria for all of the tested parameters. Specifically, the method was linear in the range of 0.16-50.0 mg/L, precise (liquid-liquid extraction or non-specific protein precipitation, our method allows the simple, rapid, and efficient determination of zaltoprofen using the most affordable analytical instrument, liquid chromatography with ultraviolet detection. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Characterization of pitches by liquid chromatography using cellulose 3,5-dinitrobenzoate as the packing material

    Energy Technology Data Exchange (ETDEWEB)

    Arai, K.; Judo, R.; Ota, E. [Gunma University, Gunma (Japan). Dept. of Chemistry

    1997-08-01

    Characterization of coal tar, petroleum and PVC pitches by a liquid chromatography using cellulose 3,5-dinitrobenzoate (DNB-cellulose) as the packing material was investigated. Separation mechanism based on charge-transfer interaction between the dinitrobenzoyl group and polyaromatic compounds was expected to be useful for separation of the constituents of the pitches. First, 26 model polyaromatic compounds were tested to examine the characteristic feature of the packing material by liquid chromatography. The compounds were found to be classified roughly into four groups with different retention volume, principally according to the number of condensed rings. The nonplanar structure and aliphatic side chain of the polyaromatic compounds also affected the separation behavior. Both benzene soluble-hexane soluble and benzene soluble-hexane insoluble fractions of the three pitches were separated on DNB-cellulose. It was found that coal tar pitch contains relatively large amounts of some highly condensed polyaromatic compounds with condensed rings of 4 to 5; petroleum pitch has small amounts of such specific highly condensed polyaromatic compounds, while PVC pitch has large amounts of less condensed polyaromatic compounds and there is no significant amount of highly condensed compound in it. Thus DNB-cellulose was useful as the convenient packing material for liquid chromatography to characterize pitches.

  15. Integrated gas and liquid chromatography tandem mass spectrometry for forensic engine lubricating oil identification

    International Nuclear Information System (INIS)

    Shang, D.; McPherson, B.

    2009-01-01

    This paper presented a method for rapid chemical characterization of engine lubricating oils. Motor oils typically contain up to 5 per cent additives, such as detergent, antifoamant, dispersant, emulsifier, antioxidant, friction modifier, colour stabilizer and corrosion inhibitors. Different lube oil products usually have either different additives in various concentrations. As such, the formulation of additives in lube oil products should provide fingerprint information for forensic oil identification. The characterization method used in this study was based on a newly developed fast solvent liquid-liquid sample extraction procedure that combined the use of both liquid chromatography tandem mass spectrometry (LC-MS) and gas chromatography-mass spectrometry (GC-MS) simultaneously together with gas chromatography flame ionization detection (GC-FID). The method was used on a blind sample testing of commercially available engine lubricating products. The sample extraction procedure involved extraction of additives into acidified acetonitrile, two hexane washes of hydrophobic components of lube oil, filtration, and dilution with solvents for GC and LC analysis. The new method proved to be rapid and easy to use. It enabled the identification of unknown additives and hydrocarbons in many different types of fresh lube oils. Further tests will be needed to determine if this method can be used on real-world weathered samples. The method is part of an ongoing effort to deal with mysterious chemical spills, an important aspect of environmental protection and emergency preparedness. 8 refs., 7 figs

  16. Intact-protein trapping columns for proteomic analysis in capillary high-performance liquid chromatography.

    Science.gov (United States)

    Guan, Xia; Yan, Guoquan; Gao, Mingxia; Hong, Guangfeng; Deng, Chunhui; Zhang, Xiangmin

    2010-10-29

    A new type of monolithic trapping columns with high mechanical strength was prepared by thin-layer sol-gel coating method and applied to trapping intact proteins for on-line capillary liquid chromatography. Monolithic trapping columns were fabricated by entrapping C8 reversed-phase particles into the capillary columns through a sol-gel network, which was formed by hydrolysis and polycondensation of methyltriethoxysilane. Hundreds times of trapping/untrapping for intact proteins were carried out. The trapping columns showed long-term stability up to 300 bar. Recovery, loading capacity and reproducibility of trapping columns were evaluated using four proteins. The recovery of four protein mixtures for the C8 monolithic trapping columns was 99.3% on average. The loading capacity of 5 mm × 320 μm i.d. C8 trapping columns for the protein mixtures was 30 μg. Day-to-day relative standard deviation (RSD) values for recoveries of protein mixtures on the same C8 trapping column ranged from 2.34 to 5.87%, column-to-column RSD values were from 3.01 to 6.81%. The C8 trapping columns were used to trap normal mouse liver intact proteins in a capillary liquid chromatography system. Results demonstrated high efficiency of the monolithic trapping columns for trapping intact proteins for proteomic analysis in on-line capillary liquid chromatography system. Copyright © 2010 Elsevier B.V. All rights reserved.

  17. Multiclass mycotoxin analysis in edible oils using a simple solvent extraction method and liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Eom, Taeyong; Cho, Hyun-Deok; Kim, Junghyun; Park, Mihee; An, Jinyoung; Kim, Moosung; Kim, Sheen-Hee; Han, Sang Beom

    2017-11-01

    A simple and rapid method for the simultaneous determination of 11 mycotoxins - aflatoxins B 1 , B 2 , G 1 and G 2 ; fumonisins B 1 , B 2 and B 3 ; ochratoxin A; zearalenone; deoxynivalenol; and T-2 toxin - in edible oils was established using liquid chromatography tandem mass spectrometry (LC-MS/MS). In this study, QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe), QuEChERS with dispersive liquid-liquid microextraction, and solvent extraction were examined for sample preparation. Among these methods, solvent extraction with a mixture of formic acid/acetonitrile (5/95, v/v) successfully extracted all target mycotoxins. Subsequently, a defatting process using n-hexane was employed to remove the fats present in the edible oil samples. Mass spectrometry was carried out using electrospray ionisation in polarity switching mode with multiple reaction monitoring. The developed LC-MS/MS method was validated by assessing the specificity, linearity, recovery, limit of quantification (LOQ), accuracy and precision with reference to Commission Regulation (EC) 401/2006. Mycotoxin recoveries of 51.6-82.8% were achieved in addition to LOQs ranging from 0.025 ng/g to 1 ng/g. The edible oils proved to be relatively uncomplicated matrices and the developed method was applied to 9 edible oil samples, including soybean oil, corn oil and rice bran oil, to evaluate potential mycotoxin contamination. The levels of detection were significantly lower than the international regulatory standards. Therefore, we expect that our developed method, based on simple, two-step sample preparation process, will be suitable for the large-scale screening of mycotoxin contamination in edible oils.

  18. Simultaneous determination of aflatoxin B₁, B₂, G₁, and G₂ in corn powder, edible oil, peanut butter, and soy sauce by liquid chromatography with tandem mass spectrometry utilizing turbulent flow chromatography.

    Science.gov (United States)

    Fan, Sufang; Li, Qiang; Zhang, Xiaoguang; Cui, Xiaobin; Zhang, Dongsheng; Zhang, Yan

    2015-05-01

    A novel fully automated method based on dual column switching using turbulent flow chromatography followed by liquid chromatography with tandem mass spectrometry was developed for the determination of aflatoxin B1 , B2 , G1 , and G2 in corn powder, edible oil, peanut butter, and soy sauce samples. After ultrasound-assisted extraction, samples were directly injected to the chromatographic system and the analytes were concentrated into the clean-up loading column. Through purge switching, the analytes were transferred to the analytical column for subsequent detection by mass spectrometry. Different types of TurboFlow(TM) columns, transfer flow rate, transfer time were optimized. The limits of detection and quantification of this method ranged between 0.2-2.0 and 0.5-4.0 μg/kg for aflatoxins in different matrixes, respectively. Recoveries of aflatoxins were in range of 83-108.1% for all samples, matrix effects were in range of 34.1-104.7%. The developed method has been successfully applied in the analysis of aflatoxin B1 , B2 , G1 , and G2 in real samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Influence of ZnO nanostructures in liquid crystal interfaces for bistable switching applications

    Energy Technology Data Exchange (ETDEWEB)

    Pal, Kaushik, E-mail: kaushikpal@whu.edu.cn [School of Power and Mechanical Engineering, Wuhan University, 8 East Lake South Road, Wuhan 430072 (China); Zhan, Bihong, E-mail: bihong_zhan@whu.edu.cn [School of Power and Mechanical Engineering, Wuhan University, 8 East Lake South Road, Wuhan 430072 (China); Madhu Mohan, M.L.N. [Liquid Crystal Research Laboratory (LCRL), Bannari Amman Institute of Technology, Sathyamangalam 638 401 (India); Schirhagl, Romana [University Medical Center Groningen, Department of BioMedical Engineering, Ant. Deusinglaan 1, 9713 AV Groningen (Netherlands); Wang, Guoping, E-mail: guopingwang@whu.edu.cn [School of Power and Mechanical Engineering, Wuhan University, 8 East Lake South Road, Wuhan 430072 (China)

    2015-12-01

    Graphical abstract: - Highlights: • One step bench top novel synthesis and growth dynamics of ZnO structures are successfully performed. • Nanostructures dispersing liquid crystals (NDLC) is recently found to have significant influence on the nucleation and growth of many functional nanocrystals (NCs), and provide a fundamental approach to modify the crystallographic phase, size, morphology, and electronic configuration of nanomaterials. • Electro-optical switching application ensures the bright field droplet design marble pattern of smectic G phase, nematic and most significant twist nematic phase pattern are obtained. • Spontaneous polarization, rotational viscosity and response time study, exploring smart applications in LCD technology. - Abstract: The controlled fabrication of nanometer-scale objects is without doubt one of the central issues in current science and technology. In this article, we exhibit a simple, one-step bench top synthesis of zinc oxide nano-tetrapods and nano-spheres which were tailored by the facial growth of nano-wires (diameter ≈ 24 nm; length ≈ 118 nm) and nano-cubes (≈395 nm edge) to nano-sphere (diameter ≈ 585 nm) appeaded. The possibilities of inexpensive, simple solvo-chemical synthesis of nanostructures were considered. In this article, a successful attempt has been made that ZnO nano-structures dispersed on well aligned hydrogen bonded liquid crystals (HBLC) comprising azelaic acid (AC) with p-n-alkyloxy benzoic acid (nBAO) by varying the respective alkyloxy carbon number (n = 5). The dispersion of nanomaterials with HBLC is an effective route to enhance the existing functionalities. A series of these composite materials were analyzed by polarizing optical microscope's electro-optical switching. An interesting feature of AC + nBAO is the inducement of tilted smectic G phase with increasing carbon chain length. Phase diagrams of the above hybrid ZnO nanomaterial influenced LC complex and pure LC were

  20. Investigation of forced and total degradation products of amlodipine besylate by liquid chromatography and liquid chromatography-mass spectrometry

    Directory of Open Access Journals (Sweden)

    Stoiljković Zora Ž.

    2014-01-01

    Full Text Available An isocratic, reversed-phase liquid chromatographic method was applied for the investigation of the degradation products of amlodipine besylate under the stressed conditions in solution. Amlodipine besylate stock solutions were subjected to acid and alkali hydrolysis, chemical oxidation and photodegradation as well as to the electrochemical degradation by cyclic voltammetry in 0.05 mol/L NaHCO3 on gold electrode. The total degradation of amlodipine besylate was achieved in 5 mol/L NaOH at 80°C for 6 h and the compound with molecular formula C15H16NOCl was identified as a main degradation product. Under acidic (5 mol/L HCl at 80°C for 6 h stress conditions 75.2% of amlodipine besylate degradation was recorded. Oxidative degradation in the solution of 3% H2O2-methanol 80:20 at 80°C for 6 h showed that amlodipine besylate degraded to 80.1%. After 14 days of expose in photostability chamber amlodipine besylate solution showed degradation of 32.2%. In electrochemical degradation after 9 hours of cyclization the beginning of amlodipine oxidation was shifted for 200 mV to more negative potentials, with the degradation of 66.5%. Mass spectrometry analysis confirmed the presence of dehydro amlodipine derivate with molecular formula C20H23N2O5Cl in oxidative and acidic conditions while in electrochemical degradation was detected in traces. [Projekat Ministarsva nauke Republike Srbije, br. 172013

  1. Localised polymer networks in chiral nematic liquid crystals for high speed photonic switching

    International Nuclear Information System (INIS)

    Tartan, Chloe C.; Salter, Patrick S.; Booth, Martin J.; Morris, Stephen M.; Elston, Steve J.

    2016-01-01

    Self-assembled periodic structures based upon chiral liquid crystalline materials have significant potential in the field of photonics ranging from fast-switching optoelectronic devices to low-threshold lasers. The flexoelectro-optic effect, which is observed in chiral nematic liquid crystals (LCs) when an electric field is applied perpendicular to the helical axis, has significant potential as it exhibits analogue switching in 10–100 μs. However, the major technological barrier that prohibits the commercial realisation of this electro-optic effect is the requirement of a uniform, in-plane alignment of the helix axis between glass substrates. Here, it is shown that periodic polymer structures engineered in the nematic phase of a chiral nematic LC device using direct laser writing can result in the spontaneous formation of the necessary uniform lying helix (ULH) state. Specifically, two-photon polymerization is used in conjunction with a spatial light modulator so as to correct for aberrations introduced by the bounding glass substrates enabling the polymer structures to be fabricated directly into the device. The ULH state appears to be stable in the absence of an externally applied electric field, and the optimum contrast between the bright and dark states is obtained using polymer structures that have periodicities of the order of the device thickness.

  2. Localised polymer networks in chiral nematic liquid crystals for high speed photonic switching

    Energy Technology Data Exchange (ETDEWEB)

    Tartan, Chloe C., E-mail: chloe.tartan@eng.ox.ac.uk, E-mail: steve.elston@eng.ox.ac.uk; Salter, Patrick S.; Booth, Martin J.; Morris, Stephen M.; Elston, Steve J., E-mail: chloe.tartan@eng.ox.ac.uk, E-mail: steve.elston@eng.ox.ac.uk [Department of Engineering Science, University of Oxford, Parks Road, Oxford OX1 3PJ (United Kingdom)

    2016-05-14

    Self-assembled periodic structures based upon chiral liquid crystalline materials have significant potential in the field of photonics ranging from fast-switching optoelectronic devices to low-threshold lasers. The flexoelectro-optic effect, which is observed in chiral nematic liquid crystals (LCs) when an electric field is applied perpendicular to the helical axis, has significant potential as it exhibits analogue switching in 10–100 μs. However, the major technological barrier that prohibits the commercial realisation of this electro-optic effect is the requirement of a uniform, in-plane alignment of the helix axis between glass substrates. Here, it is shown that periodic polymer structures engineered in the nematic phase of a chiral nematic LC device using direct laser writing can result in the spontaneous formation of the necessary uniform lying helix (ULH) state. Specifically, two-photon polymerization is used in conjunction with a spatial light modulator so as to correct for aberrations introduced by the bounding glass substrates enabling the polymer structures to be fabricated directly into the device. The ULH state appears to be stable in the absence of an externally applied electric field, and the optimum contrast between the bright and dark states is obtained using polymer structures that have periodicities of the order of the device thickness.

  3. Electrothermally Driven Fluorescence Switching by Liquid Crystal Elastomers Based On Dimensional Photonic Crystals.

    Science.gov (United States)

    Lin, Changxu; Jiang, Yin; Tao, Cheng-An; Yin, Xianpeng; Lan, Yue; Wang, Chen; Wang, Shiqiang; Liu, Xiangyang; Li, Guangtao

    2017-04-05

    In this article, the fabrication of an active organic-inorganic one-dimensional photonic crystal structure to offer electrothermal fluorescence switching is described. The film is obtained by spin-coating of liquid crystal elastomers (LCEs) and TiO 2 nanoparticles alternatively. By utilizing the property of LCEs that can change their size and shape reversibly under external thermal stimulations, the λ max of the photonic band gap of these films is tuned by voltage through electrothermal conversion. The shifted photonic band gap further changes the matching degree between the photonic band gap of the film and the emission spectrum of organic dye mounting on the film. With rhodamine B as an example, the enhancement factor of its fluorescence emission is controlled by varying the matching degree. Thus, the fluorescence intensity is actively switched by voltage applied on the system, in a fast, adjustable, and reversible manner. The control chain of using the electrothermal stimulus to adjust fluorescence intensity via controlling the photonic band gap is proved by a scanning electron microscope (SEM) and UV-vis reflectance. This mechanism also corresponded to the results from the finite-difference time-domain (FDTD) simulation. The comprehensive usage of photonic crystals and liquid crystal elastomers opened a new possibility for active optical devices.

  4. Chiral ligand exchange high-speed countercurrent chromatography: mechanism, application and comparison with conventional liquid chromatography in enantioseparation of aromatic α-hydroxyl acids

    OpenAIRE

    Tong, Shengqiang; Shen, Mangmang; Cheng, Dongping; Ito, Yoichiro; Yan, Jizhong

    2014-01-01

    This work concentrates on the separation mechanism and application of chiral ligand exchange high-speed countercurrent chromatography (HSCCC) in enantioseparations, and comparison with traditional chiral ligand exchange high performance liquid chromatography (HPLC). The enantioseparation of ten aromatic α-hydroxyl acids were performed by these two chromatographic methods. Results showed that five of the racemates were successfully enantioseparated by HSCCC while only three of the racemates co...

  5. EXTRACTION AND QUANTITATIVE ANALYSIS OF ELEMENTAL SULFUR FROM SULFIDE MINERAL SURFACES BY HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY. (R826189)

    Science.gov (United States)

    A simple method for the quantitative determination of elemental sulfur on oxidized sulfide minerals is described. Extraction of elemental sulfur in perchloroethylene and subsequent analysis with high-performance liquid chromatography were used to ascertain the total elemental ...

  6. Gas chromatography-mass spectrometry and high-performance liquid chromatographic analyses of thermal degradation products of common plastics.

    Science.gov (United States)

    Pacáková, V; Leclercq, P A

    1991-08-30

    The thermo-oxidation of five commonly used materials, namely low-density polyethylene, retarded polyethylene, paper with a polyethylene foil, a milk package and filled polypropylene, was studied. Capillary gas chromatography and gas chromatography-mass spectrometry were used to analyze the volatile degradation products, while high-performance liquid chromatography was employed to measure polycyclic aromatic hydrocarbons. The results are discussed from the point of view of toxicity of the products.

  7. Coupling of column liquid chromatography and surface-enhanced resonance Raman spectroscopy via a thin-layer chromatographic plate.

    NARCIS (Netherlands)

    Coulter, S.K.; Gooijer, C.; Velthorst, N.H.; Brinkman, U.A.T.; Somsen, G.W.

    1997-01-01

    Surface-enhanced resonance Raman (SERR) spectroscopy was used to characterize compounds separated by column liquid chromatography (LC). Three percent of the effluent from a conventional-size LC column were immobilized on a moving thinlayer chromatography (TLC) plate using a spray-jet

  8. Direct solid-phase microextraction combined with gas and liquid chromatography for the determination of lidocaine in human urine

    NARCIS (Netherlands)

    Koster, E.H M; Hofman, N.S K; de Jong, G.J.

    Solid-phase microextraction (SPME) has been combined with gas chromatography (GC) and liquid chromatography (LC) for the determination of lidocaine in human urine. A polydimethylsiloxane (PDMS) coated fibre was directly immersed into buffered urine. Extraction conditions such as time, pH, ionic

  9. Determination of polar organophosphorus pesticides in vegetables and fruits using liquid chromatography with tandem mass spectrometry: Selection of extraction solvent

    NARCIS (Netherlands)

    Mol, H.G.J.; Dam, R.C.J. van; Steijger, O.M.

    2003-01-01

    A method based on liquid chromatography (LC)-mass spectrometry (MS)/MS was developed for sensitive determination of a number of less gas chromatography (GC)-amenable organophosphorus pesticides (OPs; acephate, methamidophos, monocrotophos, omethoate, oxydemeton-methyl and vamidothion) in cabbage and

  10. Quantitative analysis of pharmaceuticals in biological fluids using high-performance liquid chromatography coupled to mass spectrometry: a review.

    Science.gov (United States)

    Plumb, R S; Dear, G J; Mallett, D N; Higton, D M; Pleasance, S; Biddlecombe, R A

    2001-01-01

    1. The development of bio-analysis of drug molecules over the last 10 years is reviewed, focusing on advances in sample preparation, liquid chromatography and detection. 2. Developments have led to improvements in detection sensitivity, enhancements in specificity and increased capacity. 3. Emerging technologies such as monolithic column chromatography and miniaturized chip-based systems are discussed.

  11. tRNA separation by high-performance liquid chromatography using an aggregate of ODS-Hypersil and trioctylmethylammonium chloride

    NARCIS (Netherlands)

    Bischoff, Rainer; Graeser, E.; Mclaughlin, L.W.

    1983-01-01

    High-performance liquid chromatography on a reversed-phase support treated with a tetraalkylammonium salt was used to separate tRNAs from baker's yeast. While resolution by this column appears to result from both anion-exchange and reversed-phase chromatography, it is the hydrophobic interactions

  12. Preventive doping control analysis: Liquid and gas chromatography time-to-flight mass spectrometry for detection of designer steriods

    NARCIS (Netherlands)

    Georgakopoulos, C.G.; Vonaparti, A.; Stamou, M.; Kiousi, P.; Lyris, E.; Angelis, Y.S.; Tsoupras, G.; Wuest, B.; Nielen, M.W.F.; Panderi, I.; Koupparis, M.

    2007-01-01

    A new combined doping control screening method for the analysis of anabolic steroids in human urine using liquid chromatography/electrospray ionization orthogonal acceleration time-of-flight mass spectrometry (LCoaTOFMS) and gas chromatography/electron ionization orthogonal acceleration

  13. Analysis of host-cell proteins in biotherapeutic proteins by comprehensive online two-dimensional liquid chromatography/mass spectrometry

    OpenAIRE

    Doneanu, Catalin E; Xenopoulos, Alex; Fadgen, Keith; Murphy, Jim; Skilton, St. John; Prentice, Holly; Stapels, Martha; Chen, Weibin

    2012-01-01

    Assays for identification and quantification of host-cell proteins (HCPs) in biotherapeutic proteins over 5 orders of magnitude in concentration are presented. The HCP assays consist of two types: HCP identification using comprehensive online two-dimensional liquid chromatography coupled with high resolution mass spectrometry (2D-LC/MS), followed by high-throughput HCP quantification by liquid chromatography, multiple reaction monitoring (LC-MRM). The former is described as a “discovery” assa...

  14. Overview of online two-dimensional liquid chromatography based on cell membrane chromatography for screening target components from traditional Chinese medicines.

    Science.gov (United States)

    Muhammad, Saqib; Han, Shengli; Xie, Xiaoyu; Wang, Sicen; Aziz, Muhammad Majid

    2017-01-01

    Cell membrane chromatography is a simple, specific, and time-saving technique for studying drug-receptor interactions, screening of active components from complex mixtures, and quality control of traditional Chinese medicines. However, the short column life, low sensitivity, low column efficiency (so cannot resolve satisfactorily mixture of compounds), low peak capacity, and inefficient in structure identification were bottleneck in its application. Combinations of cell membrane chromatography with multidimensional chromatography such as two-dimensional liquid chromatography and high sensitivity detectors like mass have significantly reduced many of the above-mentioned shortcomings. This paper provides an overview of the current advances in online two-dimensional-based cell membrane chromatography for screening target components from traditional Chinese medicines with particular emphasis on the instrumentation, preparation of cell membrane stationary phase, advantages, and disadvantages compared to alternative approaches. The last section of the review summarizes the applications of the online two-dimensional high-performance liquid chromatography based cell membrane chromatography reported since its emergence to date (2010-June 2016). © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Determination of parabens in serum by liquid chromatography-tandem mass spectrometry: Correlation with lipstick use.

    Science.gov (United States)

    Tahan, Gabriella Padovani; Santos, Nayara de Kássia Souza; Albuquerque, Ana Carolina; Martins, Isarita

    2016-08-01

    Parabens are the most widely used preservative and are considered to be relatively safe compounds. However, studies have demonstrated that they may have estrogenic activity, and there is ongoing debate regarding the safety and potential cancer risk of using products containing these compounds. In the present work, liquid chromatography-tandem mass spectrometry was applied to determine methylparaben and propylparaben concentrations in serum, and the results were correlated with lipstick application. Samples were analyzed using liquid-liquid extraction, followed by liquid chromatography-tandem mass spectrometry. The validation results demonstrated the linearity of the method over a range of 1-20 ng/mL, in addition to the method's precision and accuracy. A statistically significant difference was demonstrated between serum parabens in women who used lipstick containing these substances compared with those not using this cosmetic (p = 0.0005 and 0.0016, respectively), and a strong association was observed between serum parabens and lipstick use (Spearman correlation = 0.7202). Copyright © 2016 Elsevier Inc. All rights reserved.

  16. Incorporation of ionic liquid into porous polymer monoliths to enhance the separation of small molecules in reversed-phase high-performance liquid chromatography.

    Science.gov (United States)

    Wang, Jiafei; Bai, Ligai; Wei, Zhen; Qin, Junxiao; Ma, Yamin; Liu, Haiyan

    2015-06-01

    An ionic liquid was incorporated into the porous polymer monoliths to afford stationary phases with enhanced chromatographic performance for small molecules in reversed-phase high-performance liquid chromatography. The effect of the ionic liquid in the polymerization mixture on the performance of the monoliths was studied in detail. While monoliths without ionic liquid exhibited poor resolution and low efficiency, the addition of ionic liquid to the polymerization mixture provides highly increased resolution and high efficiency. The chromatographic performances of the monoliths were demonstrated by the separations of various small molecules including aromatic hydrocarbons, isomers, and homologues using a binary polar mobile phase. The present column efficiency reached 27 000 plates/m, which showed that the ionic liquid monoliths are alternative stationary phases in the separation of small molecules by high-performance liquid chromatography. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Deformation and degradation of polymers in ultra-high-pressure liquid chromatography.

    Science.gov (United States)

    Uliyanchenko, Elena; van der Wal, Sjoerd; Schoenmakers, Peter J

    2011-09-28

    Ultra-high-pressure liquid chromatography (UHPLC) using columns packed with sub-2 μm particles has great potential for separations of many types of complex samples, including polymers. However, the application of UHPLC for the analysis of polymers meets some fundamental obstacles. Small particles and narrow bore tubing in combination with high pressures generate significant shear and extensional forces in UHPLC systems, which may affect polymer chains. At high stress conditions flexible macromolecules may become extended and eventually the chemical bonds in the molecules can break. Deformation and degradation of macromolecules will affect the peak retention and the peak shape in the chromatogram, which may cause errors in the obtained results (e.g. the calculated molecular-weight distributions). In the present work we explored the limitations of UHPLC for the analysis of polymers. Degradation and deformation of macromolecules were studied by collecting and re-injecting polymer peaks and by off-line two-dimensional liquid chromatography. Polystyrene standards with molecular weight of 4 MDa and larger were found to degrade at UHPLC conditions. However, for most polymers degradation could be avoided by using low linear velocities. No degradation of 3-MDa PS (and smaller) was observed at linear velocities up to 7 mm/s. The column frits were implicated as the main sources of polymer degradation. The extent of degradation was found to depend on the type of the column and on the column history. At high flow rates degradation was observed without a column being installed. We demonstrated that polymer deformation preceded degradation. Stretched polymers eluted from the column in slalom chromatography mode (elution order opposite to that in SEC or HDC). Under certain conditions we observed co-elution of large and small PS molecules though a convolution of slalom chromatography and hydrodynamic chromatography. Copyright © 2011 Elsevier B.V. All rights reserved.

  18. Recent advances in fast-switching liquid-crystal mode based on uniform lying helix (ULH) (Conference Presentation)

    Science.gov (United States)

    Wittek, Michael; Siemianowski, Simon; Fiebranz, Bernd; Klasen-Memmer, Melanie

    2017-02-01

    Uniform lying Helix (ULH) is one of the most promising new LC modes for fast switching applications with alternative driving schemes such as FSC (field sequential colour). ULH operates via flexoelectric switching, unlike current commercially available liquid crystal modes that operate via dielectric switching. The realisation of mixtures with suitable flexoelectric properties requires unique materials composed of specially designed ´bi-mesogenś and also the addition of a chiral dopant. Recent advances, updated mixture performance and other challenges such as alignment and driving for this new mode are discussed.

  19. Comparison of separation power of ultra performance liquid chromatography and comprehensive two-dimensional liquid chromatography in the separation of phenolic compounds in beverages.

    Science.gov (United States)

    Kivilompolo, Maarit; Hyötyläinen, Tuulia

    2008-10-01

    In this study, 1-D and 2-D liquid chromatographic systems, namely, conventional HPLC, UPLC, HPLC x HPLC and HPLC x UPLC systems were developed and evaluated for the separation of phenolic acids in wine and juices. In the LC x LC studies, the first dimension separation was based on RPLC and the second dimension was performed with ion-pair chromatography. Three different columns, namely two short columns packed with either 2.5 or 1.7 microm particles and a monolithic column, were tested for the fast second dimension separation. The best results were obtained when the monolithic column was applied for the second dimension separation. The peak capacities for comprehensive 2-D systems varied from 330 to 616.

  20. Home-made online hyphenation of pressurized liquid extraction, turbulent flow chromatography, and high performance liquid chromatography, Cistanche deserticola as a case study.

    Science.gov (United States)

    Song, Qingqing; Li, Jun; Liu, Xiao; Zhang, Yuan; Guo, Liping; Jiang, Yong; Song, Yuelin; Tu, Pengfei

    2016-03-18

    Incompatibility between the conventional pressurized liquid extraction (PLE) devices and high performance liquid chromatography (HPLC) extensively hinders direct and green chemical analysis of herbal materials. Herein, a facile PLE module was configured, and then it was online hyphenated with HPLC via a turbulent flow chromatography (TFC) column. Regarding PLE module, a long PEEK tube (0.13 × 1000 mm) was employed to generate desired pressure (approximately 13.0 MPa) when warm acidic water (70 °C) was delivered as extraction solvent at a high flow rate (2.5 mL/min), and a hollow guard column (3.0 × 4.0 mm) was implemented to hold crude materials. Effluent was collected from the outlet of PEEK tube, concentrated, and subjected onto HPLC coupled with hybrid ion trap-time of flight mass spectrometer to assess the extraction efficiency and also to profile the chemical composition of Cistanche deserticola (CD) that is honored as "Ginseng of the desert". Afterwards, a TFC column was introduced to accomplish online transmission of low molecule weight components from PLE module to HPLC coupled with diode array detection, and two electronic 6-port/2-channel valves were in charge of alternating the whole system between extraction (0-3.0 min) and elution (3.0-35.0 min) phases. Quantitative method was developed and validated for simultaneous determination of eight primary phenylethanoid glycosides in CD using online PLE-TFC-HPLC. All findings demonstrated that the home-made platform is advantageous at direct chemical analysis, as well as time-, solvent-, and material-savings, suggesting a robust tool for chemical fingerprinting of herbs. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. Determination of Alternaria mycotoxins in wine and juice using ionic liquid modified countercurrent chromatography as a pretreatment method followed by high-performance liquid chromatography.

    Science.gov (United States)

    Fan, Chen; Cao, Xueli; Liu, Man; Wang, Wei

    2016-03-04

    Alternariol (AOH), alternariol monomethyl ether (AME), and tenuazonic acid (TeA) are some of the main Alternaria mycotoxins that can be found as contaminants in food materials. The objective of this study was to develop a pretreatment method with countercurrent chromatography (CCC) for enrichment and cleanup of trace Alternaria mycotoxins in food samples prior to high-performance liquid chromatography (HPLC) analysis. An Analytical CCC instrument with a column volume 22.5mL was used, and a two-phase solvent system composed of ethyl acetate and water modified with 6% [HOOMIM][Cl] in mass to volume ratio was selected. Under the optimized CCC operation conditions, trace amounts of AOH, AME, and TeA in large volume of liquid sample were efficiently extracted and enriched in the stationary phase, and then eluted out just by reversing the stationary phase as mobile phase in the opposite flowing direction tail-to-head. The enrichment and elution strategies are unique and can be fulfilled online with high enrichment factors (87-114) and high recoveries (81.14-110.94%). The method has been successively applied to the determination of Alternaria mycotoxins in real apple juice and wine samples with the limits of detection (LOD) in the range of 0.03-0.14μgL(-1). Totally 12 wine samples and 15 apple juice samples from the local market were analyzed. The detection rate of AOH and AME in both kinds of the samples were more than 50%, while TeA was found in relatively high level of 1.75-49.61μgL(-1) in some of the apple juice samples. The proposed method is simple, rapid, and sensitive and could also be used for the analysis and monitoring of Alternaria mycotoxin in other food samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. A high-performance liquid chromatography assay for quantification of cardiac myosin heavy chain isoform protein expression.

    Science.gov (United States)

    Lemon, Douglas D; Papst, Philip J; Joly, Kristin; Plato, Craig F; McKinsey, Timothy A

    2011-01-01

    Stress signaling in the myocardium results in enhanced expression of fetal β-myosin heavy chain (β-MyHC) and reduced expression of adult α-myosin heavy chain (α-MyHC), with the net outcome of diminished myofibrillar ATPase activity and impaired contractility. Pharmacological approaches aimed at preventing this myosin isoform "switch" could provide therapeutic benefit to patients with heart failure. Myosin isoform protein expression is typically quantified using gel electrophoresis methods, which are time-consuming and prone to variability. Here we describe a facile, reversed-phase high-performance liquid chromatography (HPLC) method for rapidly determining the relative amounts of full-length α- and β-MyHC in rat hearts. The assay was validated using cardiac tissues from rats in which a key transcriptional regulator of MyHC expression, the thyroid hormone receptor, was pharmacologically manipulated. This novel assay should facilitate drug discovery efforts focused on the MyHC axis. Copyright © 2010 Elsevier Inc. All rights reserved.

  3. Validation of a Multiresidue Analysis Method for 379 Pesticides in Human Serum Using Liquid Chromatography-Tandem Mass Spectrometry.

    Science.gov (United States)

    Shin, Yongho; Lee, Jonghwa; Lee, Jiho; Lee, Junghak; Kim, Eunhye; Liu, Kwang-Hyeon; Lee, Hye Suk; Kim, Jeong-Han

    2018-04-04

    A screening method for simultaneous analysis of 379 pesticides in human serum was developed using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Electrospray ionization with positive/negative switching mode of LC-MS/MS was adopted, and scheduled multiple reaction monitoring for each target compound was established. The limit of quantitation was 10 ng/mL for 94.5% of the total pesticides, and the correlation coefficients of calibration were ≥0.990 for 93.9% of the pesticides. For the sample preparation, scaled-down QuEChERS were used. Serum (100 μL) was extracted with acetonitrile (400 μL), partitioned with magnesium sulfate (40 mg) and sodium chloride (10 mg), and the upper layer was used for analysis without further cleanup steps. For the accuracy and precision tests, most of the pesticides showed excellent results in intra- and interday conditions. In the recovery tests at 10, 50, and 250 ng/mL, 85.8-91.8% of all target compounds satisfied the recovery range of 70-120% (relative standard deviation ≤20%).

  4. Ionic liquid foam floatation coupled with ionic liquid dispersive liquid-liquid microextraction for the separation and determination of estrogens in water samples by high-performance liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Zhang, Rui; Wang, Chuanliu; Yue, Qiaohong; Zhou, Tiecheng; Li, Na; Zhang, Hanqi; Hao, Xiaoke

    2014-11-01

    An ionic liquid foam floatation coupled with ionic liquid dispersive liquid-liquid microextraction method was proposed for the extraction and concentration of 17-α-estradiol, 17-β-estradiol-benzoate, and quinestrol in environmental water samples by high-performance liquid chromatography with fluorescence detection. 1-Hexyl-3-methylimidazolium tetrafluoroborate was applied as foaming agent in the foam flotation process and dispersive solvent in microextraction. The introduction of the ion-pairing and salting-out agent NH4 PF6 was beneficial to the improvement of recoveries for the hydrophobic ionic liquid phase and analytes. Parameters of the proposed method including concentration of 1-hexyl-3-methylimidazolium tetrafluoroborate, flow rate of carrier gas, floatation time, types and concentration of ionic liquids, salt concentration in samples, extraction time, and centrifugation time were evaluated. The recoveries were between 98 and 105% with relative standard deviations lower than 7% for lake water and well water samples. The isolation of the target compounds from the water was found to be efficient, and the enrichment factors ranged from 4445 to 4632. This developing method is free of volatile organic solvents compared with regular extraction. Based on the unique properties of ionic liquids, the application of foam floatation, and dispersive liquid-liquid microextraction was widened. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Analysis of trace dicyandiamide in stream water using solid phase extraction and liquid chromatography UV spectrometry.

    Science.gov (United States)

    Qiu, Huidong; Sun, Dongdi; Gunatilake, Sameera R; She, Jinyan; Mlsna, Todd E

    2015-09-01

    An improved method for trace level quantification of dicyandiamide in stream water has been developed. This method includes sample pretreatment using solid phase extraction. The extraction procedure (including loading, washing, and eluting) used a flow rate of 1.0mL/min, and dicyandiamide was eluted with 20mL of a methanol/acetonitrile mixture (V/V=2:3), followed by pre-concentration using nitrogen evaporation and analysis with high performance liquid chromatography-ultraviolet spectroscopy (HPLC-UV). Sample extraction was carried out using a Waters Sep-Pak AC-2 Cartridge (with activated carbon). Separation was achieved on a ZIC(®)-Hydrophilic Interaction Liquid Chromatography (ZIC-HILIC) (50mm×2.1mm, 3.5μm) chromatography column and quantification was accomplished based on UV absorbance. A reliable linear relationship was obtained for the calibration curve using standard solutions (R(2)>0.999). Recoveries for dicyandiamide ranged from 84.6% to 96.8%, and the relative standard deviations (RSDs, n=3) were below 6.1% with a detection limit of 5.0ng/mL for stream water samples. Copyright © 2015. Published by Elsevier B.V.

  6. Ultrapreconcentration and determination of organophosphorus pesticides in water by solid-phase extraction combined with dispersive liquid-liquid microextraction and high-performance liquid chromatography.

    Science.gov (United States)

    Chen, Junhua; Zhou, Guangming; Deng, Yongli; Cheng, Hongmei; Shen, Jie; Gao, Yi; Peng, Guilong

    2016-01-01

    Solid-phase extraction coupled with dispersive liquid-liquid microextraction was developed as an ultra-preconcentration method for the determination of four organophosphorus pesticides (isocarbophos, parathion-methyl, triazophos and fenitrothion) in water samples. The analytes considered in this study were rapidly extracted and concentrated from large volumes of aqueous solutions (100 mL) by solid-phase extraction coupled with dispersive liquid-liquid microextraction and then analyzed using high performance liquid chromatography. Experimental variables including type and volume of elution solvent, volume and flow rate of sample solution, salt concentration, type and volume of extraction solvent and sample solution pH were investigated for the solid-phase extraction coupled with dispersive liquid-liquid microextraction with these analytes, and the best results were obtained using methanol as eluent and ethylene chloride as extraction solvent. Under the optimal conditions, an exhaustive extraction for four analytes (recoveries >86.9%) and high enrichment factors were attained. The limits of detection were between 0.021 and 0.15 μg/L. The relative standard deviations for 0.5 μg/L of the pesticides in water were in the range of 1.9-6.8% (n = 5). The proposed strategy offered the advantages of simple operation, high enrichment factor and sensitivity and was successfully applied to the determination of four organophosphorus pesticides in water samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Study of the separation limits of continuous solid support free liquid-liquid chromatography: separation of capsaicin and dihydrocapsaicin by centrifugal partition chromatography.

    Science.gov (United States)

    Goll, Johannes; Frey, Andreas; Minceva, Mirjana

    2013-04-05

    Sequential centrifugal partition chromatography (sCPC) is a cyclic solid support-free liquid-liquid chromatographic process, in which a continuously introduced feed mixture is separated into two sequentially collected product streams. The few experimental demonstrations of this concept already revealed its potential for the preparative separation of pharmaceuticals and fine chemicals. In this work not only the possibilities, but also the limits of the sCPC technology are explored. A feed mixture consisting of capsaicin and dihydrocapsaicin, whose molecular structure differs in only one double bond, was selected for this purpose. The sCPC unit operating parameters needed for a complete separation of the feed mixture were selected using the recently published approach, which uses the partition coefficient of the feed components and the hydrodynamic characteristics of the system as input data. A complete separation of capsaicin and dihydrocapsaicin with the solvent system heptane/ethyl acetate/methanol/water:1/1/1/1 (v/v/v/v) was achieved, although the separation factor was only 1.32. The sCPC unit separation performance was successfully simulated using the cell model. Copyright © 2013 Elsevier B.V. All rights reserved.

  8. Critical comparison of the on-line and off-line molecularly imprinted solid-phase extraction of patulin coupled with liquid chromatography.

    Science.gov (United States)

    Lhotská, Ivona; Holznerová, Anežka; Solich, Petr; Šatínský, Dalibor

    2017-12-01

    Reaching trace amounts of mycotoxin contamination requires sensitive and selective analytical tools for their determination. Improving the selectivity of sample pretreatment steps covering new and modern extraction techniques is one way to achieve it. Molecularly imprinted polymers as selective sorbent for extraction undoubtedly meet these criteria. The presented work is focused on the hyphenation of on-line molecularly imprinted solid-phase extraction with a chromatography system using a column-switching approach. Making a critical comparison with a simultaneously developed off-line extraction procedure, evaluation of pros and cons of each method, and determining the reliability of both methods on a real sample analysis were carried out. Both high-performance liquid chromatography methods, using off-line extraction on molecularly imprinted polymer and an on-line column-switching approach, were validated, and the validation results were compared against each other. Although automation leads to significant time savings, fewer human errors, and required no handling of toxic solvents, it reached worse detection limits (15 versus 6 μg/L), worse recovery values (68.3-123.5 versus 81.2-109.9%), and worse efficiency throughout the entire clean-up process in comparison with the off-line extraction method. The difficulties encountered, the compromises made during the optimization of on-line coupling and their critical evaluation are presented in detail. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Ultrafiltration liquid chromatography combined with high-speed countercurrent chromatography for screening and isolating potential α-glucosidase and xanthine oxidase inhibitors from Cortex Phellodendri.

    Science.gov (United States)

    Li, Sainan; Liu, Chunming; Guo, Liping; Zhang, Yuchi; Wang, Jing; Ma, Bing; Wang, Yueqi; Wang, Yumeng; Ren, Junqi; Yang, Xiaojing; Qin, Yao; Tang, Ying

    2014-09-01

    Cortex Phellodendri is a typical Chinese herb with a large number of alkaloids existing in all parts of it. The most common methods for screening and isolating alkaloids are mostly labor intensive and time consuming. In this study, a new assay based upon ultrafiltration liquid chromatography was developed for the rapid screening of ligands for α-glucosidase and xanthine oxidase. The C. Phellodendri extract was found to contain two alkaloids with both α-glucosidase- and xanthine oxidase binding activities and one lactone with α-glucosidase-binding activity. Subsequently, with the help of high-speed countercurrent chromatography, the specific binding ligands including palmatine, berberine, and obaculactone with purities of 97.38, 96.12, and 96.08%, respectively, were successfully separated. An optimized low-toxicity two-phase solvent system composed of ethyl acetate/n-butanol/ethanol/water (3.5:1.7:0.5:5, v/v/v/v) was used to isolate the three compounds mentioned above from C. Phellodendri. The targeted compounds were identified by liquid chromatography coupled with mass spectrometry and NMR spectroscopy. Therefore, ultrafiltration liquid chromatography combined with high-speed countercurrent chromatography is not only a powerful tool for screening and isolating α-glucosidase and xanthine oxidase inhibitors in complex samples but is also a useful platform for discovering bioactive compounds for the prevention and treatment of diabetes mellitus and gout. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Osteoblast cell membrane chromatography coupled with liquid chromatography and time-of-flight mass spectrometry for screening specific active components from traditional Chinese medicines.

    Science.gov (United States)

    Wang, Nani; Zhang, Qiaoyan; Xin, Hailiang; Shou, Dan; Qin, Luping

    2017-11-01

    A method using osteoblast membrane chromatography coupled with liquid chromatography and time-of-flight mass spectrometry was developed to recognize and identify the specific active components from traditional Chinese medicines. Primary rat osteoblasts were used for the preparation of the stationary phase in the cell chromatography method. Retention components from the cell chromatography were collected and analyzed by liquid chromatography with time-of-flight mass spectrometry. This method was applied in screening active components from extracts of four traditional Chinese medicines. In total, 24 potentially active components with different structures were retained by osteoblast cell chromatography. There were five phenolic glucosides and one triterpenoid saponin from Curculigo orchioides Gaertn, two organic acids and ten flavonoids from Epimedium sagittatum Maxim, one phthalide compound and one organic acid from Angelica sinensis Diels, and two flavonoids and two saponins from Anemarrhena asphodeloides Bunge. Among those, four components (icariin, curculigoside, ferulaic acid, and timosaponin BII) were used for in vitro pharmacodynamics validation. They significantly increased the osteoblast proliferation, alkaline phosphatase activity, levels of bone gla protein and collagen type 1, and promoted mineralized nodule formation. The developed method was an effective screening method for finding active components from complex medicines that act on bone diseases. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Liquid Chromatography-Tandem Mass Spectrometry: An Emerging Technology in the Toxicology Laboratory.

    Science.gov (United States)

    Zhang, Yan Victoria; Wei, Bin; Zhu, Yu; Zhang, Yanhua; Bluth, Martin H

    2016-12-01

    In the last decade, liquid chromatography-tandem mass spectrometry (LC-MS/MS) has seen enormous growth in routine toxicology laboratories. LC-MS/MS offers significant advantages over other traditional testing, such as immunoassay and gas chromatography-mass spectrometry methodologies. Major strengths of LC-MS/MS include improvement in specificity, flexibility, and sample throughput when compared with other technologies. Here, the basic principles of LC-MS/MS technology are reviewed, followed by advantages and disadvantages of this technology compared with other traditional techniques. In addition, toxicology applications of LC-MS/MS for simultaneous detection of large panels of analytes are presented. Copyright © 2016 Elsevier Inc. All rights reserved.

  12. Recent trends in sorption-based sample preparation and liquid chromatography techniques for food analysis.

    Science.gov (United States)

    Maciel, Edvaldo V Soares; de Toffoli, Ana Lúcia; Lanças, Fernando Mauro

    2018-04-20

    The accelerated rising of the world's population increased the consumption of food, thus demanding more rigors in the control of residue and contaminants in food-based products marketed for human consumption. In view of the complexity of most food matrices, including fruits, vegetables, different types of meat, beverages, among others, a sample preparation step is important to provide more reliable results when combined with high performance liquid chromatography separations. An adequate sample preparation step before the chromatographic analysis is mandatory in obtaining higher precision and accuracy in order to improve the extraction of the target analytes, one of the priorities in analytical chemistry. The recent discovery of new materials such as ionic liquids, graphene-derived materials, molecularly imprinted polymers, restricted access media, magnetic nanoparticles, and carbonaceous nanomaterials, provided high sensitivity and selectivity results in an extensive variety of applications. These materials, as well as their several possible combinations, have been demonstrated to be highly appropriate for the extraction of different analytes in complex samples such as food products. The main characteristics and application of these new materials in food analysis will be presented and discussed in this paper. Another topic discussed in this review covers the main advantages and limitations of sample preparation microtechniques, as well as their off-line and on-line combination with high performance liquid chromatography for food analysis. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

  13. Multiple heart-cutting two dimensional liquid chromatography quadrupole time-of-flight mass spectrometry of pyrrolizidine alkaloids.

    Science.gov (United States)

    van de Schans, Milou G M; Blokland, Marco H; Zoontjes, Paul W; Mulder, Patrick P J; Nielen, Michel W F

    2017-06-23

    Pyrrolizidine alkaloids (PAs) and their and the corresponding N-oxides (PAs-ox) are genotoxic plant metabolites which can be present as unwanted contaminants in food products of herbal origin like tea and food supplements. PAs and PAs-ox come in a wide variety of molecular structures including many structural isomers. For toxicity assessment it is important to determine the composition of a sample and to resolve all isomeric PAs and PAs-ox, which is currently not possible in one liquid or gas chromatographic (LC or GC) run. In this study an online two dimensional liquid chromatography quadrupole time-of-flight mass spectrometry (2D-LC QToF-MS) method was developed to resolve isomeric PAs and PAs-ox. After comprehensive column and mobile phase selection a polar endcapped C 18 column was used at pH 3 in the first dimension, and a cross-linked C 18 column at pH 10 in the second dimension. Injection solvents, column IDs, flow rates and temperatures were carefully optimized. The method with column selection valve switching described in this study was able to resolve and visualize 20 individual PAs/PAs-ox (6 sets of isomers) in one 2D-LC QToF-MS run. Moreover, it was shown that all isomeric PAs/PAs-ox could be unambiguously annotated. The method was shown to be applicable for the determination and quantification of isomeric PAs/PAs-ox in plant extracts and could be easily extended to include other PAs and PAs-ox. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. Calculation for liquid-liquid equilibria of quaternary alkane-ethyl acetate-methanol-water systems used in counter-current chromatography.

    Science.gov (United States)

    Chen, Jian; Zhao, Mengqiang; Yu, Yanmei; Li, Zongcheng

    2007-06-01

    The calculation of liquid-liquid equilibrium compositions of solvent systems is very important for the work on counter-current chromatography (CCC), especially the phase composition and volume ratio obtained from liquid-liquid equilibrium calculation. In this work, liquid-liquid equilibria of quaternary Arizona solvent systems, alkane-ethyl acetate-methanol-water, and related ternary systems are correlated and predicted using the non-random two-liquid model (NRTL). Hexane, heptane and isooctane are the used alkanes. The parameters in the model are regressed only with the special systems considered. Detailed comparison with experimental data shows that liquid-liquid equilibria of these systems can be predicted with greatly improved accuracy as compared to the group contribution method (UNIFAC).

  15. Voltage-controlled optical switch in planar nematic liquid crystal film

    Science.gov (United States)

    Shih, Chia-Chi; Chen, Yu-Jen; Wu, Sean; Tsai, Cheng-Che; Jiang, I.-Min

    2009-10-01

    This study presents an integrated device that consists of a directional coupler and an electro-optic switch. The device is designed to include a nematic liquid crystal cell, comprising a grating-like electrode. Applying the appropriate voltage to the cell yields a periodically distributed refractive index. An incident polarized beam will couple to an adjacent channel if it is parallel to the channel. The coupling efficiency is controlled by applied voltage. An obliquely injected polarized beam will be reflected and refracted in the channel, and propagated along a curved path. The route of the beam can be controlled by applying the voltage. A multiport routing was achieved for voltage modulation. In addition, the distribution of refractive index is also investigated by employing conoscopic technique experimentally and numerically.

  16. Optothermal Switching of Cholesteric Liquid Crystals: A Study of Azobenzene Derivatives and Laser Wavelengths

    Directory of Open Access Journals (Sweden)

    Tai-Chieh Huang

    2015-09-01

    Full Text Available The laser-initiated thermal (optothermal switching of cholesteric liquid crystals (CLCs is characterized by using different azobenzene (Azo derivatives and laser wavelengths. Under 405-nm laser irradiation, Azo-doped CLCs undergo phase transition from cholesteric to isotropic. No cis-to-trans photoisomerization occurs when the 405-nm laser irradiation is blocked because only a single laser is used. The fast response of Azo-doped CLCs under the on–off switching of the 405-nm laser occurs because of the optothermal effect of the system. The 660-nm laser, which cannot be used as irradiation to generate the trans–cis photoisomerization of Azo, is used in Anthraquinone (AQ-Azo-doped CLCs to examine the optothermal effect of doped Azo. The results show that the LC-like Azo derivative bearing two methyl groups ortho to the Azo moiety (A4 can greatly lower the clearing temperature and generate large amount of heat in AQ-A4-doped CLCs.

  17. Fundamental studies on the switching in liquid nitrogen environment using vacuum switches for application in future high-temperature superconducting medium-voltage power grids

    International Nuclear Information System (INIS)

    Golde, Karsten

    2016-01-01

    By means of superconducting equipment it is possible to reduce the transmission losses in distribution networks while increasing the transmission capacity. As a result even saving a superimposed voltage level would be possible, which can put higher investment costs compared to conventional equipment into perspective. For operation of superconducting systems it is necessary to integrate all equipment in the cooling circuit. This also includes switchgears. Due to cooling with liquid nitrogen, however, only vacuum switching technology comes into question. Thus, the suitability of vacuum switches is investigated in this work. For this purpose the mechanics of the interrupters is considered first. Material investigations and switching experiments at ambient temperature and in liquid nitrogen supply information on potential issues. For this purpose, a special pneumatic construction is designed, which allows tens of thousands of switching cycles. Furthermore, the electrical resistance of the interrupters is considered. Since the contact system consists almost exclusively of copper, a remaining residual resistance and appropriate thermal losses must be considered. Since they have to be cooled back, an appropriate evaluation is given taking environmental parameters into account. The dielectric strength of vacuum interrupters is considered both at ambient temperature as well as directly in liquid nitrogen. For this purpose different contact distances are set at different interrupter types. A distinction is made between internal and external dielectric strength. Conditioning and deconditioning effects are minimized by an appropriate choice of the test circuit. The current chopping and resulting overvoltages are considered to be one of the few drawbacks of vacuum switching technology. Using a practical test circuit the height of chopping current is determined and compared for different temperatures. Due to strong scattering the evaluation is done using statistical methods. At

  18. Low Density Solvent-Based Dispersive Liquid-Liquid Microextraction for the Determination of Synthetic Antioxidants in Beverages by High-Performance Liquid Chromatography

    Science.gov (United States)

    Çabuk, Hasan; Köktürk, Mustafa

    2013-01-01

    A simple and efficient method was established for the determination of synthetic antioxidants in beverages by using dispersive liquid-liquid microextraction combined with high-performance liquid chromatography with ultraviolet detection. Butylated hydroxy toluene, butylated hydroxy anisole, and tert-butylhydroquinone were the antioxidants evaluated. Experimental parameters including extraction solvent, dispersive solvent, pH of sample solution, salt concentration, and extraction time were optimized. Under optimal conditions, the extraction recoveries ranged from 53 to 96%. Good linearity was observed by the square of correlation coefficients ranging from 0.9975 to 0.9997. The relative standard deviations ranged from 1.0 to 5.2% for all of the analytes. Limits of detection ranged from 0.85 to 2.73 ng mL−1. The method was successfully applied for determination of synthetic antioxidants in undiluted beverage samples with satisfactory recoveries. PMID:23853535

  19. Low Density Solvent-Based Dispersive Liquid-Liquid Microextraction for the Determination of Synthetic Antioxidants in Beverages by High-Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Hasan Çabuk

    2013-01-01

    Full Text Available A simple and efficient method was established for the determination of synthetic antioxidants in beverages by using dispersive liquid-liquid microextraction combined with high-performance liquid chromatography with ultraviolet detection. Butylated hydroxy toluene, butylated hydroxy anisole, and tert-butylhydroquinone were the antioxidants evaluated. Experimental parameters including extraction solvent, dispersive solvent, pH of sample solution, salt concentration, and extraction time were optimized. Under optimal conditions, the extraction recoveries ranged from 53 to 96%. Good linearity was observed by the square of correlation coefficients ranging from 0.9975 to 0.9997. The relative standard deviations ranged from 1.0 to 5.2% for all of the analytes. Limits of detection ranged from 0.85 to 2.73 ng mL−1. The method was successfully applied for determination of synthetic antioxidants in undiluted beverage samples with satisfactory recoveries.

  20. Quantification of PSP toxins in toxic shellfish matrices using post-column oxidation liquid chromatography and pre-column oxidation liquid chromatography methods suggests post-column oxidation liquid chromatography as a good monitoring method of choice.

    Science.gov (United States)

    Rey, Verónica; Botana, Ana M; Botana, Luis M

    2017-04-01

    Different shellfish samples were analyzed by Pre- and Post-Column Oxidation Liquid Chromatography to compare the toxins profiles and get information about the degree of accomplishment of both methods. Comparison of the results obtained, the linear correlation coefficient (r 2  = 0.94) and the paired t test (two tails, α = 0.05), indicated that there were not significant differences between both sets of data. Nevertheless, important differences related to toxins profiles were found: it was remarkable the difference in results for both Gonyautoxins 1 and 4 and Decarbamoylgonyautoxins 2 and 3, depending on the method of choice, due to an overestimation in the Pre-Column method. It was necessary to modify the elution conditions in the Post-Column method to avoid the interference of matrix peaks at retention times closer to the retention times of the calibrants, mostly when working with oyster and scallop matrices, although it is a good method to use routinely. Copyright © 2017 Elsevier Ltd. All rights reserved.

  1. Characterization of rhamnolipids by liquid chromatography/mass spectrometry after solid-phase extraction.

    Science.gov (United States)

    Behrens, Beate; Engelen, Jeannine; Tiso, Till; Blank, Lars Mathias; Hayen, Heiko

    2016-04-01

    Rhamnolipids are surface-active agents with a broad application potential that are produced in complex mixtures by bacteria of the genus Pseudomonas. Analysis from fermentation broth is often characterized by laborious sample preparation and requires hyphenated analytical techniques like liquid chromatography coupled to mass spectrometry (LC-MS) to obtain detailed information about sample composition. In this study, an analytical procedure based on chromatographic method development and characterization of rhamnolipid sample material by LC-MS as well as a comparison of two sample preparation methods, i.e., liquid-liquid extraction and solid-phase extraction, is presented. Efficient separation was achieved under reversed-phase conditions using a mixed propylphenyl and octadecylsilyl-modified silica gel stationary phase. LC-MS/MS analysis of a supernatant from Pseudomonas putida strain KT2440 pVLT33_rhlABC grown on glucose as sole carbon source and purified by solid-phase extraction revealed a total of 20 congeners of di-rhamnolipids, mono-rhamnolipids, and their biosynthetic precursors 3-(3-hydroxyalkanoyloxy)alkanoic acids (HAAs) with different carbon chain lengths from C8 to C14, including three rhamnolipids with uncommon C9 and C11 fatty acid residues. LC-MS and the orcinol assay were used to evaluate the developed solid-phase extraction method in comparison with the established liquid-liquid extraction. Solid-phase extraction exhibited higher yields and reproducibility as well as lower experimental effort.

  2. Methods for peptide and protein quantitation by liquid chromatography-multiple reaction monitoring mass spectrometry.

    Science.gov (United States)

    Zhang, Haixia; Liu, Qinfeng; Zimmerman, Lisa J; Ham, Amy-Joan L; Slebos, Robbert J C; Rahman, Jamshedur; Kikuchi, Takefume; Massion, Pierre P; Carbone, David P; Billheimer, Dean; Liebler, Daniel C

    2011-06-01

    Liquid chromatography-multiple reaction monitoring mass spectrometry of peptides using stable isotope dilution (SID) provides a powerful tool for targeted protein quantitation. However, the high cost of labeled peptide standards for SID poses an obstacle to multiple reaction monitoring studies. We compared SID to a labeled reference peptide (LRP) method, which uses a single labeled peptide as a reference standard for all measured peptides, and a label-free (LF) approach, in which quantitation is based on analysis of un-normalized peak areas for detected MRM transitions. We analyzed peptides from the Escherichia coli proteins alkaline phosphatase and β-galactosidase spiked into lysates from human colon adenocarcinoma RKO cells. We also analyzed liquid chromatography-multiple reaction monitoring mass spectrometry data from a recently published interlaboratory study by the National Cancer Institute Clinical Proteomic Technology Assessment for Cancer network (Addona et al. (2009) Nat. Biotechnol. 27: 633-641), in which unlabeled and isotopically labeled synthetic peptides or their corresponding proteins were spiked into human plasma. SID displayed the highest correlation coefficients and lowest coefficient of variation in regression analyses of both peptide and protein spike studies. In protein spike experiments, median coefficient of variation values were about 10% for SID and 20-30% for LRP and LF methods. Power calculations indicated that differences in measurement error between the methods have much less impact on measured protein expression differences than biological variation. All three methods detected significant (p set of 10 pairs of human lung tumor and control tissues. Further, the LRP and LF methods both detected significant differences (p set of lung tissue samples. The data indicate that the LRP and LF methods provide cost-effective alternatives to SID for many quantitative liquid chromatography-multiple reaction monitoring mass spectrometry

  3. The development of an evaluation method for capture columns used in two-dimensional liquid chromatography.

    Science.gov (United States)

    Cao, Liwei; Yu, Danhua; Wang, Xinliang; Ke, Yanxiong; Jin, Yu; Liang, Xinmiao

    2011-11-07

    Capture columns are important interface tools for on line two-dimensional liquid chromatography (2D-LC). In this study, a systematic method was developed to evaluate and optimize the capture ability of capture columns by off-line method. First, the parameter Δt(R) (Δt(R)=t(2)-t(1)-t(0)-W) was introduced to quantitatively represent the capture ability of the capture column by connecting a capture column behind the first dimensional column. Based on the value of Δt(R), an appropriate capture column was selected after the first dimensional column was fixed. Then, the capture ability of the selected column was promoted by adjusting the mobile phase of the first dimensional column. Capture ability was also optimized using complex sample analysis software system (CSASS) software. Second, the elution mode of the trapped compounds on the capture column was investigated by connecting the capture column before the second dimensional column. More specifically, in mode I, capture column was connected to the second dimension without changing the flow rate direction and the trapped compounds must pass through the capture column and be eluted into the second dimensional column. The contrary connection mode was mode II. It was found that mode I is more suitable method for 2D-LC. Finally, an off-line reversed-phase/hydrophilic interaction liquid chromatography two-dimensional liquid chromatography (RP/HILIC 2D-LC) system with a C18 capture column was developed to demonstrate the practical application of this method. Copyright © 2011 Elsevier B.V. All rights reserved.

  4. Vortex-assisted surfactant-enhanced-emulsification liquid-liquid microextraction of biogenic amines in fermented foods before their simultaneous analysis by high-performance liquid chromatography.

    Science.gov (United States)

    Donthuan, Jaruwan; Yunchalard, Sirinda; Srijaranai, Supalax

    2014-11-01

    A simple, rapid, sensitive, and environmentally friendly method, based on modified dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography was developed for the simultaneous determination of five biogenic amines in fermented food samples. Biogenic amines were derivatized with 9-fluorenylmethyl chloroformate, extracted by vortex-assisted surfactant-enhanced emulsification liquid-liquid microextraction, and then analyzed by high-performance liquid chromatography. Five biogenic amine compounds were separated within 30 min using a C18 column and gradient elution with acetonitrile and 1% acetic acid. Factors influencing the derivatization and extraction efficiency such as type and volume of extraction solvent, type, and concentration of surfactant, pH, salt addition, and vortex time were optimized. Under the optimum conditions, the method provided the enrichment factors in the range of 161-553. Good linearity was obtained from 0.002-0.5 mg/L for cadaverine and tyramine, 0.003-1 mg/L for tryptamine and histamine, and 0.005-1 mg/L for spermidine with coefficient of determination (R(2) ) > 0.992. The limits of detection ranged from 0.0010 to 0.0026 mg/L. The proposed method was successfully applied to analysis of biogenic amines in fermented foods such as fermented fish (plaa-som), wine and beer where good recoveries were obtained in the range of 83.2-112.5% © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Denaturing high-performance liquid chromatography mutation analysis in patients with reduced Protein S levels

    DEFF Research Database (Denmark)

    Bathum, Lise; Münster, Anna-Marie; Nybo, Mads

    2008-01-01

    diagnosis and risk estimation. The aim was to design a high-throughput genetic analysis based on denaturing high-performance liquid chromatography to identify sequence variations in the gene coding for Protein S. PATIENTS: In total, 55 patients referred to the Section of Thrombosis and Haemostasis, Odense......BACKGROUND: Patients with congenital Protein S deficiency have increased risk of venous thromboembolism. However, Protein S levels show large intra-individual variation and the biochemical assays have low accuracy and a high interlaboratory variability. Genetic analysis might aid in a more precise......, giving a precise diagnosis and subsequently a better risk estimation....

  6. Determination of limonin and nomilin contents in different citrus cultivars using high performance liquid chromatography

    International Nuclear Information System (INIS)

    Bilal, H.; Hassan, S.; Sahar, S.; Akram, W.; Sahar, S.

    2013-01-01

    High perlorrnance liquid chromatography (HPLC) analysis was done to quantify the amount of limonoids (nomilin and nomilin) in seven selected citrus cultivars. According to the HPLC analysis red blood orange (Citrus sinensis var red blood orange) had maximum amount of limonin (479.77 ug/rnl.), while rough lemon (Citrus jambhiri) had no limonin content. in case of nomonin, rough lemon (Citrus jambhir) had maximum amount of nomilin (54.23 micro g/ML)) while succari (citrus sinensis var succari) had very low amount of nomilin (0.37 micro g/Ml). (author)

  7. Study of Saiga Horn Using High-Performance Liquid Chromatography with Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Kateřina Mikulíková

    2012-01-01

    Full Text Available The saiga horns have been investigated the using of modern analytic methods. High-performance liquid chromatography (HPLC with mass-spectrometric (MS and MS/MS detection and polyacrylamide gel electrophoresis (PAGE were used. It could be concluded that basic proteins of the saiga horns are keratins and collagen. The basic representation protein in all samples is keratin type I microfibrillar (from sheep, keratin type II microfibrillar (from sheep, collagen type I (α1 (from bovine and collagen type I (α2 (from bovine. Free amino acids we determined in all samples are nontreated by enzyme.

  8. Determination of alpha-Tocopherol (vitamin E) in irradiated garlic by high performance liquid chromatography (HPLC)

    International Nuclear Information System (INIS)

    Rios, Magda Dias Goncalves; Penteado, Marilene de Vuono Camargo

    2003-01-01

    The effects of 60 Co ionizing radiations in doses of 0, 75, 100, 150, 200 and 250Gy on garlic, upon the α-tocopherol concentration were studied. The α-tocopherol contents were established by high performance liquid chromatography (HPLC), after direct hexane extraction from the garlic samples. The α-tocopherol was determined through normal phase column, and mobile phase was composed by hexane: iso-propyl alcohol (99:01 v/v), with 2mL/min flow rate and fluorescence detector. It is statistically shown that an irradiation dose of up to 150 Gy does not affect the garlic α-tocopherol content. (author)

  9. Measurements of urinary adipic acid and suberic acid using high-performance liquid chromatography.

    Science.gov (United States)

    Yoshioka, K; Shimojo, N; Nakanishi, T; Naka, K; Okuda, K

    1994-05-13

    A sensitive and specific method was developed for measuring medium-chain dicarboxylic acids (adipic and suberic acid) in urine. These acids were extracted from urine with diethyl ether and converted into fluorescent derivatives with 9-anthryldiazomethane, which can be separated by high-performance liquid chromatography. The reproducibility was high and the recovery from urine was above 90%. Urinary concentrations of adipic acid in streptozotocin-induced diabetic rats were significantly higher than those in control rats. In diabetic patients, both adipic acid and suberic acid tended to be high, but not significantly. This method should be useful for measuring dicarboxylic acids in urine.

  10. Determination of 90SR in food using extraction chromatography and LSC - Liquid Scintillation Counting

    International Nuclear Information System (INIS)

    Temba, Eliane S.C.; Amaral, Angela M.; Reis Junior, Aluisio S.; Monteiro, Roberto P.G.

    2013-01-01

    A methodology for the determination of 90 Sr in food is described. The procedure involved a preliminary freeze-drying of the samples followed by dry-ashing and sample digestion. The separation procedure was carried out using extraction chromatography with Sr Resin, from Eichrom, and 90 Sr was measured by liquid scintillation counting (LSC). A certified reference material, IAEA-375, was analyzed in order to evaluate the reliability of the method, and the results showed good agreement between the measured and certified values. The chemical yield was above 90% and the typical counting efficiency was 82%. The calculated limit of detection was 4.8 x 10 -3 Bq g -1 . (author)

  11. Determination of sulfonamides in meat by liquid chromatography coupled with atmospheric pressure chemical ionization mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Dal Ho; Choi, Jong Oh; Kim, Jin Seog [Korea Research Institute of Standards and Science, Daejon (Korea, Republic of); Lee, Dai Woon [Yonsei Univ., Seoul (Korea, Republic of)

    2002-11-01

    Liquid chromatography/atmospheric pressure chemical ionization-mass spectrometry (LC-APCI-MS) has been used for the determination of sulfonamides in meat. Five typical sulfonamides were selected as target compounds, and beef meat was selected as a matrix sample. As internal standards, sulfapyridine and isotope labeled sulfamethazine ({sup 13}C{sub 6}-SMZ) were used. Compared to the results of recent reports, our results have shown improved precision to a RSD of 1.8% for the determination of sulfamethazine spiked with 75 ng/g level in meat.

  12. Determination of TBP, HDEHP and TOPO complexed with ferrous thiocyanate by reversed phase liquid chromatography

    International Nuclear Information System (INIS)

    Akliouant, Z.; Meddour, L.; Azzouz, A.

    1992-02-01

    The present work deals with the analysis of some organophosphorus extracting agents, e.g. TBP, HDEHP and TOPO by reversed phase liquid chromatography via previous complexation with ferrous thiocyanate. The absorbance wavelengths of the resulting complexes, i.e. TBP:FeSCNK, HDEHP:FeSCNK and TOPO:FeSCNK are respectively 427, 446 and 487nm. Thus, an improvement of such a technique consists in the organophosphorus compounds detection by colorimetry. Subsequently all products and intermediates present in synthesis media can be easily analysed in the same wavelengths range without previous separation or purification

  13. Increasing flexibility in two-dimensional liquid chromatography by pulsed elution of the first dimension

    DEFF Research Database (Denmark)

    Jakobsen, Simon S.; Christensen, Jan H.; Verdier, Sylvain

    2017-01-01

    This work demonstrates the development of an online two-dimensional liquid chromatography (2D-LC) method where the first dimension column is eluted by a sequence of pulses of increasing eluotropic strength generated by the LC pumps (pulsed-elution 2D-LC). Between the pulses, the first dimension...... online comprehensive 2D-LC: undersampling, difficulties in refocusing, and lack of flexibility in the selection of column dimensions and flow rates because the two dimensions constrain each other. The pulsed-elution 2D-LC was applied for the analysis of a basic fraction of vacuum gas oil. Peak capacity...

  14. Off-line mixed-mode liquid chromatography coupled with reversed phase high performance liquid chromatography-high resolution mass spectrometry to improve coverage in lipidomics analysis.

    Science.gov (United States)

    Narváez-Rivas, Mónica; Vu, Ngoc; Chen, Guan-Yuan; Zhang, Qibin

    2017-02-15

    The confident identification and in-depth profiling of molecular lipid species remain to be a challenge in lipidomics analysis. In this work, an off-line two-dimensional mixed-mode and reversed-phase liquid chromatography (RPLC) method combined with high-field quadrupole orbitrap mass spectrometer (Q Exactive HF) was developed to profile lipids from complex biological samples. In the first dimension, 22 different lipid classes were separated on a monolithic silica column with elution order from neutral to polar lipids. A total of 13 fractions were collected and run on a RPLC C30 column in the second dimension for further separation of the lipid molecular species based on their hydrophobicity, with the elution order being determined by both the length and degree of unsaturation in the fatty-acyl chain. The method was applied to analyze lipids extracted from rat plasma and rat liver. Fatty acid methyl ester analysis by gas chromatography-mass spectrometry was used to identify the fatty acyls from total lipid extracts, which provided a more confident identification of the lipid species present in these samples. More than 800 lipids were identified in each sample and their molecular structures were confidentially confirmed using tandem mass spectrometry (MS/MS). The number of lipid molecular species identified in both rat plasma and rat liver by this off-line two-dimensional method is approximately twice of that by one-dimensional RPLC-MS/MS employing a C30 column. This off-line two-dimensional mixed-mode LC-RPLC-MS/MS method is a promising technique for comprehensive lipid profiling in complex biological matrices. Copyright © 2016 Elsevier B.V. All rights reserved.

  15. Salting-out homogenous extraction followed by ionic liquid/ionic liquid liquid-liquid micro-extraction for determination of sulfonamides in blood by high performance liquid chromatography.

    Science.gov (United States)

    Liu, Zhongling; Yu, Wei; Zhang, Hanqi; Gu, Fanbin; Jin, Xiangqun

    2016-12-01

    Salting-out homogenous extraction followed by ionic liquid/ionic liquid dispersive liquid-liquid micro-extraction system was developed and applied to the extraction of sulfonamides in blood. High-performance liquid chromatography was applied to the determination of the analytes. The blood sample was centrifuged to obtain the serum. After the proteins in the serum were removed in the presence of acetonitrile, ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate, dipotassium hydrogen phosphate, ionic liquid 1-Hexyl-3-methylimidazolium hexafluorophosphate were added into the resulting solution. After the resulting mixture was ultrasonically shaken and centrifuged, the precipitate was separated. The acetonitrile was added in the precipitate and the analytes were extracted into the acetonitrile phase. The parameters affecting the extraction efficiency, such as volume of ionic liquid, amount of dipotassium hydrogen phosphate, volume of dispersant, extraction time and temperature were investigated. The limits of detection of sulfamethizole (STZ), sulfachlorpyridazine (SCP), sulfamethoxazole (SMX) and Sulfisoxazole (SSZ) were 4.78, 3.99, 5.21 and 3.77μgL -1 , respectively. When the present method was applied to the analysis of real blood samples, the recoveries of analytes ranged from 90.0% to 113.0% and relative standard deviations were lower than 7.2%. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Quantitative Analysis of Tetramethylenedisulfotetramine ("Tetramine") Spiked into Beverages by Liquid Chromatography Tandem Mass Spectrometry with Validation by Gas Chromatography Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Owens, J; Hok, S; Alcaraz, A; Koester, C

    2008-11-13

    Tetramethylenedisulfotetramine, commonly known as tetramine, is a highly neurotoxic rodenticide (human oral LD{sub 50} = 0.1 mg/kg) used in hundreds of deliberate food poisoning events in China. Here we describe a method for quantitation of tetramine spiked into beverages, including milk, juice, tea, cola, and water and cleaned up by C8 solid phase extraction and liquid-liquid extraction. Quantitation by high performance liquid chromatography tandem mass spectrometry (LC/MS/MS) was based upon fragmentation of m/z 347 to m/z 268. The method was validated by gas chromatography mass spectrometry (GC/MS) operated in SIM mode for ions m/z 212, 240, and 360. The limit of quantitation was 0.10 {micro}g/mL by LC/MS/MS versus 0.15 {micro}g/mL for GC/MS. Fortifications of the beverages at 2.5 {micro}g/mL and 0.25 {micro}g/mL were recovered ranging from 73-128% by liquid-liquid extraction for GC/MS analysis, 13-96% by SPE and 10-101% by liquid-liquid extraction for LC/MS/MS analysis.

  17. Quantitative Analysis of Tetramethylenedisulfotetramine ('Tetramine') Spiked into Beverages by Liquid Chromatography Tandem Mass Spectrometry with Validation by Gas Chromatography Mass Spectrometry

    International Nuclear Information System (INIS)

    Owens, J.; Hok, S.; Alcaraz, A.; Koester, C.

    2008-01-01

    Tetramethylenedisulfotetramine, commonly known as tetramine, is a highly neurotoxic rodenticide (human oral LD 50 = 0.1 mg/kg) used in hundreds of deliberate food poisoning events in China. Here we describe a method for quantitation of tetramine spiked into beverages, including milk, juice, tea, cola, and water and cleaned up by C8 solid phase extraction and liquid-liquid extraction. Quantitation by high performance liquid chromatography tandem mass spectrometry (LC/MS/MS) was based upon fragmentation of m/z 347 to m/z 268. The method was validated by gas chromatography mass spectrometry (GC/MS) operated in SIM mode for ions m/z 212, 240, and 360. The limit of quantitation was 0.10 (micro)g/mL by LC/MS/MS versus 0.15 (micro)g/mL for GC/MS. Fortifications of the beverages at 2.5 (micro)g/mL and 0.25 (micro)g/mL were recovered ranging from 73-128% by liquid-liquid extraction for GC/MS analysis, 13-96% by SPE and 10-101% by liquid-liquid extraction for LC/MS/MS analysis.

  18. Novel materials and methods for solid-phase extraction and liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Ambrose, Diana [Iowa State Univ., Ames, IA (United States)

    1997-06-24

    This report contains a general introduction which discusses solid-phase extraction and solid-phase micro-extraction as sample preparation techniques for high-performance liquid chromatography, which is also evaluated in the study. This report also contains the Conclusions section. Four sections have been removed and processed separately: silicalite as a sorbent for solid-phase extraction; a new, high-capacity carboxylic acid functionalized resin for solid-phase extraction; semi-micro solid-phase extraction of organic compounds from aqueous and biological samples; and the high-performance liquid chromatographic determination of drugs and metabolites in human serum and urine using direct injection and a unique molecular sieve.

  19. Preparation of a silica stationary phase co-functionalized with Wulff-type phenylboronate and C12 for mixed-mode liquid chromatography.

    Science.gov (United States)

    Li, Hengye; Zhang, Xuemeng; Zhang, Lin; Wang, Xiaojin; Kong, Fenying; Fan, Dahe; Li, Lei; Wang, Wei

    2017-04-15

    A silica stationary phase was designed and synthesized through the co-functionalization of silica with Wulff-type phenylboronate and C12 for mixed-mode liquid chromatography applications. The as-synthesized stationary phase was characterized by elemental analysis and Fourier Transform-InfraRed Spectroscopy (FT-IR). Retention mechanisms, including boronate affinity (BA), reversed-phase (RP) and anion-exchange (AE), were involved. Retention mechanism switching was easily realized by adjustment of the mobile phase constitution. Cis-diol compounds could be selectively captured under neutral conditions in BA mode and off-line separated in RP mode. Neutral, basic, acidic and amphiprotic compounds were chromatographed on the column in RP chromatography, while inorganic anions were chromatographed in AE chromatography to characterize the mixed-mode nature of the prepared stationary phase. In addition, the RP performance was compared with an octadecyl silica column in terms of column efficiency (N/m), asymmetry factor (A f ), retention factor (k) and resolution (Rs). The prepared stationary phase offered multiple interactions with analytes in addition to hydrophobic interactions under RP elution conditions. Based on the mixed-mode properties, off-line 2D-LC, for selective capture and separation of urinary nucleosides, was successfully realized on a single column, demonstrating its powerful application potential for complex samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Application of high-speed counter-current chromatography coupled with high-performance liquid chromatography-diode array detection for the preparative isolation and purification of hyperoside from Hypericum perforatum with online purity monitoring.

    Science.gov (United States)

    Zhou, Tingting; Chen, Bin; Fan, Guorong; Chai, Yifeng; Wu, Yutian

    2006-05-26

    Following preparative isolation and purification by high-speed counter-current chromatography (HSCCC), the collected fractions were generally analyzed by high-performance liquid chromatography (HPLC) to determine the relative purities of each fraction. Our paper reports for the first time a preparative isolation-purity detection hyphenated system: online coupling of HSCCC with high-performance liquid chromatography-diode array detection (HSCCC-HPLC-DAD). The introduction of online purity analysis in HSCCC has dramatically improved the efficiency of this technique by overcoming the drawbacks of post analysis in HSCCC isolation. The effluent from the outlet of HSCCC was splitted into two parts: one was collected, while the other was introduced directly into an HPLC-DAD system for purity analysis through a switch valve. Therefore, the purities of the obtained fractions from HSCCC were monitored, and fractions with high purities were collected. This strategy has been successfully demonstrated with the preparative isolation and purification of hyperoside from Hypericum perforatum (St. Jone's Wort); a model of TBE-300A HSCCC was used to isolate and separate hyperoside from H. perforatum with a two-phase solvent system composed of ethyl acetate-ethanol-water at the volume ratio of 5:1:5 (v/v) using online detection technique. The isolation was done in less than 3.5 h, and a total of 83.0-mg hyperoside at over 99.0% purity was yielded from 300 mg of the partially purified extract. This new strategy possesses general utility in the preparation of bioactive compounds from traditional Chinese medicine (TCM).

  1. Analysis of trace inorganic anions in weak acid salts by single pump cycling-column-switching ion chromatography.

    Science.gov (United States)

    Huang, Zhongping; Ni, Chengzhu; Zhu, Zhuyi; Pan, Zaifa; Wang, Lili; Zhu, Yan

    2015-05-01

    The application of ion chromatography with the single pump cycling-column-switching technique was described for the analysis of trace inorganic anions in weak acid salts within a single run. Due to the hydrogen ions provided by an anion suppressor electrolyzing water, weak acid anions could be transformed into weak acids, existing as molecules, after passing through the suppressor. Therefore, an anion suppressor and ion-exclusion column were adopted to achieve on-line matrix elimination of weak acid anions with high concentration for the analysis of trace inorganic anions in weak acid salts. A series of standard solutions consisting of target anions of various concentrations from 0.005 to 10 mg/L were analyzed, with correlation coefficients r ≥ 0.9990. The limits of detection were in the range of 0.67 to 1.51 μg/L, based on the signal-to-noise ratio of 3 and a 25 μL injection volume. Relative standard deviations for retention time, peak area, and peak height were all less than 2.01%. A spiking study was performed with satisfactory recoveries between 90.3 and 104.4% for all anions. The chromatographic system was successfully applied to the analysis of trace inorganic anions in five weak acid salts. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Determination of trace inorganic anions in weak acids by single-pump column-switching ion chromatography.

    Science.gov (United States)

    Zhu, Haibao; Chen, Huadong; Zhong, Yingying; Ren, Dandan; Qian, Yaling; Tang, Hongfang; Zhu, Yan

    2010-08-01

    Ion chromatography has been proposed for the determination of three common inorganic anions (chloride, nitrate, and sulfate) in nine weak acids (tartaric acid, citric acid, formic acid, acetic acid, metacetonic acid, butyric acid, butanedioic acid, hexafluorophosphoric acid, and salicylic acid) using a single pump, two valves, a single eluent, and a single conductivity detector. The present system uses ion exclusion, concentrator, and anion-exchange columns connected in series via 6-port and 10-port valves in a Dionex ICS-2100 ion chromatograph. The valves were switched for the determination of three inorganic anions from weak acids in a single chromatographic run. Sample matrices of weak acids with a series of concentrations can be investigated. Complete separations of the previously mentioned anions are demonstrated within 40 min. Under the optimum conditions, the relative standard deviation values ranged from 1.3 to 3.8%. The detection limits of the three inorganic anions (S/N = 3) were in the range of 0.3-1.7 microg/L. The recoveries were in the range of 75.2-117.6%. With this system, automation for routine analysis, short analysis time, and low cost can be achieved.

  3. Analysis of lignans in Magnoliae Flos by turbulent flow chromatography with online solid-phase extraction and high-performance liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Zhou, Xuan; Chen, Cen; Ye, Xiaolan; Song, Fenyun; Fan, Guorong; Wu, Fuhai

    2016-04-01

    In this study, a method coupling turbulent flow chromatography with online solid-phase extraction and high-performance liquid chromatography with tandem mass spectrometry was developed for analyzing the lignans in Magnoliae Flos. By the online pretreatment of turbulent flow chromatography solid-phase extraction, the impurities removal and analytes concentration were automatically processed, and the lignans were separated rapidly and well. Seven lignans of Magnoliae Flos including epieudesmin, magnolin, 1-irioresinol-B-dimethyl ether, epi-magnolin, fargesin aschantin, and demethoxyaschantin were identified by comparing their retention behavior, UV spectra, and mass spectra with those of reference substances or literature data. The developed method was validated, and the good results showed that the method was not only automatic and rapid, but also accurate and reliable. The turbulent flow chromatography with online solid-phase extraction and high-performance liquid chromatography with tandem mass spectrometry method holds a high potential to become an effective method for the quality control of lignans in Magnoliae Flos and a useful tool for the analysis of other complex mixtures. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Simultaneous determination of ramipril, ramiprilat and telmisartan in human plasma using liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Gupta, V K; Jain, Rajeev; Lukram, Ojitkumar; Agarwal, Shilpi; Dwivedi, Ashish

    2011-01-15

    A rapid and sensitive liquid chromatography tandem mass spectrometry method has been developed and validated for the simultaneous determination of ramipril, ramiprilat and telmisartan in human plasma. The solid-phase extraction technique was used for the extraction of ramipril, ramiprilat and telmisartan from human plasma. Trandolaprilat and hydrochlorothiazide were used as the internal standards (ISs). Chromatography was performed on a Hypurity C18, 5 μm, 50 mm × 4.6mm column, with the mobile phase consisting of ammonium acetate and acetonitrile (in a 20:80 ratio), followed by detection using mass spectrometry. The method involves a simple reversed isocratic chromatography condition and mass spectrometry detection, which enables detection at sub-nanogram levels. The method was validated and the lower limit of quantification for ramipril, ramiprilat and telmisartan was found to be 0.1 ng mL(-1), 0.1 ng mL(-1) and 2 ng mL(-1), respectively. The mean recovery for ramipril, ramiprilat and telmisartan ranged from 90.1 to 104.1%. This method increased the sensitivity and selectivity; resulting in high-throughput analysis of ramipril, ramiprilat and telmisartan using two different ISs in a single experiment for bioequivalence studies, with a chromatographic run time of 1.5 min only. Copyright © 2010 Elsevier B.V. All rights reserved.

  5. Enhanced fluidity liquid chromatography of inulin fructans using ternary solvent strength and selectivity gradients.

    Science.gov (United States)

    Bennett, Raffeal; Olesik, Susan V

    2018-01-25

    The value of exploring selectivity and solvent strength ternary gradients in enhanced fluidity liquid chromatography (EFLC) is demonstrated for the separation of inulin-type fructans from chicory. Commercial binary pump systems for supercritical fluid chromatography only allow for the implementation of ternary solvent strength gradients which can be restrictive for the separation of polar polymeric analytes. In this work, a custom system was designed to extend the capability of EFLC to allow tuning of selectivity or solvent strength in ternary gradients. Gradient profiles were evaluated using the Berridge function (RF 1 ), normalized resolution product (NRP), and gradient peak capacity (P c ). Selectivity gradients provided the separation of more analytes over time. The RF 1 function showed favor to selectivity gradients with comparable P c to that of solvent strength gradients. NRP did not strongly correlate with P c or RF 1 score. EFLC with the hydrophilic interaction chromatography, HILIC, separation mode was successfully employed to separate up to 47 fructan analytes in less than 25 min using a selectivity gradient. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. Description of adsorption in liquid chromatography under non-ideal conditions.

    Science.gov (United States)

    Ortner, Franziska; Ruppli, Chantal; Mazzotti, Marco

    2018-04-17

    A thermodynamically consistent description of binary adsorption in reversed phase chromatography is presented, accounting for thermodynamic nonidealities in the liquid and the adsorbed phase. The investigated system involves the adsorbent Zorbax 300SB-C18, as well as phenetole (PNT) and 4-tert-butylphenol (TBP) as solutes and methanol and water as inert components forming the eluent. The description is based on adsorption isotherms which are a function of the liquid phase activities, in order to account for non-idealities in the liquid phase. Liquid phase activities are calculated with a UNIQUAC model established in this work, based on experimental phase equilibrium data. The binary interaction in the adsorbed phase is described by the adsorbed solution theory (AST), assuming an ideal (IAST) or real (RAST) adsorbed phase. Implementation of the established adsorption model in a chromatographic code achieves a quantitative description of experimental elution profiles, with feed compositions exploiting the entire miscible region, and involving a broad range of different eluent compositions (ratio methanol:water). The quantitative agreement of model and experimental data serves as a confirmation of the underlying physical (thermodynamic) concepts, and of their applicability to a broad range of operating conditions.

  7. [Simultaneous determination of pantothenic acid and D-panthenol in cosmetics by high performance liquid chromatography].

    Science.gov (United States)

    Mao, Xiqin; Hu, Xia; Pan, Wei

    2010-11-01

    A high performance liquid chromatographic method (HPLC) and sample pretreatment method were developed for the simultaneous determination of pantothenic acid (vitamin B5) and D-panthenol (provitamin B5) in cosmetics with different matrices (including of creams, lotions, aqueous cosmetics, oily cosmetics, wax-based cosmetics, nail polish etc). A liquid-liquid extraction system composed of water and water-immiscible solvent was used to preliminarily separate the target components from other oil-soluble components and surfactants in cosmetics, then macromolecular water-soluble matrices in cosmetics were removed by coprecipitation with potassium ferrocyanide-zinc acetate precipitating agent, and then under acid condition, pantothenic acid and D-panthenol were enriched on a C18 solid-phase extraction sorbent. After the removal of other water-soluble impurities, target components were eluted by 40% methanol and then separated and quantitatively analyzed by high performance liquid chromatography with external standard method. Good linear relationship was achieved in the concentration range of 0.1-10 microg/g for pantothenic acid and D-panthenol. The linear correlation coefficients were separately 0.998 9 and 0.999 6. The average recoveries of the target components in cosmetics were more than 90%. Limit of detection of the method was 30 microg/g and the limit of quantification was 100 microg/g. This method can be used to simultaneously determine pantothenic acid and D-panthenol in cosmetics. The results are accurate and reliable.

  8. Safety concerns in ultrahigh pressure capillary liquid chromatography using air-driven pumps.

    Science.gov (United States)

    Xiang, Yanqiao; Maynes, Daniel R; Lee, Milton L

    2003-04-04

    Ultrahigh pressure liquid chromatography (UHPLC) is an emerging technique which utilizes pressures higher than 10,000 p.s.i. to overcome the flow resistance imposed when using very small particles as packing materials in fused-silica capillary columns (1 p.s.i.=6894.76 Pa). This technique has demonstrated exceptionally high separation speeds and chromatographic efficiencies. However, safety is a concern when extremely high pressures are used. In this study, the safety aspects of capillary column rupture during operation were identified and carefully evaluated. First, liquid jets may be formed as a result of blow-out of the on-column frits or from rupture of the capillary at or near the column inlet. Second, incorrect installation of the capillary at the injector, failure of the ferrule used in the capillary connection, or rupture of the capillary can produce high speed projectiles of silica particles or column fragments. Experiments were carried out in the laboratory to produce liquid (water) jets and capillary projectiles using a UHPLC system, and the power density, an important parameter describing water jets in industrial practice, was calculated. Experimental results were in accordance with theoretical calculations. Both indicated that water jets and capillary projectiles under ultrahigh pressures might lead to skin penetration under limited conditions. The use of a plexiglass shroud to cover an initial length of the installed capillary column can eliminate any safety-related concerns about liquid jets or capillary projectiles.

  9. Rapid determination of some psychotropic drugs in complex matrices by tandem dispersive liquid-liquid microextraction followed by high performance liquid chromatography.

    Science.gov (United States)

    Asghari, Alireza; Fahimi, Ebrahim; Bazregar, Mohammad; Rajabi, Maryam; Boutorabi, Leila

    2017-05-01

    Simple and rapid determinations of some psychotropic drugs in some pharmaceutical wastewater and human plasma samples were successfully accomplished via the tandem dispersive liquid-liquid microextraction combined with high performance liquid chromatography-ultraviolet detection (TDLLME-HPLC-UV). TDLLME of the three psychotropic drugs clozapine, chlorpromazine, and thioridazine was easily performed through two consecutive dispersive liquid-liquid microextractions. By performing this convenient method, proper sample preconcentrations and clean-ups were achieved in just about 7min. In order to achieve the best extraction efficiency, the effective parameters involved were optimized. The optimal experimental conditions consisted of 100μL of CCl 4 (as the extraction organic solvent), and the pH values of 13 and 2 for the donor and acceptor phases, respectively. Under these optimum experimental conditions, the proposed TDLLME-HPLC-UV technique provided a good linearity in the range of 5-3000ngmL -1 for the three psychotropic drugs with the correlation of determinations (R 2 s) higher than 0.996. The limits of quantification (LOQs) and limits of detection (LODs) obtained were 5.0ngmL -1 and 1.0-1.5ngmL -1 , respectively. Also the proper enrichment factors (EFs) of 96, 99, and 88 for clozapine, chlorpromazine, and thioridazine, respectively, and good extraction repeatabilities (relative standard deviations below 9.3%, n=5) were obtained. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Homochiral metal-organic framework used as a stationary phase for high-performance liquid chromatography.

    Science.gov (United States)

    Kong, Jiao; Zhang, Mei; Duan, Ai-Hong; Zhang, Jun-Hui; Yang, Rui; Yuan, Li-Ming

    2015-02-01

    Metal-organic frameworks are promising porous materials. Chiral metal-organic frameworks have attracted considerable attention in controlling enantioselectivity. In this study, a homochiral metal-organic framework [Co(2) (D-cam)(2) (TMDPy)] (D-cam = D-camphorates, TMDPy = 4,4'-trimethylenedipyridine) with a non-interpenetrating primitive cubic net has been used as a chiral stationary phase in high-performance liquid chromatography. It has allowed the successful separation of six positional isomers and six chiral compounds. The good selectivity and baseline separation, or at least 60% valley separation, confirmed its excellent molecular recognition characteristics. The relative standard deviations for the retention time of run-to-run and column-to-column were less than 1.8 and 3.1%, respectively. These results demonstrate that [Co(2) (D-cam)(2) (TMDPy)] may represent a promising chiral stationary phase for use in high-performance liquid chromatography. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Hb A1c Separation by High Performance Liquid Chromatography in Hemoglobinopathies

    Directory of Open Access Journals (Sweden)

    Vani Chandrashekar

    2016-01-01

    Full Text Available Hb A1c measurement is subject to interference by hemoglobin traits and this is dependent on the method used for determination. In this paper we studied the difference between Hb A1c measured by HPLC in hemoglobin traits and normal chromatograms. We also studied the correlation of Hb A1c with age. Hemoglobin analysis was carried out by high performance liquid chromatography. Spearman’s rank correlation was used to study correlation between A1c levels and age. Mann-Whitney U test was used to study the difference in Hb A1c between patients with normal hemoglobin and hemoglobin traits. A total of 431 patients were studied. There was positive correlation with age in patients with normal chromatograms only. No correlation was seen in Hb E trait or beta thalassemia trait. No significant difference in Hb A1c of patients with normal chromatograms and patients with hemoglobin traits was seen. There is no interference by abnormal hemoglobin in the detection of A1c by high performance liquid chromatography. This method cannot be used for detection of A1c in compound heterozygous and homozygous disorders.

  12. DETECTION AND QUANTIFICATION OF PHYTOCHEMICAL MARKERS OF Ilex paraguariensis BY LIQUID CHROMATOGRAPHY

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    Rodrigo M. C. Pinto

    2015-11-01

    Full Text Available Ilex paraguariensis (yerba-mate is used as a beverage, and its extract requires adequate quality control methods in order to guarantee quality and safe use. Strategies to develop and optimize a chromatographic method to quantify theobromine, caffeine, and chlorogenic acid in I. paraguariensis extracts were evaluated by applying a quality by design (QbD model and ultra high-performance liquid chromatography (UHPLC. The presence of these three phytochemical markers in the extracts was evaluated using UHPLC-MS and was confirmed by the chromatographic bands in the total ion current traces (m/z of 181.1 [M+H]+, 195.0 [M+H]+, and 353.0 [M−H]−, respectively. The developed method was then transferred to a high-performance liquid chromatography (HPLC platform, and the three phytochemical markers were used as external standards in the validation of a method for analyses of these compounds in extracts using a diode array detector (DAD. The validated method was applied to quantify the chlorogenic acid, caffeine, and theobromine in the samples. HPLC-DAD chromatographic fingerprinting was also used in a multivariate approach to process the entire data and to separate the I. paraguariensis extracts into two groups. The developed method is very useful for qualifying and quantifying I. paraguariensis extracts.

  13. [Rapid determination of 8 urinary carbamate pesticides by liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Liu, Hualiang; Wang, Yuan; Zhu, Baoli

    2015-11-01

    To establish a method for simultaneously determining the urinary concentrations of 8 carbamate pesticides. After being purified by acetonitrile precipitation, urine samples were transferred to a liquid chromatography-tandem mass spectrometry system, and the concentrations of 8 carbamate pesticides were determined by external standard method. A C18 column was used for ultra-high-performance liquid chromatography; methanol/ammonium acetate solution was used as the mobile phase for gradient elution; the mass spectrometer was operated in a multi-reaction monitoring mode. The calibration curves were linear when the urinary concentrations of these carbamate pesticides were 20~800 µg/L, and the recovery rates were 61.0%~121% at spiked levels of 20, 200 and 800 µg/L, with a relative standard deviation of 1.7%~5.5%. This determination method meets the Guide for establishing occupational health standards-part 5: Determination methods of chemicals in biological materials, and can be used for simultaneous determination of 8 carbamate pesticides in the urine of poisoning patients.

  14. Development of Hydrophilic Interaction Liquid Chromatography Method for the Analysis of Moxonidine and Its Impurities

    Directory of Open Access Journals (Sweden)

    Slavica Filipic

    2016-01-01

    Full Text Available Fast and simple hydrophilic interaction liquid chromatography (HILIC method was developed and validated for the analysis of moxonidine and its four impurities (A, B, C, and D in pharmaceutical dosage form. All experiments were performed on the Agilent Technologies 1200 high-performance liquid chromatography (HPLC system using Zorbax RX-SIL, 250 mm × 4.6 mm, 5 μm column as stationary phase (T=25°C, F=1 mL/min, and λ=255 nm, and mixture of acetonitrile and 40 mM ammonium formate buffer (pH 2.8 80 : 20 (v/v as mobile phase. Under the optimal chromatographic conditions, selected by central composite design, separation and analysis of moxonidine and its four impurities are enabled within 12 minutes. Validation of the method was conducted in accordance with ICH guidelines. Based on the obtained results selectivity, linearity (r≥0.9976, accuracy (recovery: 93.66%–114.08%, precision (RSD: 0.56%–2.55%, and robustness of the method were confirmed. The obtained values of the limit of detection and quantification revealed that the method can be used for determination of impurities levels below 0.1%. Validated method was applied for determination of moxonidine and its impurities in commercially available tablet formulation. Obtained results confirmed that validated method is fast, simple, and reliable for analysis of moxonidine and its impurities in tablets.

  15. Validation of a technique by high-performance liquid chromatography for the determination of total isoflavones

    Directory of Open Access Journals (Sweden)

    Pilar A. Soledispa Cañarte

    2017-04-01

    Full Text Available Context: Isoflavones may act as selective regulators in the prevention of various diseases. The most important source of isoflavones is the soy, from which different phytotherapeutics are elaborated of use in Ecuadorian population. However, its concentration varies depending on several factors, therefore quality assessment need to be carried out through out several analytical methods. Aims: To validate an analytical method by high precision liquid chromatography (HPLC to quantify total isoflavones in herbal medicine. Methods: To quantify isoflavones, it was used a brand liquid chromatography with UV/VIS detector at 260 nm, C-18 column using isocratic method. The mobile phase was composed of 2% acetic acid: acetonitrile (75:25. The quantification was performed against reference standard. The parameters for the validation followed the established in the USP 33. Results: The chromatogram presented six peaks with elution between 1.557 and 18.913 min. The linearity of the system and the method got r2 equal to 0.98 and 0.99 respectively. The coefficients of variation 1.5% in the study of repetitiveness and 2% in intermediate precision. The accuracy of the adjusted lineal model exhibited r=0.95 and intercept reliable interval (-0.921; 1.743. Conclusions: The validated method was specific, accurate, precise and linear. It can be used for quality control and stability studies of isoflavones present in herbal medicine.

  16. Microfluidic platform for liquid chromatography-tandem mass spectrometry analyses of complex peptide mixtures.

    Science.gov (United States)

    Xie, Jun; Miao, Yunan; Shih, Jason; Tai, Yu-Chong; Lee, Terry D

    2005-11-01

    A microfluidic chip that integrates all the fluidic components of a gradient liquid chromatography (LC) system is described. These chips were batch-fabricated on a silicon wafer using photolithographic processes and with Parylene as the main structural material. The fabricated chip includes three electrolysis-based electrochemical pumps, one for loading the sample and the other two for delivering the solvent gradient; platinum electrodes for delivering current to the pumps and establishing the electrospray potential; a low-volume static mixer; a column packed with silica-based reversed-phase support; integrated frits for bead capture; and an electrospray nozzle. The fabricated structures were able to withstand pressures in excess of 250 psi. The device was used to perform a liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis of a mixture of peptides from the trypsin digestion of bovine serum albumen (BSA). Gradient elution through the 1.2-cm column was performed at a flow rate of 80 nL/min. Compared to the analysis of the same sample using a commercial nanoflow LC system, the chromatographic resolution was nearly as good, and the total cycle time was significantly reduced because of the minimal volume between the pumps and the column. Results demonstrate the potential of mass-produced, low-cost microfluidic systems capable of performing LC separations for proteomics applications.

  17. Targeted liquid chromatography tandem mass spectrometry to quantitate wheat gluten using well-defined reference proteins.

    Directory of Open Access Journals (Sweden)

    Kathrin Schalk

    Full Text Available Celiac disease (CD is an inflammatory disorder of the upper small intestine caused by the ingestion of storage proteins (prolamins and glutelins from wheat, barley, rye, and, in rare cases, oats. CD patients need to follow a gluten-free diet by consuming gluten-free products with gluten contents of less than 20 mg/kg. Currently, the recommended method for the quantitative determination of gluten is an enzyme-linked immunosorbent assay (ELISA based on the R5 monoclonal antibody. Because the R5 ELISA mostly detects the prolamin fraction of gluten, a new independent method is required to detect prolamins as well as glutelins. This paper presents the development of a method to quantitate 16 wheat marker peptides derived from all wheat gluten protein types by liquid chromatography tandem mass spectrometry (LC-MS/MS in the multiple reaction monitoring mode. The quantitation of each marker peptide in the chymotryptic digest of a defined amount of the respective reference wheat protein type resulted in peptide-specific yields. This enabled the conversion of peptide into protein type concentrations. Gluten contents were expressed as sum of all determined protein type concentrations. This new method was applied to quantitate gluten in wheat starches and compared to R5 ELISA and gel-permeation high-performance liquid chromatography with fluorescence detection (GP-HPLC-FLD, which resulted in a strong correlation between LC-MS/MS and the other two methods.

  18. Analysis of triacylglycerols on porous graphitic carbon by high temperature liquid chromatography.

    Science.gov (United States)

    Merelli, Bérangère; De Person, Marine; Favetta, Patrick; Lafosse, Michel

    2007-07-20

    The retention behaviour of several triacylglycerols (TAGs) and fats on Hypercarb, a porous graphitic carbon column (PGC), was investigated in liquid chromatography (LC) under isocratic elution mode with an evaporative light scattering detector (ELSD). Mixtures of chloroform/isopropanol were selected as mobile phase for a suitable retention time to study the influence of temperature. The retention was different between PGC and non-aqueous reversed phase liquid chromatography (NARP-LC) on octadecyl phase. The retention of TAGs was investigated in the interval 30-70 degrees C. Retention was greatly affected by temperature: it decreases as the column temperature increases. Selectivity of TAGs was also slightly influenced by the temperature. Moreover, this chromatographic method is compatible with a mass spectrometer (MS) detector by using atmospheric pressure chemical ionisation (APCI): same fingerprints of cocoa butter and shea butter were obtained with LC-ELSD and LC-APCI-MS. These preliminary results showed that the PGC column could be suitable to separate quickly triacylglycerols in high temperature conditions coupled with ELSD or MS detector.

  19. Detection of various freshwater cyanobacterial toxins using ultra-performance liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Oehrle, Stuart A; Southwell, Ben; Westrick, Judy

    2010-05-01

    Several freshwater cyanobacteria species have the capability to produce toxic compounds, frequently referred to as cyanotoxins. The most prevalent of these cyanotoxins is microcystin LR. Recognizing the potential health risk, France, Italy, Poland, Australia, Canada, and Brazil have set either standards or guidelines for the amount of microcystin LR permissible in drinking water based on the World Health Organization guideline of one microg/L of microcystin LR. Recently, the United States Environmental Protection Agency has begun to evaluate the occurrence and health effects of cyanotoxins and their susceptibility to water treatment under the Safe Drinking Water Act through the Contaminant Candidate List (CCL). A recent update of the Contaminant Candidate List focuses research and data collection on the cyanotoxins microcystin LR, anatoxin-a, and cylindrospermopsin. Liquid Chromatography/Tandem-Mass Spectrometry (LC/MS/MS) is a powerful tool for the analysis of various analytes in a wide variety of matrices because of its sensitivity and selectivity. The use of smaller column media (sub 2 microm particles) was investigated to both improve the speed, sensitivity and resolution, and to quantify the CCL cyanotoxins, in a single analysis, using Ultra-Performance Liquid Chromatography (UPLC) combined with tandem mass spectrometry. Natural waters and spiked samples were analyzed to show proof-of-performance. The presented method was able to clearly resolve each of the cyanotoxins in less than eight minutes with specificity and high spike recoveries. Copyright 2009 Elsevier Ltd. All rights reserved.

  20. Core-shell microspheres with porous nanostructured shells for liquid chromatography.

    Science.gov (United States)

    Ahmed, Adham; Skinley, Kevin; Herodotou, Stephanie; Zhang, Haifei

    2018-01-01

    The development of new stationary phases has been the key aspect for fast and efficient high-performance liquid chromatography separation with relatively low backpressure. Core-shell particles, with a solid core and porous shell, have been extensively investigated and commercially manufactured in the last decade. The excellent performance of core-shell particles columns has been recorded for a wide range of analytes, covering small and large molecules, neutral and ionic (acidic and basic), biomolecules and metabolites. In this review, we first introduce the advance and advantages of core-shell particles (or more widely known as superficially porous particles) against non-porous particles and fully porous particles. This is followed by the detailed description of various methods used to fabricate core-shell particles. We then discuss the applications of common silica core-shell particles (mostly commercially manufactured), spheres-on-sphere particles and core-shell particles with a non-silica shell. This review concludes with a summary and perspective on the development of stationary phase materials for high-performance liquid chromatography applications. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Comparison of capillary electrophoresis and high performance liquid chromatography methods for caffeine determination in decaffeinated coffee

    Directory of Open Access Journals (Sweden)

    Carolina Schaper Bizzotto

    2013-03-01

    Full Text Available Decaffeinated coffee accounts for 10 percent of coffee sales in the world; it is preferred by consumers that do not wish or are sensitive to caffeine effects. This article presents an analytical comparison of capillary electrophoresis (CE and high performance liquid chromatography (HPLC methods for residual caffeine quantification in decaffeinated coffee in terms of validation parameters, costs, analysis time, composition and treatment of the residues generated, and caffeine quantification in 20 commercial samples. Both methods showed suitable validation parameters. Caffeine content did not differ statistically in the two different methods of analysis. The main advantage of the high performance liquid chromatography (HPLC method was the 42-fold lower detection limit. Nevertheless, the capillary electrophoresis (CE detection limit was 115-fold lower than the allowable limit by the Brazilian law. The capillary electrophoresis (CE analyses were 30% faster, the reagent costs were 76.5-fold, and the volume of the residues generated was 33-fold lower. Therefore, the capillary electrophoresis (CE method proved to be a valuable analytical tool for this type of analysis.

  2. Measuring DNA nucleobase adducts using neutral hydrolysis and liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Tarun, Maricar; Rusling, James F

    2005-01-01

    The detection and identification of DNA adducts is important for predicting human cancer risk posed by chemicals and for uncovering potential genotoxicity of new drug and agricultural chemical candidates. For compounds that react with DNA to form N7-guanine and/or N3-adenine adducts, neutral thermal hydrolysis provides a simple procedure for sample preparation. The N7-guanine and N3-adenine adducts are selectively ejected from the DNA chain, resulting in a clean sample matrix enriched in nucleobase adducts. Coupling neutral thermal hydrolysis with liquid chromatography-mass spectrometry (LC-MS) provides sensitive methods to detect and quantitate DNA adducts, and structural information is provided by MS. Combining these technologies with capillary liquid chromatography sample preconcentration systems can provide exquisitely sensitive detection. In this review, we first summarize the chemistry of nucleobase adduct formation, briefly summarize modern methods to detect DNA adducts, and then describe neutral thermal hydrolysis coupled to LC-MS/MS and some of its applications to DNA damage studies. Finally, we review recent applications of neutral thermal hydrolysis and LC-MS to toxicity screening of chemicals.

  3. Sol-gel coated ion sources for liquid chromatography-direct electron ionization mass spectrometry.

    Science.gov (United States)

    Riboni, Nicolò; Magrini, Laura; Bianchi, Federica; Careri, Maria; Cappiello, Achille

    2017-07-25

    Advances in interfacing liquid chromatography and electron ionization mass spectrometry are presented. New ion source coatings synthesized by sol-gel technology were developed and tested as vaporization surfaces in terms of peak intensity, peak width and peak delay for the liquid chromatography-direct electron ionization mass spectrometry (Direct-EI) determination of environmental pollutants like polycyclic aromatic hydrocarbons and steroids. Silica-, titania-, and zirconia-based coatings were sprayed inside the stainless steel ion source and characterized in terms of thermal stability, film thickness and morphology. Negligible weight losses until 350-400 °C were observed for all the materials, with coating thicknesses in the 6 (±1)-11 (±2) μm range for optimal ionization process. The best performances in terms of both peak intensity and peak width were obtained by using the silica-based coating: the detection of the investigated compounds was feasible at low ng μl -1 levels with a good precision (RSD < 9% for polycyclic aromatic hydrocarbons and <11% for hormones). Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Separation optimization of quercetin, hesperetin and chrysin in honey by micellar liquid chromatography and experimental design.

    Science.gov (United States)

    Hadjmohammadi, Mohammad Reza; Nazari, S Saman S J

    2010-10-01

    The chemometrics approach was applied for the separation optimization of flavonoid markers (quercetin, hesperetin and chrysin) in honey using micellar liquid chromatography (MLC). The investigated method combines SPE of flavonoids from honey using C(18) cartridge and their separation and quantification by micellar liquid chromatography. A two level full factorial design was carried out to evaluate the effect of four experimental factors including concentration of SDS, alkyl chain length of the alcohol used as the organic modifier (N), volume percentage of the organic modifier (V(m)) and volume percentage of acetic acid (AcOH) in mobile phase on analytes retention times. Experiments for analytes retention times modeling and optimization of separation were performed according to central composite design. Multiple linear regression method was used for the construction of the best model based on experimental retention times. Pareto optimal method was used to find suitable compatibility between resolution and analysis time of analytes in honey. The optimum mobile phase composition for separation and determination of analytes in honey were [SDS]=0.124  mol/L; 7.8% v/v ethanol and 5.0% v/v AcOH. Limits of detection and linear range of flavonoid markers were 0.0079-0.0126, 0.05-50.0  mg/L, respectively.

  5. A simple and simultaneous identification method for aloe, catechu and gambir by high performance liquid chromatography.

    Science.gov (United States)

    Zhao, Yan; Kim, Young Ho; Lee, Wonjae; Lee, Young Keun; Kim, Kyung Tae; Kang, Jong Seong

    2016-01-05

    An effective and rapid method was developed for the simultaneous identification of aloe, catechu and gambir by high performance liquid chromatography-diode array detector (HPLC-DAD). Identification of three maker compounds presented in three medicinal materials was performed on high performance liquid chromatography-mass spectrometry (HPLC-MS). Under the optimal HPLC chromatographic conditions, sixty-two samples were processed on an Optimapak C18 column using a solvent system of acetonitrile (from 10% to 35%) and 0.1% phosphoric acid solution (from 90% to 65%) at a total flow rate of 1.0 mL/min and detected at 270 nm. All calibration curves exhibited good linear relationship (r(2)>0.9992). The relative standard deviation values of intra-day and inter-day precision were less than 1% and 2%, respectively. The recoveries of three analytes ranged from 99.48 to 100.97% with low RSDs (China and Korea without their correct identification. It indicates the existent of high potential medicinal risk by misuse of three medicinal materials. The developed HPLC method can be applied to prevent unexpected biological activity due to misapplication of medicinal materials. Copyright © 2015 Elsevier B.V. All rights reserved.

  6. Development and application of liquid chromatography coupled to isotope ratio mass spectrometry

    International Nuclear Information System (INIS)

    Zhang, Lijun

    2014-01-01

    Stable isotope analysis has found widespread applications in various disciplines such as archaeology, geochemistry, biology, food authenticity, and forensic science. Coupling chromatography to isotope ratio mass spectrometry for compound-specific isotope analysis (CSIA) is a trend, as it provides several advantages over bulk isotope analysis, e.g., relatively simple sample preparation, the ability to measure individual compounds in a complex mixture in one run, and the reduced sample size required for precise isotope analysis. Gas chromatography coupled to isotope ratio mass spectrometry (GC/IRMS) has been well-established for compound-specific isotope analysis of volatile organic compounds within the last two decades. However, an interface combining liquid chromatography with isotope ratio mass spectrometry (LC/IRMS) was not commercially available until 2004. The current design of the interface requires using a carbon-free eluent in chromatographic separation. This requirement limits the application of the most frequently used reversed-phase liquid chromatography in CSIA, because the elution strength of water at room temperature is too low to serve as mobile phase in reversed-phase separations. In order to increase the elution strength of water, we propose using high temperature water for chromatographic elution. The polarity of water decreases with an increase of temperature, yielding increased elution strength in reversed-phase columns. Therefore, high temperature water can be used as eluent instead of organic solvent for combining reversed-phase liquid chromatography with isotope ratio mass spectrometry (RPLC/IRMS). Additionally, temperature gradients can replace organic solvent gradients to increase chromatographic resolution. This is very important for LC/IRMS analysis, as precise isotope analysis requires baseline separation of analytes. In this thesis, high-temperature reversed-phase liquid chromatography was coupled to, and for the first time carefully

  7. Development and application of liquid chromatography coupled to isotope ratio mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Lijun

    2014-02-19

    Stable isotope analysis has found widespread applications in various disciplines such as archaeology, geochemistry, biology, food authenticity, and forensic science. Coupling chromatography to isotope ratio mass spectrometry for compound-specific isotope analysis (CSIA) is a trend, as it provides several advantages over bulk isotope analysis, e.g., relatively simple sample preparation, the ability to measure individual compounds in a complex mixture in one run, and the reduced sample size required for precise isotope analysis. Gas chromatography coupled to isotope ratio mass spectrometry (GC/IRMS) has been well-established for compound-specific isotope analysis of volatile organic compounds within the last two decades. However, an interface combining liquid chromatography with isotope ratio mass spectrometry (LC/IRMS) was not commercially available until 2004. The current design of the interface requires using a carbon-free eluent in chromatographic separation. This requirement limits the application of the most frequently used reversed-phase liquid chromatography in CSIA, because the elution strength of water at room temperature is too low to serve as mobile phase in reversed-phase separations. In order to increase the elution strength of water, we propose using high temperature water for chromatographic elution. The polarity of water decreases with an increase of temperature, yielding increased elution strength in reversed-phase columns. Therefore, high temperature water can be used as eluent instead of organic solvent for combining reversed-phase liquid chromatography with isotope ratio mass spectrometry (RPLC/IRMS). Additionally, temperature gradients can replace organic solvent gradients to increase chromatographic resolution. This is very important for LC/IRMS analysis, as precise isotope analysis requires baseline separation of analytes. In this thesis, high-temperature reversed-phase liquid chromatography was coupled to, and for the first time carefully

  8. PREPARATIVE ISOLATION AND PURIFICATION OF FIVE FLAVONOIDS FROM POGOSTEMON CABLIN BENTH BY HIGH-SPEED COUNTERCURRENT CHROMATOGRAPHY AND PREPARATIVE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

    OpenAIRE

    Li, Kang; Zhang, Hongwu; Xie, Huichun; Liang, Yong; Wang, Xiaohong; Ito, Yoichiro

    2011-01-01

    High-speed countercurrent chromatography (HSCCC) and preparative high-performance liquid chromatography (prep-HPLC) were successively used for the separation of pogostone and four flavonoids from Pogostemon cablin (Blanco) Benth. An efficient HSCCC separation was achieved on a two-phase solvent system composed of n-hexane–ethyl acetate–methanol–water (11:5:11:5, v/v/v/v). Three well-separated peaks were obtained in the HSCCC chromatogram. The first and the second fractions each contained two ...

  9. Separation of epigallocatechin and flavonoids from Hypericum perforatum L. by high-speed counter-current chromatography and followed by preparative liquid chromatography

    OpenAIRE

    Wei, Yun; Xie, Qianqian; Dong, Wanting; Ito, Yoichiro

    2008-01-01

    High-speed countercurrent chromatography (HSCCC) and preparative liquid chromatography were successively used for separation of epigallocatechin and flavonoids from Hypericum perforatum L. The two-phase solvent system composed of ethyl acetate-methanol -water (10:1:10, v/v) was used for HSCCC. About a 900 mg amount of the crude extract was separated by HSCCC, yielding 7.8 mg of quercetrin at a purity of over 97%, 12.6 mg of quercetin at a purity of over 93%, and 38.9 mg of a mixture of hypero...

  10. Characterization of polyaniline-coated stationary phases by using the linear solvation energy relationship in the hydrophilic interaction liquid chromatography mode using capillary liquid chromatography.

    Science.gov (United States)

    Taraba, Lukáš; Křížek, Tomáš; Hodek, Ondřej; Kalíková, Květa; Coufal, Pavel

    2017-02-01

    A polyaniline coating was used to modify the surface of bare silica gel and octadecyl silica stationary phases to characterize the properties of altered materials. It was assumed that the mixed-mode retention was established on the basis of the polyaniline chemical structure and its combination with the original sorbents. Polyaniline was deposited onto the original surfaces during the chemical polymerization of aniline hydrochloride. The prepared materials were slurry packed into capillary columns and systematic chromatographic characterization was performed using the linear solvation energy relationship, also employing descriptors that allow inclusion of ionic interactions in the proposed retention mechanism. The retention times of 80 solutes with various chemical structures were measured in the hydrophilic interaction liquid chromatography mode. The obtained results demonstrated the significant contribution of the polyaniline coating to the retention mechanism under the given conditions; the assumed mixed-mode retention was confirmed. The dominant retention interaction for both modified stationary phases was based on the protonation of nitrogen atoms in the polyaniline structure, leading to suitable retention and selectivity for the hydrophilic analytes, especially anionic and zwitterionic species. Thus, especially, the polyaniline-coated bare silica gel sorbent seems to be promising for potential applications related to the separation of polar compounds. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Quantitative analysis of pharmacokinetic study samples by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS).

    Science.gov (United States)

    Mück, W

    1999-09-01

    The basis of all pharmacokinetic evaluations are powerful assays to quantify drugs and/or metabolites in biological matrices using modern sensitive instrumental analytical techniques, such as capillary gas chromatography and high-performance liquid chromatography (HPLC). Being both specific and universal, mass spectrometry (MS) is an ideal chromatographic detector. Due to recent exciting achievements in the interfacing of liquid chromatography (LC) and MS, LC-MS, like the successfully preceding hyphenated technique gas chromatography-mass spectrometry (GC-MS), has now become a valuable technique in the analyst's toolbox. The key features of LC-MS are explained and four examples demonstrating its potential for highly specific and sensitive routine drug assays with the option of high sample throughput in pharmacokinetic investigations are presented.

  12. Illicit Drug Analysis Using Two-Dimension Liquid Chromatography/Tandem Mass Spectrometry.

    Science.gov (United States)

    Mallet, Claude; Botch-Jones, Sabra

    2016-10-01

    For the identification of illicit drugs in forensic toxicological casework, analysis can be delayed and potentially compromised due to lengthy sample preparation techniques. For a complete forensic identification, a robust methodology is required and the current trend in forensic laboratories is the use of liquid chromatography coupled to mass spectrometry (LC/MS or LC/MS-MS). However, to achieve satisfactory results, extensive and time-consuming sample preparation protocols are required to reach sub-ng/mL levels. The concept of sequential 2D extraction was designed to capture the retention behavior of a target analyte in response to various extraction parameters. Therefore, optimized conditions can be selected to excise a region of interest during extraction. The utilization of multi-dimensional chromatography combined with a micro-extraction technique was evaluated to decrease sample preparation time while enhancing the separation integrity observed with current single-dimensional chromatography techniques. A wide range of illicit drugs were spiked in human urine and extracted using three extraction protocols for performance evaluation. The extraction process was performed using a reversed-phase solid phase extraction (SPE) in 1D, 2D-optimized, 2D-sequential and cumulative elution modes. The chosen 2D chromatography conditions that were used in this application were identified using a 6 × 6 automated methods development protocol (144 methods total). The extraction of urine samples containing target analytes was completed in less than 20 min. The analysis was performed using 200 µL of the final organic solvent (MeOH) extracts. The limit of detection for all drugs was measured at 100 pg/mL (ppt) from a 1 mL sample volume. Several analytes showed excellent signal at 10 pg/mL (ppt). © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  13. Determination of Polycyclic Aromatic Hydrocarbons in Automobile Exhaust by Means of High-Performance Liquid Chromatography with Fluorescence Detection

    DEFF Research Database (Denmark)

    Nielsen, Tom

    1979-01-01

    A chromatographic method has been developed and applied to the determination of polycyclic aromatic hydrocarbons (PAHs) in particulate matter in automobile exhaust, in petrols, and in crankcase oils. The PAHs were purified from other organic compounds by thin-layer chromatography, separated by high......-performance liquid chromatography, and measured by means of on-line fluorescence detection. The identities of the PAHs were verified by comparing the emission spectra obtained by a stop-flow technique with those of standard PAHs...

  14. Determination of artificial sweeteners in sewage sludge samples using pressurised liquid extraction and liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Ordoñez, Edgar Y; Quintana, José Benito; Rodil, Rosario; Cela, Rafael

    2013-12-13

    An analytical method for the determination of six artificial sweeteners in sewage sludge has been developed. The procedure is based on pressurised liquid extraction (PLE) with water followed by solid-phase extraction (SPE) and subsequent liquid chromatography-tandem mass spectrometry analysis. After optimisation of the different PLE parameters, extraction with aqueous 500mM formate buffer (pH 3.5) at 80°C during a single static cycle of 21min proved to be best conditions. After a subsequent SPE, quantification limits, referred to dry weight (dw) of sewage sludge, ranged from 0.3ng/g for acesulfame (ACE) to 16ng/g for saccharin (SAC) and neohespiridine dihydrochalcone. The trueness, expressed as recovery, ranged between 72% and 105% and the precision, expressed as relative standard deviation, was lower than 16%. Moreover, the method proved its linearity up to the 2μg/g range. Finally, the described method was applied to the determination of the artificial sweeteners in primary and secondary sewage sludge from urban wastewater treatment plants. Four of the six studied artificial sweeteners (ACE, cyclamate, SAC and sucralose) were found in the samples at concentrations ranging from 17 to 628ng/g dw. Copyright © 2013 Elsevier B.V. All rights reserved.

  15. Determination of Levetiracetam in Human Plasma by Dispersive Liquid-Liquid Microextraction Followed by Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Greyce Kelly Steinhorst Alcantara

    2016-01-01

    Full Text Available Levetiracetam (LEV is an antiepileptic drug that is clinically effective in generalized and partial epilepsy syndromes. The use of this drug has been increasing in clinical practice and intra- or -interindividual variability has been exhibited for special population. For this reason, bioanalytical methods are required for drug monitoring in biological matrices. So this work presents a dispersive liquid-liquid microextraction method followed by gas chromatography-mass spectrometry (DLLME-GC-MS for LEV quantification in human plasma. However, due to the matrix complexity a previous purification step is required. Unlike other pretreatment techniques presented in the literature, for the first time, a procedure employing ultrafiltration tubes Amicon® (10 kDa porous size without organic solvent consumption was developed. GC-MS analyses were carried out using a linear temperature program, capillary fused silica column, and helium as the carrier gas. DLLME optimized parameters were type and volume of extraction and dispersing solvents, salt addition, and vortex agitation time. Under chosen parameters (extraction solvent: chloroform, 130 μL; dispersing solvent: isopropyl alcohol, 400 μL; no salt addition and no vortex agitation time, the method was completely validated and all parameters were in agreement with the literature recommendations. LEV was quantified in patient’s plasma sample using less than 550 μL of organic solvent.

  16. Automated high performance liquid chromatography and liquid scintillation counting determination of pesticide mixture octanol/water partition rates

    International Nuclear Information System (INIS)

    Moody, R.P.; Carroll, J.M.; Kresta, A.M.

    1987-01-01

    Two novel methods are reported for measuring octanol/water partition rates of pesticides. A liquid scintillation counting (LSC) method was developed for automated monitoring of 14 C-labeled pesticides partitioning in biphasic water/octanol cocktail systems with limited success. A high performance liquid chromatography (HPLC) method was developed for automated partition rate monitoring of several constituents in a pesticide mixture, simultaneously. The mean log Kow +/- SD determined from triplicate experimental runs were for: 2,4-D-DMA (2,4-dichlorophenoxyacetic acid dimethylamine), 0.65 +/- .17; Deet (N,N-diethyl-m-toluamide), 2.02 +/- .01; Guthion (O,O-dimethyl-S-(4-oxo-1,2,3-benzotriazin-3(4H)-ylmethyl) phosphorodithioate), 2.43 +/- .03; Methyl-Parathion (O,O-dimethyl-O-(p-nitrophenyl) phosphorothioate), 2.68 +/- .05; and Fenitrothion (O,O-dimethyl O-(4-nitro-m-tolyl) phosphorothioate), 3.16 +/- .03. A strong positive linear correlation (r = .9979) was obtained between log Kow and log k' (log Kow = 2.35 (log k') + 0.63). The advantages that this automated procedure has in comparison with the standard manual shake-flask procedure are discussed

  17. Quantitative determination of methamphetamine in oral fluid by liquid-liquid extraction and gas chromatography/mass spectrometry.

    Science.gov (United States)

    Bahmanabadi, L; Akhgari, M; Jokar, F; Sadeghi, H B

    2017-02-01

    Methamphetamine abuse is one of the most medical and social problems many countries face. In spite of the ban on the use of methamphetamine, it is widely available in Iran's drug black market. There are many analytical methods for the detection of methamphetamine in biological specimen. Oral fluid has become a popular specimen to test for the presence of methamphetamine. The purpose of the present study was to develop a method for the extraction and detection of methamphetamine in oral fluid samples using liquid-liquid extraction (LLE) and gas chromatography/mass spectrometry (GC/MS) methods. An analytical study was designed in that blank and 50 authentic oral fluid samples were collected to be first extracted by LLE and subsequently analysed by GC/MS. The method was fully validated and showed an excellent intra- and inter-assay precision (reflex sympathetic dystrophy ˂ 10%) for external quality control samples. Recovery with LLE methods was 96%. Limit of detection and limit of quantitation were 5 and 15 ng/mL, respectively. The method showed high selectivity, no additional peak due to interfering substances in samples was observed. The introduced method was sensitive, accurate and precise enough for the extraction of methamphetamine from oral fluid samples in forensic toxicology laboratories.

  18. Determination of tropane alkaloids by heart cutting reversed phase - Strong cation exchange two dimensional liquid chromatography.

    Science.gov (United States)

    Long, Zhen; Zhang, Yanhai; Gamache, Paul; Guo, Zhimou; Steiner, Frank; Du, Nana; Liu, Xiaoda; Jin, Yan; Liu, Xingguo; Liu, Lvye

    2018-01-01

    Current Chinese Pharmacopoeia (ChP) standards apply liquid extraction combined with one dimensional liquid chromatography (1DLC) method for determining alkaloids in herbal medicines. The complex pretreatments lead to a low analytical efficiency and possible component loss. In this study, a heart cutting reversed phase - strong cation exchange two dimensional liquid chromatography (RP - SCX 2DLC) approach was optimized for simultaneously quantifying tropane alkaloids (anisodine, scopolamine and hyoscyamine) in herbal medicines and herbal medicine tablets without further treatment of the filtered extract. The chromatographic conditions were systematically optimized in terms of column type, mobile phase composition and flow rate. To improve peak capacity and obtain symmetric peak shape of alkaloids, a polar group embedded C18 column combined with chaotropic salts was used in the first dimension. To remove the disturbance of non-alkaloids, achieve unique selectivity and acquire symmetric peak shape of alkaloids, an SCX column combined with phosphate buffer was used in the second dimension. Method validation was performed in terms of linearity, precision (0.54-0.82%), recovery (94.1-105.2%), limit of detection (LOD) and limit of quantification (LOQ) of the three analytes varied between 0.067-0.115mgL -1 and 0.195-0.268mgL -1 , respectively. The method demonstrated superiority over 1DLC method in respect of resolution (less alkaloid co-eluted), sample preparation (no pretreatment procedure) and transfer rate (minimum component loss). The optimized RP - SCX 2DLC approach was subsequently applied to quantify target alkaloids in five herbal medicines and herbal medicine tablets from three different manufactures. The results demonstrated that the developed heart cutting RP - SCX 2DLC approach represented a new, strategically significant methodology for the quality evaluation of tropane alkaloid in related herbal medicines that involve complex chemical matrix. Copyright

  19. Application of dispersive liquid-liquid microextraction for the preconcentration of eight parabens in real samples and their determination by high-performance liquid chromatography.

    Science.gov (United States)

    Shen, Xiong; Liang, Jian; Zheng, Luxia; Lv, Qianzhou; Wang, Hong

    2017-11-01

    A simple and sensitive method for the simultaneous determination of eight parabens in human plasma and urine samples was developed. The samples were preconcentrated using dispersive liquid-liquid microextraction based on the solidification of floating organic drops and determined by high-performance liquid chromatography with ultraviolet detection. The influence of variables affecting the extraction efficiency was investigated and optimized using Placket-Burman design and Box-Behnken design. The optimized values were: 58 μL of 1-decanol (as extraction solvent), 0.65 mL methanol (as disperser solvent), 1.5% w/v NaCl in 5.0 mL of sample solution, pH 10.6, and 4.0 min centrifugation at 4000 rpm. The extract was injected into the high-performance liquid chromatography system for analysis. Under the optimum conditions, the linear ranges for eight parabens in plasma and urine were 1.0-1000 ng/mL, with correlation coefficients above 0.994. The limit of detection was 0.2-0.4 and 0.1-0.4 ng/mL for plasma and urine samples, respectively. Relative recoveries were between 80.3 and 110.7%, while relative standard deviations were less than 5.4%. Finally, the method was applied to analyze the parabens in 98 patients of primary breast cancer. Results showed that parabens existed widely, at least one paraben detected in 96.9% (95/98) of plasma samples and 98.0% (96/98) of urine samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Bulk chirality effect for symmetric bistable switching of liquid crystals on topologically self-patterned degenerate anchoring surface.

    Science.gov (United States)

    Park, Min-Kyu; Joo, Kyung-Il; Kim, Hak-Rin

    2017-06-26

    We demonstrate a bistable switching liquid crystal (LC) mode utilizing a topologically self-structured dual-groove surface for degenerated easy axes of LC anchoring. In our study, the effect of the bulk elastic distortion of the LC directors on the bistable anchoring surface is theoretically analyzed for balanced bistable states based on a free energy diagram. By adjusting bulk LC chirality, we developed ideally symmetric and stable bistable anchoring and switching properties, which can be driven by a low in-plane pulsed field of about 0.7 V/µm. The fabricated device has a contrast ratio of 196:1.

  1. EPA Method 8321B (SW-846): Solvent-Extractable Nonvolatile Compounds by High Performance Liquid Chromatography-Thermospray-Mass Spectrometry (HPLC-TS-MS) or Ultraviolet (UV) Detection

    Science.gov (United States)

    Method 8321B describes procedures for preparation and analysis of solid, aqueous liquid, drinking water and wipe samples using high performance liquid chromatography and mass spectrometry for extractable non-volatile compounds.

  2. Optimization of the Hewlett-Packard particle-beam liquid chromatography-mass spectrometry interface by statistical experimental design.

    Science.gov (United States)

    Huang, S K; Garza, N R

    1995-06-01

    Optimization of both sensitivity and ionization softness for the Hewlett-Packard particle-beam liquid chromatography-mass spectrometry interface has been achieved by using a statistical experimental design with response surface modeling. Conditions for both optimized sensitivity and ionization softness were found to occur at 55-lb/in.(2) nebulizer flow, 35°C desolvation chamber temperature with approximately 45% organic modifier in the presence of 0.02-F ammonium acetate and a liquid chromatography flow rate of 0.2 mL/min.

  3. Mutation analysis in {beta}{sub 2-}adrenergic receptor gene by denaturing high performance liquid chromatography (DHPLC)

    Energy Technology Data Exchange (ETDEWEB)

    Park, S.B.; Oh, C.H.; Kim, J.W.; Jang, W.C. [Dankook University, Cheonan (Korea)

    2002-06-01

    We analysed mutation of {beta}{sub 2-}adrenergic receptor gene that controls bronchial asthma by denaturing high performance liquid chromatography (DHPLC) according to ion-pair reversed-phase high performance liquid chromatography (IP-RP-HPLC). We extracted genomic DNA from 50 asthma patients, amplified DNA using PCR, and analysed PCR product by DHPLC. As a result, we obtained that mutation frequency was 15(30%) among 50 cases. Consequently DHPLC mutation detection was confirmed that the result of direct sequencing was coincide exactly. (author). 13 refs., 4 figs.

  4. Simultaneous Determination of 25 Common Pharmaceuticals in Whole Blood Using Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry

    DEFF Research Database (Denmark)

    Nielsen, Marie Katrine Klose; Johansen, Sys Stybe

    2012-01-01

    An ultra-performance liquid chromatography-tandem mass spectrometry method was developed and validated for the quantification of 25 common pharmaceuticals in whole blood. The selected pharmaceuticals represent the most frequently detected drugs in our forensic laboratory with basic properties...... elution using a Waters ACQUITY Ultra-Performance Liquid Chromatography system. Quantification was performed on a Waters tandem quadrupole ACQUITY TQD using multiple reaction monitoring in positive mode. The analytes were eluted within 11 min. The limit of quantification (LOQ) ranged from 0.002 to 0.01 mg...

  5. Combination of solvent extractants for dispersive liquid-liquid microextraction of fungicides from water and fruit samples by liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Pastor-Belda, Marta; Garrido, Isabel; Campillo, Natalia; Viñas, Pilar; Hellín, Pilar; Flores, Pilar; Fenoll, José

    2017-10-15

    A multiresidue method was developed to determine twenty-five fungicides belonging to three different chemical families, oxazoles, strobilurins and triazoles, in water and fruit samples, using dispersive liquid-liquid microextraction (DLLME) and liquid chromatography/tandem mass spectrometry (LC-MS 2 ). Solid-liquid extraction with acetonitrile was used for the analysis in fruits, the extract being used as dispersant solvent in DLLME. Since some of the analytes showed high affinity for chloroform and the others were more efficiently extracted with undecanol, a mixture of both solvents was used as extractant in DLLME. After evaporation of CHCl 3 , the enriched phase was analyzed. Enrichment factors in the 23-119 and 12-60 ranges were obtained for waters and fruits, respectively. The approach was most sensitive for metominostrobin with limits of quantification of 1ngL -1 and 5ngkg -1 in waters and fruits, respectively, while a similar sensitivity was attained for tebuconazole in fruits. Recoveries of the fungicides varied between 86 and 116%. Copyright © 2017 Elsevier Ltd. All rights reserved.

  6. Simultaneous determination of simazine, cyanazine, and atrazine in honey samples by dispersive liquid-liquid microextraction combined with high-performance liquid chromatography.

    Science.gov (United States)

    Tian, Hongzhe; Bai, Xuesong; Xu, Jing

    2017-10-01

    A rapid and simple sample preparation method was developed for simultaneous determination of three triazine herbicides in honey samples. The selected herbicides were extracted from honey samples by ionic liquid dispersive liquid-liquid microextraction, separated on a C 18 column (250 mm × 4.6 mm id, 5 μm) using acetonitrile and H 2 O as the mobile phase with gradient elution, and then detected by high-performance liquid chromatography. The parameters, such as the type and volume of the extraction and disperser solvent, ion strength, pH, extraction time, and centrifuge time were optimized in order to provide the excellent extraction performance. Good linearity was showed for all the target herbicides over the tested concentration range with correlation coefficient higher than 0.994. Three spiked levels (0.005, 0.05, 0.10 mg/kg) were applied for determination of the recoveries of the targets in honey samples in the range of 80-103% with relative standard deviations not larger than 10.6%. The limits of quantification for the analytes ranged between 1.5 and 4.0 μg/kg. The developed method was applied for determination of the target compounds residues in real samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Sensitive liquid chromatography-tandem mass spectrometry method for quantification of hydrochlorothiazide in human plasma.

    Science.gov (United States)

    Ramakrishna, N V S; Vishwottam, K N; Manoj, S; Koteshwara, M; Wishu, S; Varma, D P

    2005-12-01

    A simple, rapid, sensitive and specific liquid chromatography-tandem mass spectrometry method was developed and validated for quantification of hydrochlorothiazide (I), a common diuretic and anti-hypertensive agent. The analyte and internal standard, tamsulosin (II) were extracted by liquid-liquid extraction with diethyl ether-dichloromethane (70:30, v/v) using a Glas-Col Multi-Pulse Vortexer. The chromatographic separation was performed on a reversed-phase column (Waters symmetry C18) with a mobile phase of 10 mm ammonium acetate-methanol (15:85, v/v). The protonated analyte was quantitated in negative ionization by multiple reaction monitoring with a mass spectrometer. The mass transitions m/z 296.1 solidus in circle 205.0 and m/z 407.2 solidus in circle 184.9 were used to measure I and II, respectively. The assay exhibited a linear dynamic range of 0.5-200 ng/mL for hydrochlorothiazide in human plasma. The lower limit of quantitation was 500 pg/mL, with a relative standard deviation of less than 9%. Acceptable precision and accuracy were obtained for concentrations over the standard curve ranges. A run time of 2.5 min for each sample made it possible to analyze a throughput of more than 400 human plasma samples per day. The validated method has been successfully used to analyze human plasma samples for application in pharmacokinetic, bioavailability or bioequivalence studies. (c) 2005 John Wiley & Sons, Ltd.

  8. Determination of strychnine and brucine in rat plasma using liquid chromatography electrospray ionization mass spectrometry.

    Science.gov (United States)

    Xu, Yanyan; Si, Duanyun; Liu, Changxiao

    2009-02-20

    A simple, sensitive and selective liquid chromatography-electrospray mass spectrometric (LC-ESI-MS) method was developed and validated for simultaneous determination of strychnine and brucine in rat plasma, using tacrine as the internal standard (IS). Sample preparation involved a liquid-liquid extraction of the analytes with n-hexane, dichloromethane and isopropanol (65:30:5, v/v/v) from 0.1mL of plasma. Chromatographic separation was carried out on a Waters C(18) column using a mobile phase of methanol-20mM ammonium formate-formic acid (32:68:0.68, v/v/v). Positive selected ion monitoring mode was used for detection of strychnine, brucine and the IS at m/z 335.2, m/z 395.2 and m/z 199.2, respectively. Linearity was obtained over the concentration range of 0.5-500ng/mL for strychnine and 0.1-100ng/mL for brucine. The lower limit of quantification was 0.5ng/mL and 0.1ng/mL for strychnine and brucine, respectively. The intra- and inter-day precision for both strychnine and brucine was less than 7.74%, and accuracy ranged from -4.38% to 2.21% at all QC levels. The method has been successfully applied to a pharmacokinetic study of processed Semen Strychni after oral administration to rats.

  9. Determination of parabens using two microextraction methods coupled with capillary liquid chromatography-UV detection.

    Science.gov (United States)

    Chen, Chen-Wen; Hsu, Wen-Chan; Lu, Ya-Chen; Weng, Jing-Ru; Feng, Chia-Hsien

    2018-02-15

    Parabens are common preservatives and environmental hormones. As such, possible detrimental health effects could be amplified through their widespread use in foods, cosmetics, and pharmaceutical products. Thus, the determination of parabens in such products is of particular importance. This study explored vortex-assisted dispersive liquid-liquid microextraction techniques based on the solidification of a floating organic drop (VA-DLLME-SFO) and salt-assisted cloud point extraction (SA-CPE) for paraben extraction. Microanalysis was performed using a capillary liquid chromatography-ultraviolet detection system. These techniques were modified successfully to determine four parabens in 19 commercial products. The regression equations of these parabens exhibited good linearity (r 2 =0.998, 0.1-10μg/mL), good precision (RSD<5%) and accuracy (RE<5%), reduced reagent consumption and reaction times (<6min), and excellent sample versatility. VA-DLLME-SFO was also particularly convenient due to the use of a solidified extract. Thus, the VA-DLLME-SFO technique was better suited to the extraction of parabens from complex matrices. Copyright © 2017 Elsevier Ltd. All rights reserved.

  10. [Determination of amitrole in agricultural products by high performance liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Li, Li; Fu, Jian; Gao, Hongliang; Ren, Haitao; Lou, Xishan; Guan, Lihui

    2010-03-01

    A high performance liquid chromatography-tandem mass spectrometry method (HPLC-MS/MS) was developed for the analysis of amitrole residues in agricultural products. The samples were extracted by 25% acetone for wheat, fish, pork and liver samples, 1% acetic acid-25% acetone for maize and peanut samples, 1% acetic acid solution for honeysuckle, the powder of ginger, the powder of bunge prickly ash and tea leaves samples, 1% acetic acid solution-dichloromethane for apple, pineapple, spinach, carrot, perilla leaves samples, respectively, followed by liquid-liquid extraction with dichloromethane. The samples were then cleaned up by PCX or Envi-Carb solid-phase extraction cartridge. The amitrole was determined and confirmed by HPLC-MS/MS. The results showed a linear relationship in the range of 0.005 -0.1 mg/kg for amitrole. The correlation coefficient was 0.999 7. The average recoveries of amitrole in wheat, maize, peanut, pineapple, apple, carrot, spinach, pork, the powder of ginger, the powder of bunge prickly ash, perilla, liver, fish, honeysuckle and tea were 67.5% - 98.1%. The relative standard deviations (RSDs) were 1.0% - 9.8%. The limits of quantitation were 10 microg/kg for wheat, maize, peanut, pineapple, apple, carrot, spinach, pork, perilla, liver, fish, honeysuckle and 20 microg/kg for the powder of bunge prickly ash, the powder of ginger and tea, respectively. The method is simple, sensitive and accurate.

  11. Community air monitoring for pesticides-part 2: multiresidue determination of pesticides in air by gas chromatography, gas chromatography-mass spectrometry, and liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Hengel, Matt; Lee, P

    2014-03-01

    Two multiresidue methods were developed to determine pesticides in air collected in California. Pesticides were trapped using XAD-4 resin and extracted with ethyl acetate. Based on an analytical method from the University of California Davis Trace Analytical Laboratory, pesticides were detected by analyzing the extract by gas chromatography-mass spectrometry (GC-MS) to determine chlorothalonil, chlorthal-dimethyl, cycloate, dicloran, dicofol, EPTC, ethalfluralin, iprodione, mefenoxam, metolachlor, PCNB, permethrin, pronamide, simazine, trifluralin, and vinclozolin. A GC with a flame photometric detector was used to determine chlorpyrifos, chlorpyrifos oxon, diazinon, diazinon oxon, dimethoate, dimethoate oxon, fonophos, fonophos oxon, malathion, malathion oxon, naled, and oxydemeton. Trapping efficiencies ranged from 78 to 92 % for low level (0.5 μg) and 37-104 % for high level (50 and 100 μg) recoveries. Little to no degradation of compounds occurred over 31 days; recoveries ranged from 78 to 113 %. In the California Department of Food and Agriculture (CDFA) method, pesticides were detected by analyzing the extract by GC-MS to determine chlorothalonil, chlorpyrifos, cypermethrin, dichlorvos, dicofol, endosulfan 1, endosulfan sulfate, oxyfluorfen, permethrin, propargite, and trifluralin. A liquid chromatograph coupled to a MS was used to determine azinphos-methyl, chloropyrifos oxon, DEF, diazinon, diazinon oxon, dimethoate, dimethoate oxon, diuron, EPTC, malathion, malathion oxon, metolachlor, molinate, norflurazon, oryzalin, phosmet, propanil, simazine and thiobencarb. Trapping efficiencies for compounds determined by the CDFA method ranged from 10 to 113, 22 to 114, and 56 to 132 % for 10, 5, and 2 μg spikes, respectively. Storage tests yielded 70-170 % recovery for up to 28 days. These multiresidue methods represent flexible, sensitive, accurate, and cost-effective ways to determine residues of various pesticides in ambient air.

  12. High-expression EGFR/cell membrane chromatography-online-high-performance liquid chromatography/mass spectrometry: rapid screening of EGFR antagonists from Semen Strychni.

    Science.gov (United States)

    Sun, Meng; Guo, Ying; Dai, Bingling; Wang, Chen; He, Langchong

    2012-09-15

    Traditional methods for screening active compounds from complex system such as traditional Chinese medicines are relatively cumbersome and time-consuming. In order to improve this situation, we established an online analytical method for screening, separation and identification EGFR antagonists from traditional Chinese medicines, which is described in this study. Cells with high EGFR expression levels were used to prepare the cell membrane stationary phase for the EGFR cell membrane chromatography model with the purpose of screening active compounds. Separation of the retention fractions was achieved by the high-performance liquid chromatography, and identification was conducted via electrospray ionization quadrupole mass spectrometry. The inhibitory effects of active compounds on EGFR cell growth were also demonstrated in vitro. The screening results showed that vauquline and strychnine from Semen Strychni could be active components acting on EGFR similarly to gefitinib as a control drug. Results from biological trials showed that vauquline and strychnine inhibited cell proliferation of HEK293/EGFR cells, and inhibited Erk phosphorylation, and can effectively reduce expression of downstream signaling molecules. This EGFR cell membrane chromatography-online-high-performance liquid chromatography/tandem mass spectrometry method can be applied for rapid screening, separation and identification of EGFR antagonists from traditional Chinese medicines and should be useful for drug discovery with natural medicinal herbs. Copyright © 2012 John Wiley & Sons, Ltd.

  13. On-line hyphenation of centrifugal partition chromatography and high pressure liquid chromatography for the fractionation of flavonoids from Hippophaë rhamnoides L. berries.

    Science.gov (United States)

    Michel, Thomas; Destandau, Emilie; Elfakir, Claire

    2011-09-09

    Centrifugal Partition Chromatography (CPC), a liquid-liquid preparative chromatography using two immiscible solvent systems, benefits from numerous advantages for the separation or purification of synthetic or natural products. This study presents the on-line hyphenation of CPC-Evaporative Light Scattering Detector (CPC-ELSD) with High Performance Liquid Chromatography-UV (HPLC-UV) for the fractionation of flavonols from a solvent-free microwave extract of sea buckthorn (Hippophaë rhamnoides L., Elaeagnaceae) berries. An Arizona G system was used for the fractionation of flavonoids by CPC and a fused core Halo C18 column allowed the on-line analyses of collected fractions by HPLC. The on-line CPC/HPLC procedure allowed the simultaneous fractionation step at preparative scale combined with the HPLC analyses which provide direct fingerprint of collected fractions. Thus the crude extract was simplified and immediate information on the composition of fractions could be obtained. Furthermore, this methodology reduced the time of post-fractionation steps and facilitated identification of main molecules by Mass Spectrometry (MS). Rutin, isorhamnetin-3-O-rutinoside, isorhamnetin-3-O-glucoside, quercetin-3-O-glucoside, isorhamnetin-rhamnoside, quercetin and isorhamnetin were identified. CPC-ELSD/HPLC-UV could be considered as a high-throughput technique for the guided fractionation of bioactive natural products from complex crude extracts. Copyright © 2011 Elsevier B.V. All rights reserved.

  14. Phytochemical analysis of Hibiscus caesius using high performance liquid chromatography coupled with mass spectrometry.

    Science.gov (United States)

    Ain, Quratul; Naveed, Muhammad Na; Mumtaz, Abdul Samad; Farman, Muhammad; Ahmed, Iftikhar; Khalid, Nauman

    2015-09-01

    Various species in genus Hibiscus are traditionally known for their therapeutic attributes. The present study focused on the phytochemical analysis of a rather unexplored species Hibiscus caesius (H. caesius), using high-pressure liquid chromatography coupled with mass spectrometry (HPLC-MS). The analysis revealed five major compounds in the aqueous extract, viz. vanillic acid, protocatechoic acid, quercetin, quercetin glucoside and apigenin, being reported for the first time in H. caesius. Literature suggests that these compounds have important pharmacological traits such as anti-cancer, anti-inflammatory, anti-bacterial and hepatoprotective etc. however, this requires further pharmacological investigations at in vitro and in vivo scale. The above study concluded the medicinal potential of H. caesius.

  15. Determination of primary amino acids in wines by high performance liquid magneto-chromatography.

    Science.gov (United States)

    Barrado, E; Rodriguez, J A; Castrillejo, Y

    2009-05-15

    Eight amino acids (ethanolamine, glycine, alanine, beta-aminobutyric acid, leucine, methionine, histidine and asparagine) were identified and quantified in Spanish wines by high performance liquid magneto-chromatography (HPLMC) with UV-V spectrophotometry. For this method, the amino acids are first complexed with mono(1,10-phenanthroline)-Cu(II) to confer them paramagnetic properties, and then separated by application of a low magnetic field intensity (5.5 mT) to the stationary phase contained in the chromatographic column. Principal components analysis of the results obtained grouped together the wine samples according to their denomination of origin: "Ribera del Duero", "Rueda" or "Rioja" (Spain). Through cluster analysis, a series of correlations was also observed among certain amino acids, and between these groupings and the type of wine. These clusters were found to reflect the role played by the amino acids as primary or secondary nutrients for the bacteria involved in alcoholic and malolactic fermentation.

  16. Glucose and glycerol concentrations and their tracer enrichment measurements using liquid chromatography tandem mass spectrometry

    DEFF Research Database (Denmark)

    Bornø, Andreas; Foged, Lene; van Hall, Gerrit

    2014-01-01

    The present study describes a new liquid chromatography tandem mass spectrometry method for high-throughput quantification of glucose and glycerol in human plasma using stable isotopically labeled internal standards and is suitable for simultaneous measurements of glucose and glycerol enrichments...... in connection to in vivo metabolic studies investigating glucose turnover and lipolytic rate. Moreover, in order to keep up with this new fast analysis, simple derivatization procedures have been developed. Prior to analysis, glucose and glycerol were derivatized using benzoyl chloride in order to form...... benzoylated derivatives via new simplified fast procedures. For glucose, two internal standards were evaluated, [U-(13) C(6)]glucose and [U-(13) C(6), D(7)]glucose, and for glycerol, [U-(13) C(3), D(8)]glycerol was used. The method was validated by means of calibration curves, quality control samples...

  17. Uncovering biologically significant lipid isomers with liquid chromatography, ion mobility spectrometry and mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Kyle, Jennifer E.; Zhang, Xing; Weitz, Karl K.; Monroe, Matthew E.; Ibrahim, Yehia M.; Moore, Ronald J.; Cha, Jeeyeon; Sun, Xiaofei; Lovelace, Erica S.; Wagoner, Jessica; Polyak, Steve; Metz, Thomas O.; Dey, Sudhansu K.; Smith, Richard D.; Burnum-Johnson, Kristin E.; Baker, Erin Shammel

    2016-01-01

    Understanding how biological molecules are generated, metabolized and eliminated in living systems is important for interpreting processes such as immune response and disease pathology. While genomic and proteomic studies have provided vast amounts of information over the last several decades, interest in lipidomics has also grown due to improved analytical technologies revealing altered lipid metabolism in type 2 diabetes, cancer, and lipid storage disease. Liquid chromatography and mass spectrometry (LC-MS) measurements are currently the dominant approach for characterizing the lipidome by providing detailed information on the spatial and temporal composition of lipids. However, interpreting lipids’ biological roles is challenging due to the existence of numerous structural and stereoisomers (i.e. distinct acyl chain and double-bond positions), which are unresolvable using present LC-MS approaches. Here we show that combining structurally-based ion mobility spectrometry (IMS) with LC-MS measurements distinguishes lipid isomers and allows insight into biological and disease processes.

  18. ANALISIS RESIDU KLORPIRIFOS DALAM SAYUR-SAYURAN DENGAN TEKNIK HIGH PERFORMANCE LIQUID CHROMATOGRAPHY (HPLC

    Directory of Open Access Journals (Sweden)

    Aman Sentosa Panggabean

    2016-06-01

    Full Text Available The research about analysis of chlorpyrifos residue in vegetables by using High Performance Liquid Chromatography (HPLC technique has been done. To obtain the optimal measurement results, the measurement performed several important parameters in the chromatographic system was composition of mobile phase, volume injection sample, flow rate and pH eluent. Optimum measurement conditions obtained was mobile phase composition (water : methanol with 70 : 30, volume injection sample are 5 mL, flow rate are 0.5mL/menit and pH eluent are 7. The analytical performance that obtained is good showed with the reproducibility value as percentage coefficient variance (% CV was 0.0664%, limit of detection (LOD was 0.44 ppm, with a recovery percentage of > 95%. The results obtained showed the HPLC technique can be used for the routine analysis in the determination of chlorpyrifos for the vegetable samples. Keywords: Chlorpyrifos, Vegetables, HPLC.

  19. Quantitative profiling method for oxylipin metabolome by liquid chromatography electrospray ionization tandem mass spectrometry.

    Science.gov (United States)

    Yang, Jun; Schmelzer, Kara; Georgi, Katrin; Hammock, Bruce D

    2009-10-01

    Cyclooxygenase, lipoxygenase, and epoxygenase derived oxylipins, especially eicosanoids, play important roles in many physiological processes. Assessment of oxidized fatty acid levels is important for understanding their homeostatic and pathophysiological roles. Most reported methods examine these pathways in isolation. The work described here employed a solid phase extraction-liquid chromatography-electrospray ionization MS/MS (SPE-LC-ESI MS/MS) method to monitor these metabolites. In 21 min, 39 oxylipins were quantified along with eight corresponding internal standards. The limits of quantification were between 0.07 and 32 pg (20 pM-10 nM). Finally, the validated method was used to evaluate oxylipin profiles in lipopolysaccharide-exposed mice, an established septic inflammatory model. The method described here offers a useful tool for the evaluation of complex regulatory oxylipin responses in in vitro or in vivo studies.

  20. Analysis of bromate in drinking water using liquid chromatography-tandem mass spectrometry without sample pretreatment.

    Science.gov (United States)

    Kosaka, Koji; Asami, Mari; Takei, Kanako; Akiba, Michihiro

    2011-01-01

    An analytical method for determining bromate in drinking water was developed using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The (18)O-enriched bromate was used as an internal standard. The limit of quantification (LOQ) of bromate was 0.2 µg/L. The peak of bromate was separated from those of coexisting ions (i.e., chloride, nitrate and sulfate). The relative and absolute recoveries of bromate in two drinking water samples and in a synthesized ion solution (100 mg/L chloride, 10 mg N/L nitrate, and 100 mg/L sulfate) were 99-105 and 94-105%, respectively. Bromate concentrations in 11 drinking water samples determined by LC-MS/MS were water without sample pretreatment.

  1. Determination of captopril by high-performance liquid chromatography with direct electrogenerated chemiluminescence

    Science.gov (United States)

    Sun, Yonghua; Zhang, Zhujun; Zhang, Xinfeng

    2013-03-01

    Captopril exhibit electrogenerated chemiluminescence (ECL) in NaNO3 solution when constant current is exerted. Based on this observation, a direct ECL method coupled with high-performance liquid chromatography (HPLC) separation is developed for determination of captopril in human serum. Factors affected the ECL emission are investigated. Under the optimal conditions, the ECL intensity has a linear relationship with the concentration of captopril in the range of 4.0 × 10-6-2.0 × 10-3 g mL-1 and the detection limit is 2 × 10-6 g mL-1 (S/N = 3). Compared with the common electrogenerated chemiluminescence experiments, the developed method need no any other fluorescence additives.

  2. Determination of clarithromycin in human plasma by liquid chromatography-electrospray ionization tandem mass spectrometry.

    Science.gov (United States)

    Jiang, Yao; Wang, Jiang; Li, Hao; Wang, Yingwu; Gu, Jingkai

    2007-03-12

    A rapid and sensitive method has been developed for the determination of clarithromycin in human plasma with liquid chromatography-tandem mass spectrometry. Clarithromycin and the internal standard, telmisartan were precipitated from the matrix (50 microl) with 200 microl acetonitrile and separated by HPLC using formic acid:10 mM ammonium acetate:methanol (1:99:400, v/v/v) as the mobile phase. The assay based on detection by electrospray positive ionization mass spectrometry in the multiple-reaction monitoring mode was finished within 2.4 min. Linearity was over the concentration range 10-5000 ng/ml with a limit of detection of 0.50 ng/ml. Intra- and inter-day precision measured as relative standard deviation were bioequivalence study of two tablet formulations of clarithromycin.

  3. Determination of dapsone in meat and milk by liquid chromatography tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Hadjigeorgiou, M. [State General Laboratory of Cyprus, Veterinary Drug Residues Lab, Kimonos 44, 1451 Nicosia (Cyprus)], E-mail: mhadjigeorgiou@sgl.moh.gov.cy; Papachrysostomou, Ch.; Theodorou, Z.; Kanari, P.; Constantinou, S. [State General Laboratory of Cyprus, Veterinary Drug Residues Lab, Kimonos 44, 1451 Nicosia (Cyprus)

    2009-04-01

    Within the EU the use of dapsone (4,4-diaminodiphenylsulfone) is prohibited in food-producing animals and consequently it's included in the Annex IV of the Directive 90/2377/EC. A quantitative confirmatory method has been developed and validated according to the criteria defined in the Commission Decision 2002/657/EC, for the determination of dapsone in meat and milk. Samples, after homogenization in alkaline conditions and organic solvent extraction, were purified on silica gel solid phase extraction cartridges. The eluate was evaporated and redissolved in mobile phase and was analysed by liquid chromatography tandem mass spectrometry (LC-MS/MS) in positive electrospray ionisation (ESI) using deuterium labelled Sulphadimidine-d7 as internal standard. The calculated value for, decision limit, CC{alpha} is 0.12 {mu}g kg{sup -1}, and the detection capability; CC{beta} value is 0.16 {mu}g kg{sup -1}.

  4. Using the column wall itself as resistive heater for fast temperature gradients in liquid chromatography.

    Science.gov (United States)

    De Pauw, Ruben; Pursch, Matthias; Desmet, Gert

    2015-11-13

    A new system is proposed for applying fast temperature gradients in liquid chromatography. It consists of a 0.7 mm × 150 mm fused-silica column coated with a 50 μm Nickel-layer, which is connecting with a power source and a temperature control system to perform fast and reproducible temperature gradients using the column wall itself as a resistive heater. Applying a current of 4A and passive cooling results in a maximal heating and cooling rate of, respectively, 71 and -21 °C/min. Multi-segment temperature gradients were superimposed on mobile phase gradients to enhance the selectivity for three sets of mixtures (pharmaceutical compounds, a highly complex mixture and an insecticide sample). This resulted in a higher peak count or better selectivities for the various mixtures. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Measurement of lumefantrine and its metabolite in plasma by high performance liquid chromatography with ultraviolet detection

    DEFF Research Database (Denmark)

    Khalil, Insaf F; Abildrup, Ulla; Alifrangis, Lene H

    2011-01-01

    Artemether-lumefantrine (ARM-LUM) has in recent years become the first-line treatment for uncomplicated malaria in many Sub-Saharan African countries. Vigorous monitoring of the therapeutic efficacy of this treatment is needed. This requires high-quality studies following standard protocols......; ideally, such studies should incorporate measurement of drug levels in the study patients to exclude the possibility that insufficient drug levels explain an observed treatment failure. Several methods for measuring lumefantrine (LUM) in plasma by HPLC are available; however, several of these methods have...... some limitations in terms of high costs and limited feasibility arising from large required sample volumes and demanding sample preparation. Therefore, we set out to develop a simpler reversed phase high performance liquid chromatography (RP-HPLC) method based on UV detection for simultaneous...

  6. [Application of liquid chromatography-high resolution mass spectrometry in toxicological screening].

    Science.gov (United States)

    Li, Xiao-Wen; Shen, Bao-Hua; Zhuo, Xian-Yi

    2011-10-01

    Due to the diversity of toxicologically relevant substances, the uncertainty of target compounds and the specificity of samples, toxicological screening techniques have always been valued by the forensic toxicologists. Depending on its powerful separation ability, superhigh resolution and accurate mass measurement, combined with the two levels spectrum database matching and abundance ratio of isotope ion, the liquid chromatography-high resolution mass spectrometry (LC-HRMS) analyzers have increasingly advantage in screening and identification of chemical compound. This review focuses on the applications of LC-HRMS in screening and identification of drug-of-abuse, prescription drugs, pesticide and stimulant. The prospect of LC-HRMS in forensic toxicology analysis is also included.

  7. Analysis of lipophilic pigments from a phototrophic microbial mat community by high performance liquid chromatography

    Science.gov (United States)

    Palmisano, A. C.; Cronin, S. E.; Des Marais, D. J.

    1988-01-01

    As assay for lipophilic pigments in phototrophic microbial mat communities using reverse phase-high performance liquid chromatography was developed which allows the separation of 15 carotenoids and chloropigments in a single 30 min program. Lipophilic pigments in a laminated mat from a commercial salina near Laguna Guerrero Negro, Baja California Sur, Mexico reflected their source organisms. Myxoxanthophyll, echinenone, canthaxanthin, and zeaxanthin were derived from cyanobacteria; chlorophyll c, and fucoxanthin from diatoms; chlorophyll a from cyanobacteria and diatoms; bacteriochlorophylls a and c, bacteriophaeophytin a, and gamma-carotene from Chloroflexus spp.; and beta-carotene from a variety of phototrophs. Sensitivity of detection was 0.6-6.1 ng for carotenoids and 1.7-12 ng for most chloropigments. This assay represents a significant improvement over previous analyses of lipophilic pigments in microbial mats and promises to have a wider application to other types of phototrophic communities.

  8. Determination of dapsone in meat and milk by liquid chromatography tandem mass spectrometry

    International Nuclear Information System (INIS)

    Hadjigeorgiou, M.; Papachrysostomou, Ch.; Theodorou, Z.; Kanari, P.; Constantinou, S.

    2009-01-01

    Within the EU the use of dapsone (4,4-diaminodiphenylsulfone) is prohibited in food-producing animals and consequently it's included in the Annex IV of the Directive 90/2377/EC. A quantitative confirmatory method has been developed and validated according to the criteria defined in the Commission Decision 2002/657/EC, for the determination of dapsone in meat and milk. Samples, after homogenization in alkaline conditions and organic solvent extraction, were purified on silica gel solid phase extraction cartridges. The eluate was evaporated and redissolved in mobile phase and was analysed by liquid chromatography tandem mass spectrometry (LC-MS/MS) in positive electrospray ionisation (ESI) using deuterium labelled Sulphadimidine-d7 as internal standard. The calculated value for, decision limit, CCα is 0.12 μg kg -1 , and the detection capability; CCβ value is 0.16 μg kg -1

  9. Two-dimensional liquid chromatography in pharmaceutical analysis. Instrumental aspects, trends and applications.

    Science.gov (United States)

    Iguiniz, Marion; Heinisch, Sabine

    2017-10-25

    The interest in two-dimensional liquid chromatography (2D-LC) has been growing up since the last decades. This promising technique appears as a relevant solution for various analytical challenges encountered in pharmaceutical analysis. The objective of this review is to give an overview of past, current and emerging trends in 2D-LC techniques applied to pharmaceutical compounds. The referenced studies cover the late 1980s to the present. Information regarding the different aspects of this analytical technique, including chromatographic conditions, instrumental setup and compounds of interest, was compiled and summarized into a synoptic table. Particular attention is paid to key features including (i) the interfaces used for coupling the two dimensions, (ii) the application fields, and (iii) the chromatographic modes that can be combined together. Finally an attempt is made to predict future advances in two-dimensional separation techniqes for pharmaceutical analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Electrochemically-modulated liquid chromatography (EMLC): Column design, retention processes, and applications

    Energy Technology Data Exchange (ETDEWEB)

    Ting, En -Yi [Iowa State Univ., Ames, IA (United States)

    1997-10-08

    This work describes the continued development of a new separation technique, electrochemically-modulated liquid chromatography (EMLC), from column design, retention mechanisms to pharmaceutical applications. The introduction section provides a literature review of the technique as well as a brief overview of the research in each of the chapters. This section is followed by four chapters which investigate the issues of EMLC column design, the retention mechanism of monosubstituted aromatic compounds, and the EMLC-based applications to two important classes of pharmaceutical compounds (i.e., corticosteroids and benzodiazepines). These four sections have been removed to process separately for inclusion on the database. The dissertation concludes with a general summary, a prospectus, and a list of references cited in the General Introduction. 32 refs.

  11. Characterization of free and bound fatty acids in human gallstones by capillary gas liquid chromatography

    International Nuclear Information System (INIS)

    Channa, N.A.; Khand, F.D.; Noorani, M.A.; Bhanger, M.I.

    2002-01-01

    Forty-four human gallstone samples either of pure cholesterol or cholesterol and bilirubin were randomly selected and analyzed by capillary gas liquid chromatography for the relative percentage composition of free and total fatty acids. The results showed that bound fatty acids were present in higher amounts than the free fatty acids. Amongst the bound fatty acids the percentage occurrence for palmitic acid was highest followed by stearic, oleic, linoleic and myristic acids. Fatty acids myristic, palmitic and linoleic were present in higher amounts in cholesterol gallstones, whereas stearic acid in cholesterol and bilirubin gallstones. When compared, no significant difference (p < 0.05) in the levels of free and bound fatty acids were seen in gallstones of males and females. The results suggest that bound fatty acids have a role to play in the structure of gallstones. (author)

  12. Characterisation of okadaic acid related toxins by liquid chromatography coupled with mass spectrometry.

    Science.gov (United States)

    Paz, Beatriz; Daranas, Antonio H; Cruz, Patricia G; Franco, José M; Pizarro, Gemita; Souto, María L; Norte, Manuel; Fernández, José J

    2007-08-01

    In the Diarrhetic Shellfish Poisoning (DSP) phenomena, the parent toxins, namely okadaic acid (OA) and/or dinophysistoxin-2 (DTX2), are predominantly found esterified. Therefore, a toxicity assessment of a sample can only be performed after an alkaline hydrolysis step in order to recover the parent molecules in their free form. The presence of several OA diol esters has already been confirmed in Prorocentrum lima and Prorocentrum belizeanum cultures. This paper reports on the analysis of OA diol esters using liquid chromatography coupled with mass spectrometry (LC-MS/MS), and establishes a method for their detection and identification based upon their retention times (RT) and the fragmentation patterns of their mass spectra.

  13. High-performance liquid chromatography determination of dapsone, monoacetyldapsone, and pyrimethamine in filter paper blood spots

    DEFF Research Database (Denmark)

    Rønn, A M; Lemnge, M M; Angelo, H R

    1995-01-01

    A high-performance liquid chromatography method for the simultaneous analysis of dapsone (DDS), the major metabolite of DDS, monoacetyldapsone (MADDS), and pyrimethamine (PYR) was modified for capillary blood samples obtained by finger prick and dried on filter paper. Limit of quantitation using...... 150 microliters whole blood dried on filter paper was found to be 20 ng/ml for DDS and PYR and 15 ng/ml for MADDS (precision filter...... paper method and the original whole-blood method was almost comparable. Standardization could therefore be obtained by the more simple whole-blood method. Dried filter paper samples stored at 19-22 degrees C were stable for months and for 2 weeks stored at 35 degrees C. The concentrations...

  14. High performance liquid chromatography of furfural and hydroxymethylfurfural in spirits and honey.

    Science.gov (United States)

    Jeuring, H J; Kuppers, F J

    1980-11-01

    Furfural (2-furaldehyde) and hydroxymethylfurfural (5-hydroxy-2-furaldehyde, HMF) are determined in brandy and honey by reverse phase high performance liquid chromatography. Brandies and other spirits are injected without sample preparation; honey is diluted with water and the solution is filtered before injection onto a reverse phase column with detection at 285 nm. The mobile phase is methanol--water (10 + 90) and the effluent flow rate is maintained at 1.0 mL/min. External standardization is used for quantitative determination. Recoveries from cognac and honey spiked at different levels ranged from 95 to 99% (furfural) and 95 to 100% (HMF). The furfural content of the brandies was also determined by the existing colorimetric method of the Bureau National Interprofessionel du Cognac. The HMF content of the honey was correlated to the results of the classic method of Winkler.

  15. Determination of methylparaben from cosmetic products by ultra performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    MANUELA M. MINCEA

    2009-06-01

    Full Text Available A new method for the determination of methylparaben by ultra-performance liquid chromatography (UPLC was developed. Methylparaben is often used as preservative, alone or in combination with other parabens, being added to cosmetic products, pharmaceutical products and foods to avoid microbial contamination. Due to its widespread use and potential risk to human health, assessing human exposure to this compound is of interest. A good determination and quantification of methylparaben was developed with a gradient elution using a mixture of methanol and water (60:40, v/v within 1.455 min. Under optimized conditions, the linear working range extends over two orders of magnitude with relative standard deviations of intra- and inter-day precision below 2.3 %, and a detection limit of 0.02 ng μL-1 for methylparaben. The proposed method was successfully applied to the assay of methylparaben in cosmetic products with minimal sample preparation.

  16. [Systematic evaluation of retention behavior of carbohydrates in hydrophilic interaction liquid chromatography].

    Science.gov (United States)

    Fu, Qing; Wang, Jun; Liang, Tu; Xu, Xiaoyong; Jin, Yu

    2013-11-01

    A systematic evaluation of retention behavior of carbohydrates in hydrophilic interaction liquid chromatography (HILIC) was performed. The influences of mobile phase, stationary phase and buffer salt on the retention of carbohydrates were investigated. According to the results, the retention time of carbohydrates decreased as the proportion of acetonitrile in mobile phase decreased. Increased time of carbohydrates was observed as the concentration of buffer salt in mobile phase increased. The retention behavior of carbohydrates was also affected by organic solvent and HILIC stationary phase. Furthermore, an appropriate retention equation was used in HILIC mode. The retention equation lnk = a + blnC(B) + cC(B) could quantitatively describe the retention factors of carbohydrates of plant origin with good accuracy: the relative error of the predicted time to actual time was less than 0.3%. The evaluation results could provide guidance for carbohydrates to optimize the experimental conditions in HILIC method development especially for carbohydrate separation

  17. High-throughput liquid chromatography for drug analysis in biological fluids: investigation of extraction column life.

    Science.gov (United States)

    Zeng, Wei; Fisher, Alison L; Musson, Donald G; Wang, Amy Qiu

    2004-07-05

    A novel method was developed and assessed to extend the lifetime of extraction columns of high-throughput liquid chromatography (HTLC) for bioanalysis of human plasma samples. In this method, a 15% acetic acid solution and 90% THF were respectively used as mobile phases to clean up the proteins in human plasma samples and residual lipids from the extraction and analytical columns. The 15% acetic acid solution weakens the interactions between proteins and the stationary phase of the extraction column and increases the protein solubility in the mobile phase. The 90% THF mobile phase prevents the accumulation of lipids and thus reduces the potential damage on the columns. Using this novel method, the extraction column lifetime has been extended to about 2000 direct plasma injections, and this is the first time that high concentration acetic acid and THF are used in HTLC for on-line cleanup and extraction column lifetime extension.

  18. Determination of selected azaarenes in water by bonded-phase extraction and liquid chromatography

    Science.gov (United States)

    Steinheimer, T.R.; Ondrus, M.G.

    1986-01-01

    A method for the rapid and simple quantitative determination of quinoline, isoquinoline, and five selected three-ring azaarenes in water has been developed. The azaarene fraction is separated from its carbon analogues on n-octadecyl packing material by edition with acidified water/acetonitrile. Concentration as great as 1000-fold is achieved readily. Instrumental analysis involves high-speed liquid chromatography on flexible-walled, wide-bore columns with fluorescence and ultraviolet detection at several wavelengths employing filter photometers in series. Method-validation data is provided as azaarene recovery efficiency from fortified samples. Distilled water, river water, contaminated ground water, and secondary-treatment effluent have been tested. Recoveries at part-per-billion levels are nearly quantitative for the three-ring compounds, but they decrease for quinoline and isoquinoline. ?? 1986 American Chemical Society.

  19. Quantitative determination of acetaminophen, phenylephrine and carbinoxamine in tablets by high-performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Carina de A. Bastos

    2009-01-01

    Full Text Available An alternative methodology for analysis of acetaminophen (Ace, phenylephrine (Phe and carbinoxamine (Car in tablets by ion-pair reversed phase high performance liquid chromatography was validated. The pharmaceutical preparations were analyzed by using a C18 column (5 μm, 300 mm, 3.9 mm and mobile phase consisting of 60% methanol and 40% potassium monobasic phosphate aqueous solution (62.46 mmol L-1 added with 1 mL phosphoric acid, 0.50 mL triethylamine and 0.25 g sodium lauryl sulfate. Isocratic analysis was performed under direct UV detection at 220 nm for Phe and Car and at 300 nm for Ace within 5 min.

  20. Detailed molecular characterization of castor oil ethoxylates by liquid chromatography multistage mass spectrometry.

    Science.gov (United States)

    Nasioudis, Andreas; van Velde, Jan W; Heeren, Ron M A; van den Brink, Oscar F

    2011-10-07

    The molecular characterization of castor oil ethoxylates (CASEOs) was studied by reverse-phase liquid chromatography (RPLC) mass spectrometry (MS) and multistage mass spectrometry (MS(n)). The developed RPLC method allowed the separation of the various CASEO components, and especially, the baseline separation of multiple nominal isobars (same nominal mass) and isomers (same exact mass). MS and MS(n) were used for the determination and structure elucidation of various structures and for the discrimination of the isobars and isomers. Different ionization techniques and adduct ions were also tested for optimization of the MS detection and the MS(n) fragmentation. A unique fragmentation pathway of ricinoleic acid is proposed, which can be used as a marker of the polymerization process and the topology of ethoxylation in the CASEO. In addition, characteristic neutral losses of ricinoleic acid reveal its (terminal or internal) position in the molecule. Copyright © 2011 Elsevier B.V. All rights reserved.

  1. Simultaneous determination of plasma total homocysteine and methionine by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Jiang, Yi; Mistretta, Brandon; Elsea, Sarah; Sun, Qin

    2017-01-01

    The sulfur-containing amino acid homocysteine is a cardiac risk factor and a biomarker for several inborn errors of metabolism in methionine synthesis. A simple LC-MS/MS method was developed and validated for determination of homocysteine and methionine in human plasma. Rapid separation was achieved using a reverse phase liquid chromatography. Mass spectrometry identification was performed in positive electrospray ionization mode for homocysteine and methionine. Accuracy, precision, linearity, recovery and sample stability were evaluated in the method validation. The test is applied in diagnosis of homocystinuria and monitoring total homocysteine levels. Moreover, simultaneous measurement of methionine helps in the differentiation of homocystinuria and some cobalamin disorders (such as cblC and cblD defects) without additional amino acid testing. Lastly, this assay is sensitive to detect reduced total homocysteine levels that are possibly seen in sulfocysteinuria and molybdenum cofactor deficiencies. Copyright © 2016. Published by Elsevier B.V.

  2. [Determination of aspirin and free salicylic acid in lysinipirine injection by high performance liquid chromatography].

    Science.gov (United States)

    Dong, Yu; Zhao, Yuan-zheng; Zhang, Yi-na

    2002-05-01

    The contents of aspirin and free salicylic acid in lysinipirine injection were determined by high performance liquid chromatography (HPLC). A Hypersil BDS C18 column was used with the mobile phase of methanol-water-acetic acid (35:65:3, volume ratio) and the detection wavelength of 280 nm. The average recoveries of aspirin and salicylic acid added were 99.27% (RSD = 0.8%) and 99.61%(RSD = 1.3%), respectively. The calibration curves had good linearity in the range of 0.028 g/L -0.141 mg/L and 0.77 mg/L -3.85 mg/L, and the correlation coefficients were 0.9999 and 0.9998 for aspirin and salicylic acid respectively.

  3. Development of high performance liquid chromatography for rapid determination of burn-up of nuclear fuels

    International Nuclear Information System (INIS)

    Joseph, M.; Karunasagar, D.; Saha, B.

    1996-01-01

    Burn-up an important parameter during evaluation of the performance of any nuclear fuel. Among the various techniques available, the preferred one for its determination is based on accurate measurement of a suitable fission product monitor and the residual heavy elements. Since isotopes of rare earth elements are generally used as burn-up monitors, conditions were standardized for rapid separation (within 15 minutes) of light rare earths using high performance liquid chromatography based on either anion exchange (Partisil 10 SAX) in methanol-nitric acid medium or by cation exchange on a reverse phase column (Spherisorb 5-ODS-2 or Supelcosil LC-18) dynamically modified with 1-octane sulfonate or camphor-10-sulfonic acid (β). Both these methods were assessed for separation of individual fission product rare earths from their mixtures. A new approach has been examined in detail for rapid assay of neodymium, which appears promising for faster and accurate measurement of burn-up. (author)

  4. Characterization of nine polyphenols in fruits of Malus pumila Mill by high-performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Lu Bai

    2016-04-01

    Full Text Available Polyphenols are important bioactive substances in apple. To explore the profiles of the nine representative polyphenols in this fruit, a high-performance liquid chromatography method has been established and validated. The validated method was successfully applied for the simultaneous characterization and quantification of these nine apple polyphenols in 11 apple extracts, which were obtained from six cultivars from Shaanxi Province, China. The results showed that only abscission of the Fuji apple sample was rich in the nine apple polyphenols, and the polyphenol contents of other samples varied. Although all the samples were collected in the same region, the contents of nine polyphenols were different. The proposed method could serve as a prerequisite for quality control of Malus products.

  5. DETERMINATION OF METOPROLOL IN PURE AND PHARMACEUTICAL DOSAGE FORMS BY SPECTROFLUOROMETRY AND HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

    Directory of Open Access Journals (Sweden)

    BILAL YILMAZ

    2011-03-01

    Full Text Available In this study, new and rapid spectrofluorometry and high performance liquid chromatography (HPLC methods were developed for determination of metoprolol in pure and pharmaceutical dosage forms. The solvent system, wavelength of detection and chromatographic conditions were optimized in order to maximize the sensitivity of both proposed methods. The linearity was established over the concentration range of 50-4000 ng ml-1 for spectrofluorometry and 5.0-300 ng ml-1 for HPLC methods. The intra- and inter-day relative standard deviation (RSD was less than 4.14 and 3.86% for spectrofluorometry and HPLC, respectively. The limit of quantitation was determined as 30 and 5.0 ng ml-1 for spectrofluorometry and HPLC, respectively. No interference was found from tablet excipients at the selected assay conditions. The methods were applied for the quality control of commercial metoprolol dosage forms to quantify the drug and to check the formulation content uniformity.

  6. Robust optimization of psychotropic drug mixture separation in hydrophilic interaction liquid chromatography.

    Science.gov (United States)

    Rakić, Tijana; Jovanović, Marko; Dumić, Aleksandra; Pekić, Marina; Ribić, Sanja; Stojanović, Biljana Jancić

    2013-01-01

    This paper presents multiobjective optimization of complex mixtures separation in hydrophilic interaction liquid chromatography (HILIC). The selected model mixture consisted of five psychotropic drugs: clozapine, thioridazine, sulpiride, pheniramine and lamotrigine. Three factors related to the mobile phase composition (acetonitrile content, pH of the water phase and concentration of ammonium acetate) were optimized in order to achieve the following goals: maximal separation quality, minimal total analysis duration and robustness of an optimum. The consideration of robustness in early phases of the method development provides reliable methods with low risk for failure in validation phase. The simultaneous optimization of all goals was achieved by multiple threshold approach combined with grid point search. The identified optimal separation conditions (acetonitrile content 83%, pH of the water phase 3.5 and ammonium acetate content in water phase 14 mM) were experimentally verified.

  7. Analysis of ACE inhibitors in pharmaceutical dosage forms by derivative UV spectroscopy and liquid chromatography (HPLC).

    Science.gov (United States)

    Bonazzi, D; Gotti, R; Andrisano, V; Cavrini, V

    1997-11-01

    Derivative UV spectroscopy and high performance liquid chromatography (HPLC) were applied to the determination of angiotensin-converting enzyme (ACE) inhibitors in their pharmaceutical dosage forms. For spectrophotometric determinations, the more appropriate derivative order was selected for each drug: ramipril (third-order), benazepril (second-order), enalapril maleate (second-order), lisinopril (first- and second-order) and quinapril (first-order). Reverse phase HPLC procedures (ODS column) were developed able to provide a single, symmetric peak for each drug; mixtures A-B, where A is 20 mM sodium heptansulphonate (pH 2.5) and B is acetonitrile-THF (95:5 v/v), proved to be suitable mobile phases to obtain selective separations of the cited ACE inhibitors. At ambient temperature, a low pH value (2.5) was found to be critical to avoid peak splitting and band broadening.

  8. Statistical quality assessment and outlier detection for liquid chromatography-mass spectrometry experiments

    Directory of Open Access Journals (Sweden)

    Schulz-Trieglaff Ole

    2009-04-01

    Full Text Available Abstract Background Quality assessment methods, that are common place in engineering and industrial production, are not widely spread in large-scale proteomics experiments. But modern technologies such as Multi-Dimensional Liquid Chromatography coupled to Mass Spectrometry (LC-MS produce large quantities of proteomic data. These data are prone to measurement errors and reproducibility problems such that an automatic quality assessment and control become increasingly important. Results We propose a methodology to assess the quality and reproducibility of data generated in quantitative LC-MS experiments. We introduce quality descriptors that capture different aspects of the quality and reproducibility of LC-MS data sets. Our method is based on the Mahalanobis distance and a robust Principal Component Analysis. Conclusion We evaluate our approach on several data sets of different complexities and show that we are able to precisely detect LC-MS runs of poor signal quality in large-scale studies.

  9. An electrospray ionization-ion mobility spectrometer as detector for high- performance liquid chromatography.

    Science.gov (United States)

    Zühlke, Martin; Riebe, Daniel; Beitz, Toralf; Löhmannsröben, Hans-Gerd; Zenichowski, Karl; Diener, Marc; Linscheid, Michael W

    2015-01-01

    The application of electrospray ionization (ESI) ion mobility (IM) spectrometry on the detection end of a high-performance liquid chromatograph has been a subject of study for some time. So far, this method has been limited to low flow rates or has required splitting of the liquid flow. This work presents a novel concept of an ESI source facilitating the stable operation of the spectrometer at flow rates between 10 μL mn(-1) and 1500 μL min(-1) without flow splitting, advancing the T-cylinder design developed by Kurnin and co-workers. Flow rates eight times faster than previously reported were achieved because of a more efficient dispersion of the liquid at increased electrospray voltages combined with nebulization by a sheath gas. Imaging revealed the spray operation to be in a rotationally symmetric multijet mode. The novel ESI-IM spectrometer tolerates high water contents (≤90%) and electrolyte concentrations up to 10mM, meeting another condition required of high-performance liquid chromatography (HPLC) detectors. Limits of detection of 50 nM for promazine in the positive mode and 1 μM for 1,3-dinitrobenzene in the negative mode were established. Three mixtures of reduced complexity (five surfactants, four neuroleptics, and two isomers) were separated in the millisecond regime in stand-alone operation of the spectrometer. Separations of two more complex mixtures (five neuroleptics and 13 pesticides) demonstrate the application of the spectrometer as an HPLC detector. The examples illustrate the advantages of the spectrometer over the established diode array detector, in terms of additional IM separation of substances not fully separated in the retention time domain as well as identification of substances based on their characteristic Ims.

  10. Alternative sample-introduction technique to avoid breakthrough in gradient-elution liquid chromatography of polymers.

    Science.gov (United States)

    Reingruber, Eva; Bedani, Filippo; Buchberger, Wolfgang; Schoenmakers, Peter

    2010-10-15

    Gradient-elution liquid chromatography (GELC) is a powerful tool for the characterization of synthetic polymers. However, gradient-elution chromatograms often suffer from breakthrough phenomena. Breakthrough can be averted by using a sample solvent as weak as the mobile phase. However, this approach is only applicable to polymers for which a sufficiently strong solvent exists which is at the same time a weak eluent. Finding such a solvent for a given polymer can be laborious or may even be impossible. Besides, when working with comprehensive two-dimensional LC the effluent of the first dimension is the injection solvent of the second dimension. In this case, it is not possible to avoid breakthrough by adjusting the eluent strength of the second-dimension injection solvent. Therefore, another strategy to avert breakthrough has to be implemented. In this work, we successfully avoided breakthrough in GELC by mixing the mobile phase not before, but after the autosampler. This was demonstrated measuring a blend of poly(methyl methacrylate) standards with different molecular-weights as model mixture with comprehensive two-dimensional GELC×size-exclusion chromatography. The strategy is thought to be applicable to all substances with a sufficiently strong dependence of retention on mobile-phase composition. This typically applies to large molecules (synthetic and natural polymers) and allows efficient refocusing. Unretained and barely retained substances are not refocused and therefore suffer in the proposed setup from peak broadening. Copyright © 2010 Elsevier B.V. All rights reserved.

  11. High performance liquid chromatography resolution of ubiquitin pathway enzymes from wheat germ

    International Nuclear Information System (INIS)

    Sullivan, M.L.; Callis, J.; Vierstra, R.D.

    1990-01-01

    The highly conserved protein ubiquitin is involved in several cellular processes in eukaryotes as a result of its covalent ligation to a variety of target proteins. Here, we describe the purification of several enzymatic activities involved in ubiquitin-protein conjugate formation and disassembly from wheat germ (Triticum vulgare) by a combination of ubiquitin affinity chromatography and anion-exchange high performance liquid chromatography. Using this procedure, ubiquitin activating enzyme (E1), several distinct ubiquitin carrier proteins (E2s) with molecular masses of 16, 20, 23, 23.5, and 25 kilodaltons, and a ubiquitin-protein hydrolase (isopeptidase) were isolated. Purified E1 formed a thiol ester linkage with 125 I-ubiquitin in an ATP-dependent manner and transferred bound ubiquitin to the various purified E2s. The ubiquitin protein hydrolase fraction was sensitive to hemin, and in an ATP-independent reaction, was capable of removing the ubiquitin moiety from both ubiquitin 125 I-lysozyme conjugates (ε-amino or isopeptide linkage) and the ubiquitin 52-amino acid extension protein fusion (α-amino or peptide linkage). Using this procedure, wheat germ represents an inexpensive source from which enzymes involved in the ubiquitin pathway may be isolated

  12. Monitoring aldehyde production during frying by reversed-phase liquid chromatography.

    Science.gov (United States)

    Lane, R H; Smathers, J L

    1991-01-01

    Acrolein (2-propenal) and other low molecular weight aldehydes (LMWAs) formed by degradation of the frying medium (triglycerides) were monitored by liquid chromatography (LC) during preparation of fried items. LMWA contents of coatings from codfish and of doughnuts and their volatiles that codistill with steam are monitored by trapping the vapors and distillate from the food matrix in a 2,4-dinitrophenylhydrazine solution. The resulting hydrazones are partitioned from the aqueous phase, first into isooctane and then into acetonitrile for LC analysis. The hydrazones are separated and quantified on a C18 reversed-phase column with acetonitrile-water as the mobile phase. LMWAs are confirmed by gas chromatography/mass spectrometry. No difference was found in LMWA content in coatings from fish fillets fried at 182 or 204 degrees C. Cake doughnuts were higher in acrolein content than yeast-raised doughnuts prepared under similar conditions. Freshness of the frying medium, frying time, and batch size did not seem to influence LMWA production from doughnuts. Results indicated that most of the LMWAs formed codistilled with steam during frying rather than remaining with the food item.

  13. 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)

  14. Evaluation of hydrophilic interaction liquid chromatography stationary phases for analysis of opium alkaloids.

    Science.gov (United States)

    Bagheri, Mohsen; Taheri, Mohammadreza; Farhadpour, Mohsen; Rezadoost, Hassan; Ghassempour, Alireza; Aboul-Enein, Hassan Y

    2017-08-18

    The separation of a mixture containing five major opium alkaloids, namely morphine, codeine, thebaine, noscapine and papaverine has been investigated in hydrophilic interaction liquid chromatography (HILIC) mode using five different stationary phases: bare silica, zwitterion, aminopropyl, diol and cyanopropyl. In order to propose the appropriate column for separation and purification, retention behaviors of the five natural opioids have been studied on mentioned HILIC stationary phases. The mechanism of separation in diverse HILIC media, based on the formation of water-rich layer on surface of the HILIC stationary phases and the physicochemical properties of opium alkaloids, such as pKa (acidic pK) and the octanol-water distribution coefficient (log Do/w) are discussed. Chromatographic responses including modified limit of detection LOD m , signal to noise ratio (S/N) m , and defined modified R Sm have considered for suggestion of the suitable column for quantitative/qualitative and preparative purposes. According to the obtained results, diol stationary phase is best suited for analytical chromatography, whereas bare silica and zwitterionic stationary phases are appropriate for preparative applications. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. Insights in groundwater organic matter from Liquid Chromatography-Organic Carbon Detection

    Science.gov (United States)

    Rutlidge, H.; Oudone, P.; McDonough, L.; Andersen, M. S.; Baker, A.; Meredith, K.; O'Carroll, D. M.

    2017-12-01

    Understanding the processes that control the concentration and characteristics of organic matter in groundwater has important implications for the terrestrial global carbon budget. Liquid Chromatography - Organic Carbon Detection (LC-OCD) is a size-exclusion based chromatography technique that separates the organic carbon into molecular weight size fractions of biopolymers, humic substances, building blocks (degradation products of humic substances), low molecular weight acids and low molecular weight neutrals. Groundwater and surface water samples were collected from a range of locations in Australia representing different surface soil, land cover, recharge type and hydrological properties. At one site hyporheic zone samples were also collected from beneath a stream. The results showed a general decrease in the aromaticity and molecular weight indices going from surface water, hyporheic downwelling and groundwater samples. The aquifer substrate also affected the organic composition. For example, groundwater samples collected from a zone of fractured rock showed a relative decrease in the proportion of humic substances, suggestive of sorption or degradation of humic substances. This work demonstrates the potential for using LC-OCD in elucidating the processes that control the concentration and characteristics of organic matter in groundwater.

  16. Chemistry and liquid chromatography methods for the analyses of primary oxidation products of triacylglycerols.

    Science.gov (United States)

    Zeb, A

    2015-05-01

    Triacylglycerols (TAGs) are one of the major components of the cells in higher biological systems, which can act as an energy reservoir in the living cells. The unsaturated fatty acid moiety is the key site of oxidation and formation of oxidation compounds. The TAG free radical generates several primary oxidation compounds. These include hydroperoxides, hydroxides, epidioxides, hydroperoxy epidioxides, hydroxyl epidioxides, and epoxides. The presence of these oxidized TAGs in the cell increases the chances of several detrimental processes. For this purpose, several liquid chromatography (LC) methods were reported in their analyses. This review is therefore focused on the chemistry, oxidation, extraction, and the LC methods reported in the analyses of oxidized TAGs. The studies on thin-layer chromatography were mostly focused on the total oxidized TAGs separation and employ hexane as major solvent. High-performance LC (HPLC) methods were discussed in details along with their merits and demerits. It was found that most of the HPLC methods employed isocratic elution with methanol and acetonitrile as major solvents with an ultraviolet detector. The coupling of HPLC with mass spectrometry (MS) highly increases the efficiency of analysis as well as enables reliable structural elucidation. The use of MS was found to be helpful in studying the oxidation chemistry of TAGs and needs to be extended to the complex biological systems.

  17. Simulating Retention in Gas-Liquid Chromatography: Benzene, Toluene, and Xylene Solutes

    Energy Technology Data Exchange (ETDEWEB)

    WICK,COLLIN D.; MARTIN,MARCUS G.; SIEPMANN, J. ILJA; SCHURE,MARK R.

    2000-07-12

    Accurate predictions of retention times, retention indices, and partition constants are a long sought-after goal for theoretical studies in chromatography. Although advances in computational chemistry have improved the understanding of molecular interactions, little attention has been focused on chromatography, let alone calculations of retention properties. Configurational-bias Monte Carlo simulations in the isobaric-isothermal Gibbs ensemble were used to investigate the partitioning of benzene, toluene, and the three xylene isomers between a squalane liquid phase and a helium vapor phase. The united-atom representation of the TraPPE (Transferable Potentials for Phase Equilibria) force field was used for all solutes and squalane. The Gibbs free energies of transfer and Kovats retention indices of the solutes were calculated directly from the partition constants (which were averaged over several independent simulations). While the calculated Kovats indices of benzene and toluene at T = 403 K are significantly higher than their experimental counterparts, much better agreement is found for the xylene isomers at T = 365 K.

  18. Ionic liquid-regenerated macroporous cellulose monolith: Fabrication, characterization and its protein chromatography.

    Science.gov (United States)

    Du, Kaifeng

    2017-04-21

    Macroporous cellulose monolith as chromatographic support was successfully fabricated from an ionic liquid dissolved cellulose solution by an emulsification method and followed by the cross-linking reaction and DEAE modification. With the physical characterization, the cellulose monolith featured by both the interconnected macropores in range of 0.5-2.5μm and the diffusion pores centered at about 10nm. Given the bimodal pore system, the monolith possessed the specific surface area of 36.4m 2 g -1 and the column permeability of about 7.45×10 -14 m 2 . After the DEAE modification, the anion cellulose monolith was evaluated for its chromatography performances. It demonstrated that the static and dynamic adsorption capacity of BSA reached about 66.7mgmL -1 and 43.9mgmL -1 at 10% breakthrough point, respectively. The results were comparable to other chromatographic adsorbent. In addition, the proteins mixture with different pI was well separated at high flow velocity (611.0cmh -1 ) and high protein recovery (over 97%), proving the macroporous cellulose monolith had excellent separation performance. In this way, the prepared cellulose monolith with bimodal pores system is expected for the potential application in high-speed chromatography. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Core-shell particles: preparation, fundamentals and applications in high performance liquid chromatography.

    Science.gov (United States)

    Hayes, Richard; Ahmed, Adham; Edge, Tony; Zhang, Haifei

    2014-08-29

    The challenges in HPLC are fast and efficient separation for a wide range of samples. Fast separation often results in very high operating pressure, which places a huge burden on HPLC instrumentation. In recent years, core-shell silica microspheres (with a solid core and a porous shell, also known as fused-core or superficially porous microspheres) have been widely investigated and used for highly efficient and fast separation with reasonably low pressure for separation of small molecules, large molecules and complex samples. In this review, we firstly show the types of core-shell particles and how they are generally prepared, focusing on the methods used to produce core-shell silica particles for chromatographic applications. The fundamentals are discussed on why core-shell particles can perform better with low back pressure, in terms of van Deemter equation and kinetic plots. The core-shell particles are compared with totally porous silica particles and also monolithic columns. The use of columns packed with core-shell particles in different types of liquid chromatography is then discussed, followed by illustrating example applications of such columns for separation of various types of samples. The review is completed with conclusion and a brief perspective on future development of core-shell particles in chromatography. Copyright © 2014 The Authors. Published by Elsevier B.V. All rights reserved.

  20. Evaluation of nanoflow liquid chromatography high resolution mass spectrometry for pesticide residue analysis in food.

    Science.gov (United States)

    Moreno-González, David; Pérez-Ortega, Patricia; Gilbert-López, Bienvenida; Molina-Díaz, Antonio; García-Reyes, Juan F; Fernández-Alba, Amadeo R

    2017-08-25

    This article reports on the evaluation of nanoflow liquid chromatography-mass spectrometry (LC-MS) for pesticide residue analysis in food. The approach is based on the use of reversed-phase C18nano columns with an integrated emitter, so that separation, ionization and detection are performed minimizing dead volumes. The use of nanoflow not only increases ionization efficiency and minimizes ionization suppression but also boost sensitivity compared to analytical-scale LC-MS methods. The nanoflow LC system was combined with full-scan high resolution mass spectrometry using a Q-Exactive Orbitrap instrument. The analytical performance was assessed for over 60 representative pesticides in five representative commodities (tomato, baby food, orange, fruit-based jam and olive oil). The sensitivity achieved with this configuration enables the implementation of high dilution factors (eg. 1:20, 1:50 or beyond) in pesticide residue workflows without compromising sensitivity, featuring limits of quantitation in the low ng kg -1 range. Using this dilution factors, signal suppression was found negligible in most cases (<10% in most cases, especially with 1:50 dilution), so that matrix-matched standards may be skipped, thus simplifying laboratory workflows. The robustness of the nanoflow LC system and its capability to withstand long analytical runs was also evaluated. Appropriate precision in terms of peak area and retention time was obtained at different concentration levels for over 125 injections without any instrument servicing. The main benefits of the nanoflow liquid chromatography approach are the high sensitivity gain and the outstanding reduction in matrix effects thanks to the high sample dilution factors that can be implemented, along with the substantial reduction in solvent usage. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Purification of human albumin by the combination of the method of Cohn with liquid chromatography

    Directory of Open Access Journals (Sweden)

    Tanaka K.

    1998-01-01

    Full Text Available Large volumes of plasma can be fractionated by the method of Cohn at low cost. However, liquid chromatography is superior in terms of the quality of the product obtained. In order to combine the advantages of each method, we developed an integrated method for the production of human albumin and immunoglobulin G (IgG. The cryoprecipitate was first removed from plasma for the production of factor VIII and the supernatant of the cryoprecipitate was fractionated by the method of Cohn. The first precipitate, containing fractions (F-I + II + III, was used for the production of IgG by the chromatographic method (see Tanaka K et al. (1998 Brazilian Journal of Medical and Biological Research, 31: 1375-1381. The supernatant of F-I + II + III was submitted to a second precipitation and F-IV was obtained and discarded. Albumin was obtained from the supernatant of the precipitate F-IV by liquid chromatography, ion-exchange on DEAE-Sepharose FF, filtration through Sephacryl S-200 HR and introduction of heat treatment for fatty acid precipitation. Viral inactivation was performed by pasteurization at 60ºC for 10 h. The albumin product obtained by the proposed procedure was more than 99% pure for the 15 lots of albumin produced, with a mean yield of 25.0 ± 0.5 g/l plasma, containing 99.0 to 99.3% monomer, 0.7 to 1.0% dimers, and no polymers. Prekallikrein activator levels were <=5 IU/ml. This product satisfies the requirements of the 1997 Pharmacopée Européenne.

  2. Analysis of drugs of abuse in wastewater by hydrophilic interaction liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    van Nuijs, Alexander L N; Tarcomnicu, Isabela; Bervoets, Lieven; Blust, Ronny; Jorens, Philippe G; Neels, Hugo; Covaci, Adrian

    2009-10-01

    The simultaneous analysis of nine drugs of abuse (DOAs) and their metabolites (amphetamine, methamphetamine, methylenedioxymethamphetamine, methadone, 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine, cocaine, benzoylecgonine, ecgonine methyl ester and 6-monoacetylmorphine) in wastewater based on hydrophilic interaction liquid chromatography (HILIC) coupled to tandem mass spectrometry (MS/MS) was optimised and validated. For each analyte, the deuterated analogue was used for quantification. The separation by HILIC showed good performance for all compounds, especially for the hydrophilic compounds, which elute early (amphetamine-like stimulants) or show no retention (ecgonine methyl ester) in reversed-phase liquid chromatography. Sample preparation based on solid-phase extraction was optimised by comparing Oasis HLB and Oasis MCX sorbents for various parameters such as sample pH, amount of sorbent bed and washing solvent. The method was validated for each compound by assessing the following parameters (following International Conference on Harmonisation guidelines): specificity, limit of quantification (LOQ), linearity, accuracy, precision, recovery and matrix effects. LOQs were 2 ng/L for 6-monoacetylmorphine, ecgonine methyl ester and amphetamine and 1 ng/L for the rest of the compounds, corresponding with the lowest point in the calibration curve. Except for 6-monoacetylmorphine, all compounds were detected from 1 to 819 ng/L in influent wastewater samples (n = 12) collected from 11 different wastewater treatment plants across Belgium. The presence of ecgonine methyl ester in wastewater could be demonstrated for the first time. In the future, the new HILIC-MS/MS method will be applied to assess the use of DOAs in Belgium using the "sewage epidemiology" approach.

  3. Structural elucidation of metolachlor photoproducts by liquid chromatography/high-resolution tandem mass spectrometry.

    Science.gov (United States)

    Nicol, Édith; Genty, Christophe; Bouchonnet, Stéphane; Bourcier, Sophie

    2015-12-15

    Metolachlor is one of the most intensively used chloroacetanilide herbicides in agriculture. It has been detected in water; consequently, under UV-visible irradiation, it can be transformed in degradation products (TPs). The structures of TPs were elucidated by liquid chromatography/high-resolution tandem mass spectrometry (LC/HR-MS/MS). The potential toxicities of these TPs were estimated by in silico tests. Aqueous solutions of metolachlor were irradiated in a self-made reactor equipped with a mercury vapor lamp. Analyses were carried out using high-performance liquid chromatography coupled to quadrupole time-of-flight (QTOF) mass spectrometer. High-resolution m/z measurements, MS/MS and isotopic labeling experiments allowed structural elucidation of metolachlor TPs. Their toxicities were estimated in silico, using the T.E.S.T. Ten major metolachlor photoproducts were characterized by LC/MS/MS after irradiation of metolachlor in aqueous solution. Elucidation of their chemical structures was identified using high-resolution measurements and MS/MS experiments. They resulted from the combination of dehalogenation, hydroxylation and cyclisation processes. The potential oral rat lethal dose (LD50) was assessed with QSAR tests for metolachlor and each photoproduct. Results indicate that most of the TPs are much more toxic than metolachlor. UV-vis irradiation of metolachlor in aqueous solution leads to the formation of ten photoproducts. QSAR estimations show that the location of added hydroxyl group(s) is of key relevance as regards to biological activity and that routine water analysis should take into account the TPs are more toxic than the parent molecule. Copyright © 2015 John Wiley & Sons, Ltd.

  4. Quantification of liquid products from the electroreduction of CO2 and CO using static headspace-gas chromatography and nuclear magnetic resonance spectroscopy

    DEFF Research Database (Denmark)

    Bertheussen, Erlend; Abghoui, Younes; Jovanov, Zarko P.

    2017-01-01

    Static headspace-gas chromatography (HS-GC) useful for ex-situ liquid product analysis. Could complement high-performance liquid chromatography and NMR spectroscopy. Particularly high sensitivity towards compounds with high vapor pressure. Detection limits below 0.5μM were shown for acetaldehyde ...

  5. Determination of organophosphorus pesticides by dispersive liquid-liquid micro extraction coupled with gas chromatography-electron capture detection

    International Nuclear Information System (INIS)

    Mohd Marsin Sanagi; Siti Umairah Mokhtar; Mazidatul Akmam Miskam; Wan Aini Wan Ibrahim

    2011-01-01

    A simple, rapid and sensitive method termed as dispersive liquid-liquid micro extraction (DLLME) combined with gas chromatography-electron capture detector (GC-ECD) was developed for the determination of selected organophosphorus pesticides (OPPs) namely chloropyrifos, dimethoate and diazinon in water sample. In this method, a mixture of carbon disulfide, CS 2 (extraction solvent) and methanol (disperser solvent) was rapidly injected using syringe into the 5.00 mL water sample to form a cloudy solution where the OPPs were extracted into the fine droplets of extraction solvent. Upon centrifugation for 3 min at 3500 rpm, the fine droplets were sedimented at the bottom of the centrifuge tube. Sedimented phase (1 μL) was injected into the GC-ECD for separation and determination of OPPs. Important extraction parameters, such as type of disperser solvent, volume of extraction solvent and volume of disperser solvent were investigated. The optimized conditions for DLLME of the selected OPPs were methanol as disperser solvent, 30 μL of extraction solvent (CS 2 ) and 1.0 mL of disperser solvent (methanol). Under the optimum extraction conditions, the method showed good linearity in the range of 0.1 to 1.0 μg/ mL with correlation coefficient (r 2 ), in the range of 0.9976 to 0.9994 and low limits of detection (LOD) between 0.047 and 0.201 μg/ mL. The proposed method provided acceptable recoveries (72.67- 144 %) with good RSDs ranging from 2.74 % to 7.48 %. This method was successfully applied to the determination of OPPs in water samples obtained from a golf course and chloropyrifos and diazinon were detected at concentration 0.18 μg/ mL and 0.07 μg/ mL, respectively. (author)

  6. Determination of pharmaceuticals in soils and sediments by pressurized liquid extraction and liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Vazquez-Roig, Pablo; Segarra, Ramón; Blasco, Cristina; Andreu, Vicente; Picó, Yolanda

    2010-04-16

    The present work describes the development of a sensitive analytical method based on pressurized liquid extraction (PLE) and pre-concentration by solid-phase extraction (SPE), followed by liquid chromatography-electrospray tandem mass spectrometry (LC-ESI-MS/MS) for the determination of seventeen pharmaceuticals in soils and sediments. The method is based on sample homogenisation using Na(2)-EDTA washed sand and extraction with water at 90 degrees C. Special emphasis was placed on the optimization of the extraction procedure to develop a green method that reduces, at a maximum, the use of organic solvents in order to eliminate matrix components during the clean-up. The proposed method was linear in a concentration range from 0.3 to 333ngg(-1), with correlation coefficients higher than 0.993. Method detection (MDLs) and quantification (MQLs) limits ranged from 0.1 to 6.8ngg(-1) and from 0.25 to 23ngg(-1), respectively. Absolute recoveries were analyte dependent, varying between 50% and 105% at the MQL level, except for fenofibrate (40%) and diclofenac (34%). The intra-day and inter-day precision was given by RSD values from 0.7% to 7.9% and from 1.6% to 14.5%, respectively. Acetaminophen, carbamazepine, ciprofloxacin, clofibric acid, codeine, diazepam, fenofibrate, metropolol, ofloxacin and propanolol were detected at concentrations from MDL to 35.62ngg(-1) in soils and sediments from marsh areas. Due to the low recoveries, results for fenofibrate and diclofenac can only be considered as semi-quantitative. The method was fully suitable for the other 15 pharmaceuticals. Copyright 2009 Elsevier B.V. All rights reserved.

  7. Determination of estrogenic mycotoxins in environmental water samples by low-toxicity dispersive liquid-liquid microextraction and liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Emídio, Elissandro Soares; da Silva, Claudia Pereira; de Marchi, Mary Rosa Rodrigues

    2015-04-24

    A novel, simple, rapid and eco-friendly method based on dispersive liquid-liquid microextraction using a bromosolvent was developed to determine six estrogenic mycotoxins (zearalenone, zearalanone, α-zearalanol, β-zearalanol, α-zearalenol and β-zearalenol) in water samples by liquid chromatography-electrospray ionization tandem mass spectrometry in the negative mode (LC-ESI-MS/MS). The optimal conditions for this method include the use of 100 μL bromocyclohexane as an extraction solvent (using a non-dispersion solvent), 10 mL of aqueous sample (adjusted to pH 4), a vortex extraction time of 2 min, centrifugation for 10 min at 3500 rpm and no ionic strength adjustment. The calibration function was linear and was verified by applying the Mandel fitting test with a 95% confidence level. No matrix effect was observed. According to the relative standard deviations (RSDs), the precision was better than 13% for the repeatability and intermediate precision. The average recoveries of the spiked compounds ranged from 81 to 118%. The method limits of detection (LOD) and quantification (LOQ) considering a 125-fold pre-concentration step were 4-20 and 8-40 ng L(-1), respectively. Next, the method was applied to the analysis of the environmental aqueous samples, demonstrating the presence of β-zearalanol and zearalanone in the river water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  8. A new concept of hollow fiber liquid-liquid-liquid microextraction compatible with gas chromatography based on two immiscible organic solvents.

    Science.gov (United States)

    Ghambarian, Mahnaz; Yamini, Yadollah; Esrafili, Ali; Yazdanfar, Najmeh; Moradi, Morteza

    2010-09-03

    A new concept of liquid-liquid-liquid microextraction (LLLME) was introduced based on applying two immiscible organic solvents in lumen and wall pores of hollow fiber (HF). With this methodology, analytes of interest can be extracted from aqueous sample, into a thin layer of organic solvent (dodecane) sustained in the pores of a porous hollow fiber, and further into a muL volume of organic acceptor (acetonitrile or methanol) located inside the lumen of the hollow fiber. Some chlorophenols (CPs) were selected as model compounds for developing and evaluating of the method performance. The analysis was performed by gas chromatography-electron capture detection (GC-ECD) without derivatization. The factors affecting the HF-LLLME of target compounds were investigated and the optimal extraction conditions were established. Under the optimum conditions, preconcentration factors in a range of 208-895 were obtained. The performance of the proposed method was studied in terms of linear dynamic ranges (LDRs from 0.02 to 100ngmL(-1)), linearity (R(2)> or =0.995), precision (RSD %HF-LLLME also served as a technique for sample clean-up. 2010 Elsevier B.V. All rights reserved.

  9. Automated dispersive liquid-liquid microextraction coupled to high performance liquid chromatography - cold vapour atomic fluorescence spectroscopy for the determination of mercury species in natural water samples.

    Science.gov (United States)

    Liu, Yao-Min; Zhang, Feng-Ping; Jiao, Bao-Yu; Rao, Jin-Yu; Leng, Geng

    2017-04-14

    An automated, home-constructed, and low cost dispersive liquid-liquid microextraction (DLLME) device that directly coupled to a high performance liquid chromatography (HPLC) - cold vapour atomic fluorescence spectroscopy (CVAFS) system was designed and developed for the determination of trace concentrations of methylmercury (MeHg + ), ethylmercury (EtHg + ) and inorganic mercury (Hg 2+ ) in natural waters. With a simple, miniaturized and efficient automated DLLME system, nanogram amounts of these mercury species were extracted from natural water samples and injected into a hyphenated HPLC-CVAFS for quantification. The complete analytical procedure, including chelation, extraction, phase separation, collection and injection of the extracts, as well as HPLC-CVAFS quantification, was automated. Key parameters, such as the type and volume of the chelation, extraction and dispersive solvent, aspiration speed, sample pH, salt effect and matrix effect, were thoroughly investigated. Under the optimum conditions, linear range was 10-1200ngL -1 for EtHg + and 5-450ngL -1 for MeHg + and Hg 2+ . Limits of detection were 3.0ngL -1 for EtHg + and 1.5ngL -1 for MeHg + and Hg 2+ . Reproducibility and recoveries were assessed by spiking three natural water samples with different Hg concentrations, giving recoveries from 88.4-96.1%, and relative standard deviations <5.1%. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Extraction and analysis of auxins in plants using dispersive liquid-liquid microextraction followed by high-performance liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Lu, Qiaomei; Chen, Lihui; Lu, Minghua; Chen, Guonan; Zhang, Lan

    2010-03-10

    Auxin plays an important role in cell differentiation, apical dominance, and tropism in plants. A new method based on dispersive liquid-liquid microextraction (DLLME) combined with high-performance liquid chromatography-fluorescence detection (HPLC-FLD) has been established to detect auxin. A mixture of CHCl(3) (extraction solvent) and acetone (disperser solvent) was injected quickly into a sample solution with desired salt concentration and pH value, and then a cloudy solution consisting of many dispersed fine droplets of CHCl(3) was formed. After centrifugation, the sedimented phase was withdrawn and directly analyzed by HPLC-FLD. Under optimal conditions, four auxins were baseline separated within 3.5 min, with the minimal limit of detection of 0.02 ng mL(-1) and coefficient correlations in the range of 0.9980-0.9995. This simple method was successfully applied to real sample analysis. Experimental results showed that DLLME was a high-performance and powerful preconcentration method to extract and enrich related plant auxin.

  11. Temperature-controlled liquid-liquid microextraction combined with high-performance liquid chromatography for the simultaneous determination of diazinon and fenitrothion in water and fruit juice samples.

    Science.gov (United States)

    Bazmandegan-Shamili, Alireza; Dadfarnia, Shayessteh; Shabani, Ali Mohammad Haji; Moghadam, Masoud Rohani; Saeidi, Mahboubeh

    2018-02-28

    A simple, environmentally benign, and rapid method based on temperature-controlled liquid-liquid microextraction using a deep eutectic solvent was developed for the simultaneous extraction/preconcentration of diazinon and fenitrothion. The method involved the addition of deep eutectic solvent to the aqueous sample followed by heating the mixture in a 75°C water bath until the solvent was completely dissolved in the aqueous phase. Then, the resultant solution was cooled in an ice bath and a cloudy solution was formed. Afterward, the mixture was centrifuged and the enriched deep eutectic solvent phase was analyzed by high-performance liquid chromatography with ultraviolet detection for quantification of the analytes. The factors affecting the extraction efficiency were optimized. Under the optimized extraction conditions, the limits of detection for diazinon and fenitrothion were 0.3 and 0.15 μg/L, respectively. The calibration curves for diazinon and fenitrothion exhibited linearity in the concentration range of 1-100 and 0.5-100 μg/L, respectively. The relative standard deviations for five replicate measurements at 10.0 μg/L level of analytes were less than 2.8 and 4.5% for intra- and interday assays, respectively. The developed method was successfully applied to the determination of diazinon and fenitrothion in water and fruit juice samples. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Facile and sensitive determination of N-nitrosamines in food samples by high-performance liquid chromatography via combining fluorescent labeling with dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Lu, Shuaimin; Wu, Di; Li, Guoliang; Lv, Zhengxian; Gong, Peiwei; Xia, Lian; Sun, Zhiwei; Chen, Guang; Chen, Xuefeng; You, Jinmao; Wu, Yongning

    2017-11-01

    The intake of N-nitrosamines (NAs) from foodstuffs is considered to be an important influence factor for several cancers. But the rapid and sensitive screening of NAs remains a challenge in the field of food safety. Inspired by that, a sensitive and rapid method was demonstrated for determination of five NAs (Nitrosopyrrolidine, Nitrosodimethylamine, Nitrosodiethylamine, Nitrosodipropylamine and Nitrosodibutylamine) using dispersive liquid-liquid microextraction (DLLME) followed by high-performance liquid chromatography with fluorescence detection (HPLC-FLD). The NAs were firstly denitrosated and labeled by 2-(11H-benzo[a]carbazol-11-yl) ethyl carbonochloridate (BCEC-Cl) and finally enriched by DLLME. Furthermore, the main DLLME conditions were optimized systematically. Under the optimal conditions, satisfactory limits of detection (LODs) were obtained with a range of 0.01-0.07ngg -1 , which were significantly lower than the reported methods. The developed method showed many merits including rapidity, simplicity, high sensitivity and excellent selectivity, which shows a broad prospect in food safety analysis. Copyright © 2017 Elsevier Ltd. All rights reserved.

  13. Dispersive Liquid-Liquid Microextraction Combined with Ultrahigh Performance Liquid Chromatography/Tandem Mass Spectrometry for Determination of Organophosphate Esters in Aqueous Samples

    Directory of Open Access Journals (Sweden)

    Haiying Luo

    2014-01-01

    Full Text Available A new technique was established to identify eight organophosphate esters (OPEs in this work. It utilised dispersive liquid-liquid microextraction in combination with ultrahigh performance liquid chromatography/tandem mass spectrometry. The type and volume of extraction solvents, dispersion agent, and amount of NaCl were optimized. The target analytes were detected in the range of 1.0–200 µg/L with correlation coefficients ranging from 0.9982 to 0.9998, and the detection limits of the analytes were ranged from 0.02 to 0.07 µg/L (S/N=3. The feasibility of this method was demonstrated by identifying OPEs in aqueous samples that exhibited spiked recoveries, which ranged between 48.7% and 58.3% for triethyl phosphate (TEP as well as between 85.9% and 113% for the other OPEs. The precision was ranged from 3.2% to 9.3% (n=6, and the interprecision was ranged from 2.6% to 12.3% (n=5. Only 2 of the 12 selected samples were tested to be positive for OPEs, and the total concentrations of OPEs in them were 1.1 and 1.6 µg/L, respectively. This method was confirmed to be simple, fast, and accurate for identifying OPEs in aqueous samples.

  14. Determination of Fusarium toxins in functional vegetable milks applying salting-out-assisted liquid-liquid extraction combined with ultra-high-performance liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Hamed, Ahmed M; Arroyo-Manzanares, Natalia; García-Campaña, Ana M; Gámiz-Gracia, Laura

    2017-11-01

    Vegetable milks are considered as functional foods due to their physiological benefits. Although the consumption of these products has significantly increased, they have received little attention in legislation with regard to contaminants. However, they may contain mycotoxins resulting from the use of contaminated raw materials. In this work, ultra-high-performance liquid chromatography tandem mass spectrometry has been proposed for the determination of the most relevant Fusarium toxins (fumonisin B 1 and B 2 , HT-2 and T-2 toxins, zearalenone, deoxynivalenol and fusarenon-X) in different functional beverages based on cereals, legumes and seeds. Sample treatment consisted of a simple salting-out-assisted liquid-liquid extraction with no further clean-up. The method provided limits of quantification between 3.2 and 57.7 µg L -1 , recoveries above 80% and precision with RSD lower than 12%. The method was also applied for studying the occurrence of these mycotoxins in market samples of vegetable functional beverages and deoxynivalenol was found in three oat-based commercial drinks.

  15. Fast, simple and efficient salting-out assisted liquid-liquid extraction of naringenin from fruit juice samples prior to their enantioselective determination by liquid chromatography.

    Science.gov (United States)

    Magiera, Sylwia; Kwietniowska, Ewelina

    2016-11-15

    In this study, an easy, simple and efficient method for the determination of naringenin enantiomers in fruit juices after salting-out-assisted liquid-liquid extraction (SALLE) and high-performance liquid chromatography (HPLC) with diode-array detection (DAD) was developed. The sample treatment is based on the use of water-miscible acetonitrile as the extractant and acetonitrile phase separation under high-salt conditions. After extraction, juice samples were incubated with hydrochloric acid in order to achieve hydrolysis of naringin to naringenin. The hydrolysis parameters were optimized by using a half-fraction factorial central composite design (CCD). After sample preparation, chromatographic separation was obtained on a Chiralcel® OJ-RH column using the mobile phase consisting of 10mM aqueous ammonium acetate:methanol:acetonitrile (50:30:20; v/v/v) with detection at 288nm. The average recovery of the analyzed compounds ranged from 85.6 to 97.1%. The proposed method was satisfactorily used for the determination of naringenin enantiomers in various fruit juices samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

  16. Detection of 10 sweeteners in various foods by liquid chromatography/tandem mass spectrometry

    Directory of Open Access Journals (Sweden)

    Chui-Shiang Chang

    2014-09-01

    Full Text Available The analytical method for sweeteners in various food matrixes is very important for food quality control and regulation enforcement. A simple and rapid method for the simultaneous determination of 10 sweeteners [acesulfame potassium (ACS-K, aspartame (ASP, cyclamate (CYC, dulcin (DUL, glycyrrhizic acid (GA, neotame (NEO, neohesperidin dihydrochalcone (NHDC, saccharin (SAC, sucralose (SCL, and stevioside (STV] in various foods by liquid chromatography/tandem mass chromatography (LC–MS/MS was developed. The chromatographic separation was performed on a Phenomenex Luna Phenyl-Hexyl (5 μm, 4.6 mm × 150 mm column with gradient elution of 10 mM ammonium acetate in water and 10 mM ammonium acetate in methanol. The recoveries of the 10 sweeteners were between 75% and 120%, and the coefficients of variation were less than 20%. The limits of quantification were 0.5 μg/kg for NHDC and SCL. For the other sweeteners, the limits of quantification were 0.1 μg/kg. Compared to the traditional high-performance liquid chromatography method, the LC–MS/MS method could provide better sensitivity, higher throughput, enhanced specificity, and more sweeteners analyzed in a single run. The samples included 27 beverages (16 alcoholic and 11 nonalcoholic beverages and 15 pickled foods (1 pickled pepper, 3 candies, and 11 candied fruits. Two remanufactured wines were found to contain 7.2, 8.5 μg/g SAC and 126.5, 123 μg/g CYC, respectively. ACS-K, ASP, SCL, and NEO were detected in five beverages and drinks. The pickled peppers and candied fruits were found to contain SAC, GA, CYC, ASP, STV, NEO, and ACS-K. The wine with sweeteners detected was remanufactured wine, not naturally fermented wine. Therefore, the ingredient label for the sweeteners of remanufactured wine should be regulated by the proper authority for inspection of sweeteners.

  17. Monitoring salivary melatonin concentrations in children with sleep disorders using liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Khan, Sohil A; George, Rani; Charles, Bruce G; Taylor, Paul J; Heussler, Helen S; Cooper, David M; McGuire, Treasure M; Pache, David; Norris, Ross L G

    2013-06-01

    Melatonin is synthesized in the pineal gland and is an important circadian phase marker, especially in the determination of sleep patterns. Both temporary and permanent abnormal sleep patterns occur in children; therefore, it is desirable to have methods for monitoring melatonin in biological fluids in the diagnosis and treatment of such disorders. The objective of the study is to develop a liquid chromatography-tandem mass spectrometry method for the determination of melatonin in saliva and to apply it to monitoring salivary concentrations in children with sleep disorders. A deuterated internal standard (d7-melatonin) was added to a diluted saliva sample (20 µL) in an autosampler vial insert, and 50 µL were injected. Plasticware was strictly avoided, and all glassware was scrupulously cleaned and then baked at 120°C for at least 48 hours to obtain satisfactory performance. Reverse-phase chromatography was performed on a C8 column using a linear gradient elution profile comprising mobile phases A (0.1% aqueous formic acid) and B (15% methanol in acetonitrile containing 0.1% formic acid), pumped at a total flow rate of 0.8 mL/min. The run time was 8 minutes. After atmospheric pressure chemical ionization, mass spectrometric detection was in positive ion mode. Mass detection was by selected reaction monitoring mode with the following mass transitions used for quantification: melatonin, m/z 233.0 → 173.8 and d7-melatonin, m/z 240.0 → 178.3. Linearity (r > 0.999) was established from 3.9 to 1000 pg/mL. Imprecision (coefficient of variation percent) was less than 11%, and accuracy was 100-105% (7.0-900 pg/mL). The method was selective, and the mean (range) ratio of the slopes of calibrations in water to those in daytime saliva samples collected from 10 healthy adult subjects was 0.989 (0.982-0.997), indicating negligible matrix effects. The application of the assay was demonstrated in healthy adults and in children being clinically investigated for sleep

  18. Monolithic columns based on a poly(styrene-divinylbenzene-methacrylic acid) copolymer for capillary liquid chromatography of small organic molecules

    Czech Academy of Sciences Publication Activity Database

    Svobodová, A.; Křížek, T.; Širc, Jakub; Šálek, Petr; Tesařová, E.; Coufal, P.; Štulík, K.

    2011-01-01

    Roč. 1218, č. 11 (2011), s. 1544-1547 ISSN 0021-9673 R&D Projects: GA AV ČR KAN200520804 Institutional research plan: CEZ:AV0Z40500505 Keywords : capillary liquid chromatography * methacrylic acid * polystyrene-based monolithic stationary phase Subject RIV: EI - Biotechnology ; Bionics Impact factor: 4.531, year: 2011

  19. Identification of very long chain fatty acids from sugar cane wax by atmospheric pressure chemical ionization liquid chromatography - mass spectroscopy

    Czech Academy of Sciences Publication Activity Database

    Řezanka, Tomáš; Sigler, Karel

    2006-01-01

    Roč. 67, - (2006), s. 916-923 ISSN 0031-9422 Institutional research plan: CEZ:AV0Z50200510 Keywords : sugar cane wax * very long chain fatty acids * liquid chromatography Subject RIV: EE - Microbiology, Virology Impact factor: 2.417, year: 2006

  20. Identification and quantification of cannabinoids in Cannabis sativa L. plants by high performance liquid chromatography-mass spectrometry

    NARCIS (Netherlands)

    Aizpurua-Olaizola, Oier; Omar, Jone; Navarro, Patricia; Olivares, Maitane; Etxebarria, Nestor; Usobiaga, Aresatz

    2014-01-01

    High performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) has been successfully applied to cannabis plant extracts in order to identify cannabinoid compounds after their quantitative isolation by means of supercritical fluid extraction (SFE). MS conditions were optimized by means

  1. Sensitive absorption detection for micro-column liquid chromatography by ultraviolet forward-scattering degenerate four-wave mixing.

    NARCIS (Netherlands)

    de Beer, T.; Beso, P.; Velthorst, N.H.; Brinkman, U.A.T.; Gooijer, C.; Hoornweg, G.Ph.

    1999-01-01

    The performance of forward-scattering degenerate four-wave mixing (F-D4WM) in the mid-ultraviolet (UV) region (351nm) as a detection technique for micro-column liquid chromatography (μLC) is studied, using nitro-substituted polycyclic aromatic hydrocarbons (NO

  2. Simultaneous Determination of Caffeine and Vitamin B6 in Energy Drinks by High-Performance Liquid Chromatography (HPLC)

    Science.gov (United States)

    Leacock, Rachel E.; Stankus, John J.; Davis, Julian M.

    2011-01-01

    A high-performance liquid chromatography experiment to determine the concentration of caffeine and vitamin B6 in sports energy drinks has been developed. This laboratory activity, which is appropriate for an upper-level instrumental analysis course, illustrates the standard addition method and simultaneous determination of two species. (Contains 1…

  3. Determination of phosphodiesterase type V inhibitors in wastewater by direct injection followed by liquid chromatography coupled to tandem mass spectrometry

    NARCIS (Netherlands)

    Causanilles, A.; Emke, E.; de Voogt, P.

    2016-01-01

    A simple, fast and reliable analytical method for the determination of phosphodiesterase type V inhibitors in wastewater was developed and validated. The method was based on direct injection followed by liquid chromatography coupled to tandem mass spectrometry with triple quadrupole as mass

  4. Development of small-volume, microfluidic chaotic mixers for future application in two-dimensional liquid chromatography

    NARCIS (Netherlands)

    Ianovska, Margaryta A.; Mulder, Patty P. M. F. A.; Verpoorte, Elisabeth

    2017-01-01

    We report a microfluidic chaotic micromixer with staggered herringbone grooves having a geometry optimized for fast mobile-phase modification at the interface of a two-dimensional liquid chromatography system. The volume of the 300 mm mixers is 1.6 microliters and they provide mixing within 26 s at

  5. Structural analysis of mycolic acids from phenol-degrading strain of Rhodococcus erythropolis by liquid chromatography-tandem mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Kolouchová, I.; Schreiberová, O.; Masák, J.; Sigler, Karel; Řezanka, Tomáš

    2012-01-01

    Roč. 57, č. 6 (2012), s. 473-483 ISSN 0015-5632 R&D Projects: GA ČR(CZ) GAP503/11/0215 Institutional support: RVO:61388971 Keywords : Rhodococcus erythropolis * mass spectrometry * liquid chromatography Subject RIV: EE - Microbiology, Virology Impact factor: 0.791, year: 2012

  6. Confirmation of synthetic glucocorticoids with liquid chromatography/mass spectrometry: Organization and results of an international interlaboratory comparison test

    NARCIS (Netherlands)

    Hauwe, O. van den; Campbell, K.; Crooks, S.R.H.; Schilt, R.; Peteghem, C.H. van

    2005-01-01

    Within the framework of a European Union (EU) research project entitled "Food Safety Screening: Synthetic Glucocorticoids (QLK1-1999-00122)," an international interlaboratory ring test was organized to compare and evaluate different liquid chromatography/mass spectrometry (LC/MS) confirmatory

  7. Chemically modified polymeric resins for separation of cations, organic acids, and small polar moleculea by high performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Morris, John B. [Iowa State Univ., Ames, IA (United States)

    1993-07-01

    This thesis is divided into 4 parts: a review, ion chromatography of metal cations on carboxylic resins, separation of hydrophilic organic acids and small polar compounds on macroporous resin columns, and use of eluent modifiers for liquid chromatographic separation of carboxylic acids using conductivity detection.

  8. Multi-podant diglycolamides and room temperature ionic liquid impregnated resins: an excellent combination for extraction chromatography of actinides

    NARCIS (Netherlands)

    Gujar, R.B.; Ansari, S.A.; Verboom, Willem; Mohapatra, P.K.

    2016-01-01

    Extraction chromatography resins, prepared by impregnating two multi-podant diglycolamide ligands, viz. diglycolamide-functionalized calix[4]arene (C4DGA) and tripodal diglycolamide (T-DGA) dissolved in the room temperature ionic liquid 1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)amide

  9. Determination of the brominated flame retardant, hexabroomcyclodocane in sediments and biota by liquid chromatography-electrospray ionization mass spectrometry

    NARCIS (Netherlands)

    Morris, S.; Bersuder, P.; Allchin, C.R.; Zegers, B.; Boon, J.P.; Leonards, P.E.G.; Boer, de J.

    2006-01-01

    A method involving reversed-phase, liquid chromatography coupled to electrospray ionisation mass spectrometry (LC-ESI-MS) was developed for separation, detection and quantitation of the alpha-, beta- and gamma-diastereoisomers of hexabromocyclododecane (HBCD). To address the lack of environmental

  10. Characterisation of Stevia Rebaudiana by comprehensive two-dimensional liquid chromatography time-of-flight mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Pól, Jaroslav; Hohnová, B.; Hyötyläinen, T.

    2007-01-01

    Roč. 1150, 1-2 (2007), s. 85-92 ISSN 0021-9673 R&D Projects: GA AV ČR KJB4031405 Institutional research plan: CEZ:AV0Z40310501 Keywords : comprehensive two-dimensional liquid chromatography * time-of-flight mass spectrometry * Stevia rebaudiana Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.641, year: 2007

  11. Quantification of antidepressants and antipsychotics in human serum by precipitation and ultra high pressure liquid chromatography-tandem mass spectrometry

    DEFF Research Database (Denmark)

    Hasselstrøm, Jørgen Bo

    2011-01-01

    precipitated with zinc sulphate and methanol containing a stable isotope labelled analog for each analyte. Quantitative analysis was performed by ultra high pressure liquid chromatography combined with a tandem mass spectrometer using a Zorbax SB-C8 column (2.0×50mm; 1.8m) with a mobile phase consisting of 0...

  12. Liquid chromatography coupled with tandem mass spectrometry for the quantitative analysis of anticancer drugs in biological matrices

    NARCIS (Netherlands)

    Stokvis, Ellen

    2004-01-01

    In this thesis, the development and validation of liquid chromatography tandem mass spectrometric (LC-MS/MS) methods for the quantitative bioanalysis of anticancer drugs are described. The monitoring of these drugs in biological fluids and tissues is important during both pre-clinical and clinical

  13. Determination of methyldibromoglutaronitrile in cosmetic products by high-performance liquid chromatography with electrochemical detection. Method validation

    DEFF Research Database (Denmark)

    Rastogi, Suresh Chandra; Zachariae, Claus; Johansen, Jeanne D

    2004-01-01

    An increased frequency of contact allergy to methyldibromoglutaronitrile (MDBGN), a commonly used preservative in cosmetics and other consumer products, has been reported in recent years. A high-performance liquid chromatography (HPLC) method for the determination of MDBGN in cosmetic products ha...

  14. Maximizing the peak production rate in off-line comprehensive two-dimensional liquid chromatography with mass spectrometry detection

    NARCIS (Netherlands)

    Eeltink, S.; Dolman, S.; Ursem, M.; Swart, R.; McLeod, F.; Schoenmakers, P.J.

    2009-01-01

    This article describes an optimization strategy to obtain the best possible performance in the shortest analysis time—called the peak production rate—for comprehensive off-line two-dimensional liquid chromatography. The demands on column technology (particle size and column length) and LC conditions

  15. Determination of olanzapine in whole blood using simple protein precipitation and liquid chromatography-tandem mass spectrometry

    DEFF Research Database (Denmark)

    Nielsen, Marie Katrine Klose; Johansen, Sys Stybe

    2009-01-01

    A simple, sensitive, and reproducible liquid chromatography-tandem mass spectrometry method has been developed and validated for the quantification of the antipsychotic drug olanzapine in whole blood using dibenzepine as internal standard (IS). After acidic methanol-induced protein precipitation...

  16. Simultaneous determination of estrogens and progestogens in honey using high performance liquid chromatography-tandem mass spectrometry

    Science.gov (United States)

    This work describes the development and validation of a method for the simultaneous determination of 13 estrogens and progestogens in honey by high performance liquid chromatography-tandem mass spectrometry. The target compounds were preconcentrated by solid phase extraction. Pretreatment variables ...

  17. Analysis of wax esters by silver-ion high-performance liquid chromatography-tandem mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Vrkoslav, Vladimír; Urbanová, Klára; Háková, Martina; Cvačka, Josef

    2013-01-01

    Roč. 1302, Aug 9 (2013), s. 105-110 ISSN 0021-9673 R&D Projects: GA ČR GA203/09/0139 Institutional support: RVO:61388963 Keywords : jojoba * human hair * wax esters * mass spectrometry * silver-ion liquid chromatography * long-chain esters Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.258, year: 2013

  18. Solving advanced micromachining problems for ultra-rapid and ultra-high resolution on-chip liquid chromatography

    NARCIS (Netherlands)

    de Malsche, Wim

    2008-01-01

    High-performance liquid chromatography (HPLC) is one of the most versatile separation techniques available for the analysis of complex samples that are typically encountered in fields such as environmental monitoring, biology, pharmacy, biochemistry, etc. A distinction between different HPLC formats

  19. Liquid chromatography-tandem mass spectrometric assay for the nucleoside reverse transcriptase inhibitor emtricitabine in human plasma

    NARCIS (Netherlands)

    Sparidans, Rolf W.; Prins, Jan M.; Schellens, Jan H. M.; Beijnen, Jos H.

    2007-01-01

    A liquid chromatography-tandem mass spectrometric assay for the determination of the antiretroviral nucleoside emtricitabine in human plasma was developed and validated using a simple sample pre-treatment procedure. After addition of 5'-deoxy-5-fluorocytidine as the internal standard and protein

  20. Determination of kava lactones in food supplements by liquid chromatography-atmospheric pressure chemical ionisation tandem mass spectrometry

    NARCIS (Netherlands)

    Bobeldijk, I.; Boonzaaijer, G.; Spies-Faber, E.J.; Vaes, W.H.J.

    2005-01-01

    Reversed-phase liquid chromatography and detection with atmospheric pressure chemical ionisation tandem mass spectrometry was used for the determination of kava extracts in herbal mixtures. One percent of kava extract can be detected, corresponding to approximately 0.05-0.2 mg/g of the individual

  1. Exploring Liquid Sequential Injection Chromatography to Teach Fundamentals of Separation Methods: A Very Fast Analytical Chemistry Experiment

    Science.gov (United States)

    Penteado, Jose C.; Masini, Jorge Cesar

    2011-01-01

    Influence of the solvent strength determined by the addition of a mobile-phase organic modifier and pH on chromatographic separation of sorbic acid and vanillin has been investigated by the relatively new technique, liquid sequential injection chromatography (SIC). This technique uses reversed-phase monolithic stationary phase to execute fast…

  2. Comparative urine analysis by liquid chromatography-mass spectrometry and multivariate statistics : Method development, evaluation, and application to proteinuria

    NARCIS (Netherlands)

    Kemperman, Ramses F. J.; Horvatovich, Peter L.; Hoekman, Berend; Reijmers, Theo H.; Muskiet, Frits A. J.; Bischoff, Rainer

    2007-01-01

    We describe a platform for the comparative profiling of urine using reversed-phase liquid chromatography-mass spectrometry (LC-MS) and multivariate statistical data analysis. Urinary compounds were separated by gradient elution and subsequently detected by electrospray Ion-Trap MS. The lower limit

  3. Identification and Quantification of the Major Constituents in Egyptian Carob Extract by Liquid Chromatography?Electrospray Ionization-Tandem Mass Spectrometry

    OpenAIRE

    Owis, Asmaa Ibrahim; El-Naggar, El-Motaz Bellah

    2016-01-01

    Background: Carob - Ceratonia siliqua L., commonly known as St John's-bread or locust bean, family Fabaceae - is one of the most useful native Mediterranean trees. There is no data about the chromatography methods performed by high performance liquid chromatography (HPLC) for determining polyphenols in Egyptian carob pods. Objective: To establish a sensitive and specific liquid chromatography?electrospray ionization (ESI)-tandem mass spectrometry (MSn) methodology for the identification of th...

  4. An optimized method for the measurement of acetaldehyde by high-performance liquid chromatography.

    Science.gov (United States)

    Guan, Xiangying; Rubin, Emanuel; Anni, Helen

    2012-03-01

    Acetaldehyde is produced during ethanol metabolism predominantly in the liver by alcohol dehydrogenase and rapidly eliminated by oxidation to acetate via aldehyde dehydrogenase. Assessment of circulating acetaldehyde levels in biological matrices is performed by headspace gas chromatography and reverse phase high-performance liquid chromatography (RP-HPLC). We have developed an optimized method for the measurement of acetaldehyde by RP-HPLC in hepatoma cell culture medium, blood, and plasma. After sample deproteinization, acetaldehyde was derivatized with 2,4-dinitrophenylhydrazine (DNPH). The reaction was optimized for pH, amount of derivatization reagent, time, and temperature. Extraction methods of the acetaldehyde-hydrazone (AcH-DNP) stable derivative and product stability studies were carried out. Acetaldehyde was identified by its retention time in comparison with AcH-DNP standard, using a new chromatography gradient program, and quantitated based on external reference standards and standard addition calibration curves in the presence and absence of ethanol. Derivatization of acetaldehyde was performed at pH 4.0 with an 80-fold molar excess of DNPH. The reaction was completed in 40 minutes at ambient temperature, and the product was stable for 2 days. A clear separation of AcH-DNP from DNPH was obtained with a new 11-minute chromatography program. Acetaldehyde detection was linear up to 80 μM. The recovery of acetaldehyde was >88% in culture media and >78% in plasma. We quantitatively determined the ethanol-derived acetaldehyde in hepatoma cells, rat blood and plasma with a detection limit around 3 μM. The accuracy of the method was volume (70 μl) plasma sampling. An optimized method for the quantitative determination of acetaldehyde in biological systems was developed using derivatization with DNPH, followed by a short RP-HPLC separation of AcH-DNP. The method has an extended linear range, is reproducible and applicable to small-volume sampling of culture

  5. Liquid chromatography automatic system with optical activity laser detector and its applications

    International Nuclear Information System (INIS)

    Fajer, V.; Naranjo, S.; Fernandez, H.; Mora, W.; Cepero, T.; Arista, E.; Mesa, G.; Cossio, G.; Arreche, J.; Fonfria, C.; Rodriguez, C.W.

    2009-01-01

    A new liquid chromatographic system with polarimetric detection and a computer program allowing the output of chromatograms to a display on line and electronic data storing was designed, built and put to work. The chromatographic system includes the laser polarimetric detector, having a measuring interval of one second, the chromatographic columns, the continuous flux polarimeter tubes of 50 and 100 mm, the programs for data acquisition, processing and storing, and the technical know-how for its most efficiently application. Thirty minutes is all the time needed to obtain a chromatogram by this method which is reasonably shorter than the time required for any other known comparable technique, and offering, besides, lower operation cost. The combination of molecular exclusion liquid chromatography and laser polarimetric detection has turned into a carbohydrate separation and quantification system of basic importance for the evaluation of plants fluids of industrial interest (sugarcane, agave, vegetable extracts, etc.). It is described here the application of this system as an early or complementary indicator of leaf scald -disease that affects sugarcane plants-. Another application on algae extracts gave good results in the separation and identification of biologically active components. The introduction of this system in several research centers in Cuba and abroad has resulted in practical information for the industry. (Author)

  6. Liquid chromatography under limiting conditions of desorption 6: separation of a four-component polymer blend.

    Science.gov (United States)

    Berek, Dušan; Macová, Eva

    2015-02-01

    Baseline separation was achieved of a model four-component polymer blend of polystyrene-poly(methyl methacrylate)-poly(ethylene oxide)-poly(2-vinyl pyridine) in a single chromatographic run with help of the unconventional method of liquid chromatography under limiting conditions of desorption. Narrow barriers of liquids were employed, which selectively decelerated elution of particular kinds of macromolecules. Bare silica gel was the column packing, and the eluent was a mixture of dimethylformamide/tetrahydrofuran/toluene 30:50:20 w/w/w. Barrier compositions were neat toluene, B#1, neat tetrahydrofuran, B#2, and dimethylformamide/tetrahydrofuran/toluene 15:55:30, B#3. Minor blend constituents (∼1%) could be identified, as well. The result represents a step toward the separation and molecular characterization of triblock-copolymers, many of which are expected to contain besides both parent homopolymers also the diblock chains and thus they are in fact four-component polymer blends. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Adaptation of a High-Pressure Liquid Chromatography System for the Measurement of Viscosity

    Directory of Open Access Journals (Sweden)

    Sonia Gregory

    2014-03-01

    Full Text Available The state-of-the-art instruments for the determination of viscosity of liquids typically require a significant amount of sample, and have relatively low throughput due to manual and sequential measurements. In this study, it was demonstrated that the pressure generated by the flow of viscous fluids through a capillary could be precisely measured employing high-pressure liquid chromatography systems (HPLC using glycerol solutions of moderate viscosity as a mobile phase, and correlated to the dynamic (absolute viscosity. The parameters allowing calculation of the viscosity of glycerol calibration standards as a function of temperature were established. The measurements were made with volumes as small as 10 μL, and the use of an autosampler permitted unattended analysis of a large number samples. The method appears to be particularly well suited for the development of viscous formulations of therapeutic, protein-based macromolecules, where the amount sample is typically limited and relatively wide ranges of conditions are considered in the optimization process. The utility of the methods was illustrated by application to the development of concentrated inactivated virus vaccines.

  8. Determination of melatonin and its isomer in foods by liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Kocadağlı, Tolgahan; Yılmaz, Cemile; Gökmen, Vural

    2014-06-15

    This study aimed to develop a reliable analytical method for the determination of melatonin and its isomers in various food products. The method entails ethanol extraction of solid samples (or dilution of liquid samples) prior to liquid chromatography coupled to triple quadruple mass spectrometry (LC-MS/MS) analysis of target analytes. The method was in-house validated and successfully applied to various food matrices. Recovery of melatonin from different matrices were found to be 86.0 ± 3.6%, 76.9 ± 5.4%, 98.6 ± 6.4%, and 67.0 ± 4.5% for beer, walnut, tomato and sour cherry samples, respectively. No melatonin could be detected in black and green tea, sour cherry, sour cherry concentrate, kefir (a fermented milk drink) and red wine while the highest amount of melatonin (341.7 ± 29.3 pg/g) was detected in crumb. The highest amounts of melatonin isomer were detected in yeast-fermented foods such as 170.7 ± 29.9 ng/ml in red wine, 14.3 ± 0.48 ng/ml in beer, and 15.7 ± 1.4 ng/g in bread crumb. Copyright © 2013 Elsevier Ltd. All rights reserved.

  9. Versatile lipid profiling by liquid chromatography–high resolution mass spectrometry using all ion fragmentation and polarity switching. Preliminary application for serum samples phenotyping related to canine mammary cancer

    Energy Technology Data Exchange (ETDEWEB)

    Gallart-Ayala, H., E-mail: laberca@oniris-nantes.fr [LUNAM, Ecole Nationale Vétérinaire, Agroalimentaire et de l’Alimentation Nantes Atlantique (Oniris), USC 1329 INRA Laboratoire d’Etude des résidus et Contaminants dans les Aliments (LABERCA), Site de la Chantrerie – CS50707, 44307 Nantes cedex 3 (France); Courant, F.; Severe, S.; Antignac, J.-P. [LUNAM, Ecole Nationale Vétérinaire, Agroalimentaire et de l’Alimentation Nantes Atlantique (Oniris), USC 1329 INRA Laboratoire d’Etude des résidus et Contaminants dans les Aliments (LABERCA), Site de la Chantrerie – CS50707, 44307 Nantes cedex 3 (France); Morio, F.; Abadie, J. [LUNAM, Ecole Nationale Vétérinaire, Agroalimentaire et de l’Alimentation Nantes Atlantique (Oniris), Cancers Animaux, Modèles pour la Recherche en Oncologie Comparée (AMaROC), Site de la Chantrerie–CS50707, 44307 Nantes cedex 3 (France); Le Bizec, B. [LUNAM, Ecole Nationale Vétérinaire, Agroalimentaire et de l’Alimentation Nantes Atlantique (Oniris), USC 1329 INRA Laboratoire d’Etude des résidus et Contaminants dans les Aliments (LABERCA), Site de la Chantrerie – CS50707, 44307 Nantes cedex 3 (France)

    2013-09-24

    Graphical abstract: -- Highlights: •Lipidomics, high resolution mass spectrometry, polarity switching, serum, canine mammary cancer. -- Abstract: Lipids represent an extended class of substances characterized by such high variety and complexity that makes their unified analyses by liquid chromatography coupled to either high resolution or tandem mass spectrometry (LC–HRMS or LC–MS/MS) a real challenge. In the present study, a new versatile methodology associating ultra high performance liquid chromatography coupled to high resolution tandem mass spectrometry (UHPLC–HRMS/MS) have been developed for a comprehensive analysis of lipids. The use of polarity switching and “all ion fragmentation” (AIF) have been two action levels particularly exploited to finally permit the detection and identification of a multi-class and multi-analyte extended range of lipids in a single run. For identification purposes, both higher energy collision dissociation (HCD) and in-source CID (collision induced dissociation) fragmentation were evaluated in order to obtain information about the precursor and product ions in the same spectra. This approach provides both class-specific and lipid-specific fragments, enhancing lipid identification. Finally, the developed method was applied for differential phenotyping of serum samples collected from pet dogs developing spontaneous malignant mammary tumors and health controls. A biological signature associated with the presence of cancer was then successfully revealed from this lipidome analysis, which required to be further investigated and confirmed at larger scale.

  10. On-line high speed lipid extraction for nanoflow liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Lee, Ju Yong; Yang, Joon Seon; Park, Se Mi; Byeon, Seul Kee; Moon, Myeong Hee

    2016-09-16

    An on-line lipid extraction method is introduced by utilizing a short capillary extraction column using HILIC and C4 particles prior to nanoflow liquid chromatography-tandem mass spectrometry (nLC-MS/MS). The on-line extraction using a urine sample spiked with PL standards showed similar or slightly higher recovery values (86%-96%) of phospholipids (PLs) compared to those obtained by the conventional off-line extraction based on the Folch method with or without using the air-exposed drying process. In this study, we demonstrated that PL oxidation can occur during the air-exposed drying process of lipid extracts in standard liquid-liquid extraction procedures, which was confirmed by the oxidized PL (OxPL) molecules that were generated from an off-line extraction using a few PL standards. Quantitative comparison of these OxPL species between on- and off-line extraction followed by nLC-MS/MS with multiple reaction monitoring (MRM) analysis showed a significant decrease (2-10 fold) in unwanted OxPL species when on-line extraction was employed. While the number of identified PLs from a urine sample was somewhat lower than those by off-line extraction, the number of OxPLs was significantly reduced (from 70 to 22) with on-line extraction. The new method offers high speed (∼5min) automated extraction of PLs with nLC-MS/MS analysis and presents the possibility of handling a biological sample with a very limited amount of lipids. Copyright © 2016 Elsevier B.V. All rights reserved.

  11. Validated method for determination of mazindol in human plasma by liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Kim, Sung-Su; Lee, Heon-Woo; Lee, Kyung-Tae

    2009-04-01

    A simple liquid chromatography/tandem mass spectrometry (LC/MS/MS) method with electrospray ionization in positive ion multiple reaction monitoring mode was developed for the quantification of mazindol (an anorectic agent) in human plasma. Fluoxetine was adopted as an internal standard (IS), and sample preparation involved one-step liquid/liquid extraction using ethyl acetate. The transition monitored were m/z 285>44 for mazindol and m/z 310>44 for IS. Chromatographic separation was achieved on a Capcell Pak MGII C(18) column using an isocratic mobile phase, consisting of acetonitrile-20mM ammonium formate in water (50:50, v/v, adjusted to pH 3.5 with formic acid) at a flow-rate of 0.2mL/min. The retention times of mazindol and fluoxetine were 1.03min and 1.45min, respectively. The lower limit of quantitation (LLOQ) was 0.1ng/mL using 200microL of plasma, and no interferences were detected in chromatograms. The bench top stability of mazindol was evaluated in buffered and non-buffered plasma. The selectivity, linearity, precision, accuracy, recovery, and stability of the devised method were fully validated and absolute and relative matrix effects were evaluated. The described method provides a fast and sensitive analytical tool for determining mazindol levels in plasma, and was successfully applied to a pharmacokinetic study in 24 healthy human subjects after oral administration of 2mg tablet formulation of mazindol under fasting conditions.

  12. Simulation of elution profiles in liquid chromatography - II: Investigation of injection volume overload under gradient elution conditions applied to second dimension separations in two-dimensional liquid chromatography.

    Science.gov (United States)

    Stoll, Dwight R; Sajulga, Ray W; Voigt, Bryan N; Larson, Eli J; Jeong, Lena N; Rutan, Sarah C

    2017-11-10

    An important research direction in the continued development of two-dimensional liquid chromatography (2D-LC) is to improve the detection sensitivity of the method. This is especially important in applications where injection of large volumes of effluent from the first dimension ( 1 D) column into the second dimension ( 2 D) column leads to severe 2 D peak broadening and peak shape distortion. For example, this is common when coupling two reversed-phase columns and the organic solvent content of the 1 D mobile phase overwhelms the 2 D column with each injection of 1 D effluent, leading to low resolution in the second dimension. In a previous study we validated a simulation approach based on the Craig distribution model and adapted from the work of Czok and Guiochon [1] that enabled accurate simulation of simple isocratic and gradient separations with very small injection volumes, and isocratic separations with mismatched injection and mobile phase solvents [2]. In the present study we have extended this simulation approach to simulate separations relevant to 2D-LC. Specifically, we have focused on simulating 2 D separations where gradient elution conditions are used, there is mismatch between the sample solvent and the starting point in the gradient elution program, injection volumes approach or even exceed the dead volume of the 2 D column, and the extent of sample loop filling is varied. To validate this simulation we have compared results from simulations and experiments for 101 different conditions, including variation in injection volume (0.4-80μL), loop filling level (25-100%), and degree of mismatch between sample organic solvent and the starting point in the gradient elution program (-20 to +20% ACN). We find that that the simulation is accurate enough (median errors in retention time and peak width of -1.0 and -4.9%, without corrections for extra-column dispersion) to be useful in guiding optimization of 2D-LC separations. However, this requires that real

  13. Toward unraveling grape tannin composition: application of online hydrophilic interaction chromatography × reversed-phase liquid chromatography-time-of-flight mass spectrometry for grape seed analysis.

    Science.gov (United States)

    Kalili, Kathithileni M; Vestner, Jochen; Stander, Maria A; de Villiers, André

    2013-10-01

    Despite the significant importance of tannins in viticulture and enology, relatively little is known about the detailed chemical composition of these molecules. This is due to challenges associated with the accurate analytical determination of the highly structurally diverse proanthocyanidins which comprise tannins. In this contribution, we address this limitation by demonstrating how online comprehensive two-dimensional liquid chromatography (LC × LC) coupled to high resolution mass spectrometry (HR-MS) can be exploited as a powerful analytical approach for the detailed characterization of grape seed tannins. Hydrophilic interaction chromatography (HILIC) and reversed-phase liquid chromatography (RP-LC) were employed in the two dimensions to provide complementary information in terms of separation according to hydrophilicity and hydrophobicity, respectively. Online coupling of HILIC × RP-LC with fluorescence detection and electrospray ionization MS delivered high resolution analysis in a practical analysis time, while allowing selective detection and facilitating compound identification. Time-of-flight (TOF) MS provided high acquisition rates and sensitivity coupled to accurate mass information, which allowed detection of procyanidins up to a degree of polymerization (DP) of 16 and a degree of galloylation up to 8 in a red grape seed extract. This analytical methodology promises to shed new light on these important grape constituents and potentially on their evolution during wine production.

  14. Detection of radiation-induced hydrocarbons in Camembert irradiated before and after the maturing process-comparison of florisil column chromatography and on-line coupled liquid chromatography-gas chromatography

    International Nuclear Information System (INIS)

    Schulzki, G.; Spiegelberg, A.; Bögl, K.W.; Schreiber, G.A.

    1995-01-01

    The influence of the maturing process on the detection of radiation-induced volatile hydrocarbons in the fat of Camembert has been investigated. Two analytical methods for separation of the hydrocarbon fraction from the lipid were applied: Florisil column chromatography with subsequent gas chromatographic-mass spectrometric (GC-MS) determination as well as on-line coupled liquid chromatography-GC-MS. The maturing process had no influence on the detection of radiation-induced volatiles. Comparable results were achieved with both analytical methods. However, preference is given to the more effective on-line coupled LC-GC method

  15. Dual reductive/oxidative electrochemistry/liquid chromatography/mass spectrometry: Towards peptide and protein modification, separation and identification.

    Science.gov (United States)

    Büter, Lars; Frensemeier, Lisa M; Vogel, Martin; Karst, Uwe

    2017-01-06

    A new hyphenated technique based on on-line dual (oxidative and reductive) electrochemistry coupled to liquid chromatography and high resolution electrospray mass spectrometry is presented. Two liquid streams are combined, with one containing a disulfide, which is reduced to the respective thiol in an electrochemical cell based on a titanium working electrode. The other stream contains phenol, which is electrochemically activated to benzoquinone on a boron-doped diamond working electrode. Upon combination of the two streams, a Michael addition takes places, leading to the covalent coupling of thiol to quinone. In continuous flow, the reaction mixture is transferred into an injection valve and the products are separated by reversed phase liquid chromatography and detected by electrospray-high resolution mass spectrometry. Proof of concept is demonstrated for low molecular mass disulfides and peptides, but further optimization will be required in future work to achieve efficient protein labelling. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Application and recovery of ionic liquids in the preparative separation of four flavonoids from Rhodiola rosea by on-line three-dimensional liquid chromatography.

    Science.gov (United States)

    Ma, Shufeng; Hu, Liming; Ma, Chaoyang; Lv, Wenping; Wang, Hongxin

    2014-09-01

    A novel on-line three-dimensional liquid chromatography method was developed to separate four main flavonoids from Rhodiola rosea. Ethyl acetate/0.5 mol/L ionic liquid 1-butyl-3-methylimidazolium chloride aqueous solution was selected as the solvent system. In the first-dimension separation, the target flavonoids were entrapped and subsequently desorbed into the second-dimension high-speed countercurrent chromatographic column for separation. In the third-dimension chromatography, the residual ionic liquid in the four separated flavonoids was removed and the used ionic liquid was recovered. As a result, 35.1 mg of compound 1, 20.4 mg of compound 2, 8.5 mg of compound 3, and 10.6 mg of compound 4 were obtained from 1.53 g R. rosea extract. They were identified as rhodiosin, rhodionin, herbacetin, and kaempferol, respectively. The recovery of ionic liquid reached 99.1% of the initial amount. The results showed that this method is a powerful technology for the separation of R. rosea flavonoids and that the ionic-liquid-based solvent system has advantages over traditional solvent systems in renewable and environmentally friendly properties. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Screening of Potential Xanthine Oxidase Inhibitors in Gnaphalium hypoleucum DC. by Immobilized Metal Affinity Chromatography and Ultrafiltration-Ultra Performance Liquid Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Hong-Jian Zhang

    2016-09-01

    Full Text Available In this study, a new method based on immobilized metal affinity chromatography (IMAC combined with ultrafiltration-ultra performance liquid chromatography-mass spectrometry (UF-UPLC-MS was developed for discovering ligands for xanthine oxidase (XO in Gnaphalium hypoleucum DC., a folk medicine used in China for the treatment of gout. By IMAC, the high flavonoid content of G. hypoleucum could be determined rapidly and efficiently. UF-UPLC-MS was used to select the bound xanthine oxidase ligands in the mixture and identify them. Finally, two flavonoids, luteolin-4′-O-glucoside and luteolin, were successfully screened and identified as the candidate XO inhibitors of G. hypoleucum. They were evaluated in vitro for XO inhibitory activity and their interaction mechanism was studied coupled with molecular simulations. The results were in favor of the hypothesis that the flavonoids of G. hypoleucum might be the active content for gout treatment by inhibiting XO.

  18. Screening of Potential Xanthine Oxidase Inhibitors in Gnaphalium hypoleucum DC. by Immobilized Metal Affinity Chromatography and Ultrafiltration-Ultra Performance Liquid Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Zhang, Hong-Jian; Hu, Yi-Juan; Xu, Pan; Liang, Wei-Qing; Zhou, Jie; Liu, Pei-Gang; Cheng, Lin; Pu, Jin-Bao

    2016-09-17

    In this study, a new method based on immobilized metal affinity chromatography (IMAC) combined with ultrafiltration-ultra performance liquid chromatography-mass spectrometry (UF-UPLC-MS) was developed for discovering ligands for xanthine oxidase (XO) in Gnaphalium hypoleucum DC., a folk medicine used in China for the treatment of gout. By IMAC, the high flavonoid content of G. hypoleucum could be determined rapidly and efficiently. UF-UPLC-MS was used to select the bound xanthine oxidase ligands in the mixture and identify them. Finally, two flavonoids, luteolin-4'-O-glucoside and luteolin, were successfully screened and identified as the candidate XO inhibitors of G. hypoleucum. They were evaluated in vitro for XO inhibitory activity and their interaction mechanism was studied coupled with molecular simulations. The results were in favor of the hypothesis that the flavonoids of G. hypoleucum might be the active content for gout treatment by inhibiting XO.

  19. Separation of three anthraquinone glycosides including two isomers by preparative high-performance liquid chromatography and high-speed countercurrent chromatography from Rheum tanguticum Maxim. ex Balf.

    Science.gov (United States)

    Chen, Tao; Li, Hongmei; Zou, Denglang; Liu, Yongling; Chen, Chen; Zhou, Guoying; Li, Yulin

    2016-08-01

    Anthraquinone glycosides, such as chrysophanol 1-O-β-d-glucoside, chrysophanol 8-O-β-d-glucoside, and physion 8-O-β-d-glucoside, are the accepted important active components of Rheum tanguticum Maxim. ex Balf. due to their pharmacological properties: antifungal, antimicrobial, cytotoxic, and antioxidant activities. However, an effective method for the separation of the above-mentioned anthraquinone glycosides from this herb is not currently available. Especially, greater difficulty existed in the separation of the two isomers chrysophanol 1-O-β-d-glucoside and chrysophanol 8-O-β-d-glucoside. This study demonstrated an efficient strategy based on preparative high-performance liquid chromatography and high-speed countercurrent chromatography for the separation of the above-mentioned anthraquinone glycosides from Rheum tanguticum Maxim.ex Balf. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Resistance switching of epitaxial VO2/Al2O3 heterostructure at room temperature induced by organic liquids

    Directory of Open Access Journals (Sweden)

    Mengmeng Yang

    2015-03-01

    Full Text Available We studied using organic liquids (cyclohexane, n-butanol, and ethylene glycol to modulate the transport properties at room temperature of an epitaxial VO2 film on a VO2/Al2O3 heterostructure. The resistance of the VO2 film increased when coated with cyclohexane or n-butanol, with maximum changes of 31% and 3.8%, respectively. In contrast, it decreased when coated with ethylene glycol, with a maximum change of −7.7%. In all cases, the resistance recovered to its original value after removing the organic liquid. This organic-liquid-induced reversible resistance switching suggests that VO2 films can be used as organic molecular sensors.

  1. Fast and comprehensive analysis of secondary metabolites in cocoa products using ultra high-performance liquid chromatography directly after pressurized liquid extraction.

    Science.gov (United States)

    Damm, Irina; Enger, Eileen; Chrubasik-Hausmann, Sigrun; Schieber, Andreas; Zimmermann, Benno F

    2016-08-01

    Fast methods for the extraction and analysis of various secondary metabolites from cocoa products were developed and optimized regarding speed and separation efficiency. Extraction by pressurized liquid extraction is automated and the extracts are analyzed by rapid reversed-phase ultra high-performance liquid chromatography and normal-phase high-performance liquid chromatography methods. After extraction, no further sample treatment is required before chromatographic analysis. The analytes comprise monomeric and oligomeric flavanols, flavonols, methylxanthins, N-phenylpropenoyl amino acids, and phenolic acids. Polyphenols and N-phenylpropenoyl amino acids are separated in a single run of 33 min, procyanidins are analyzed by normal-phase high-performance liquid chromatography within 16 min, and methylxanthins require only 6 min total run time. A fourth method is suitable for phenolic acids, but only protocatechuic acid was found in relevant quantities. The optimized methods were validated and applied to 27 dark chocolates, one milk chocolate, two cocoa powders and two food supplements based on cocoa extract. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Chiral ligand exchange high-speed countercurrent chromatography: mechanism, application and comparison with conventional liquid chromatography in enantioseparation of aromatic α-hydroxyl acids

    Science.gov (United States)

    Tong, Shengqiang; Shen, Mangmang; Cheng, Dongping; Ito, Yoichiro; Yan, Jizhong

    2014-01-01

    This work concentrates on the separation mechanism and application of chiral ligand exchange high-speed countercurrent chromatography (HSCCC) in enantioseparations, and comparison with traditional chiral ligand exchange high performance liquid chromatography (HPLC). The enantioseparation of ten aromatic α-hydroxyl acids were performed by these two chromatographic methods. Results showed that five of the racemates were successfully enantioseparated by HSCCC while only three of the racemates could be enantioseparated by HPLC using a suitable chiral ligand mobile phase additive. For HSCCC, the two-phase solvent system was composed of butanol-water (1:1, v/v), to which N-n-dodecyl-L-proline was added in the organic phase as chiral ligand and cupric acetate was added in the aqueous phase as a transition metal ion. Various operation parameters in HSCCC were optimized by enantioselective liquid-liquid extraction. Based on the results of the present studies the separation mechanism for HSCCC was proposed. For HPLC, the optimized mobile phase composed of aqueous solution containing 6 mmol L−1 L-phenylalanine and 3 mmol L−1 cupric sulfate and methanol was used for enantioseparation. Among three ligands tested on a conventional reverse stationary phase column, only one was found to be effective. In the present studies HSCCC presented unique advantages due to its high versatility of two-phase solvent systems and it could be used as an alternative method for enantioseparations. PMID:25087742

  3. Column properties and flow profiles of a flat, wide column for high-pressure liquid chromatography.

    Science.gov (United States)

    Mriziq, Khaled S; Guiochon, Georges

    2008-04-11

    The design and the construction of a pressurized, flat, wide column for high-performance liquid chromatography (HPLC) are described. This apparatus, which is derived from instruments that implement over-pressured thin layer chromatography, can carry out only uni-dimensional chromatographic separations. However, it is intended to be the first step in the development of more powerful instruments that will be able to carry out two-dimensional chromatographic separations, in which case, the first separation would be a space-based separation, LC(x), taking place along one side of the bed and the second separation would be a time-based separation, LC(t), as in classical HPLC but proceeding along the flat column, not along a tube. The apparatus described consists of a pressurization chamber made of a Plexiglas block and a column chamber made of stainless steel. These two chambers are separated by a thin Mylar membrane. The column chamber is a cavity which is filled with a thick layer (ca. 1mm) of the stationary phase. Suitable solvent inlet and outlet ports are located on two opposite sides of the sorbent layer. The design allows the preparation of a homogenous sorbent layer suitable to be used as a chromatographic column, the achievement of effective seals of the stationary phase layer against the chamber edges, and the homogenous flow of the mobile phase along the chamber. The entire width of the sorbent layer area can be used to develop separations or elute samples. The reproducible performance of the apparatus is demonstrated by the chromatographic separations of different dyes. This instrument is essentially designed for testing detector arrays to be used in a two-dimensional LC(x) x LC(t) instrument. The further development of two-dimension separation chromatographs based on the apparatus described is sketched.

  4. The analysis of carbohydrates in milk powder by a new "heart-cutting" two-dimensional liquid chromatography method.

    Science.gov (United States)

    Ma, Jing; Hou, Xiaofang; Zhang, Bing; Wang, Yunan; He, Langchong

    2014-03-01

    In this study, a new"heart-cutting" two-dimensional liquid chromatography method for the simultaneous determination of carbohydrate contents in milk powder was presented. In this two dimensional liquid chromatography system, a Venusil XBP-C4 analysis column was used in the first dimension ((1)D) as a pre-separation column, a ZORBAX carbohydrates analysis column was used in the second dimension ((2)D) as a final-analysis column. The whole process was completed in less than 35min without a particular sample preparation procedure. The capability of the new two dimensional HPLC method was demonstrated in the determination of carbohydrates in various brands of milk powder samples. A conventional one dimensional chromatography method was also proposed. The two proposed methods were both validated in terms of linearity, limits of detection, accuracy and precision. The comparison between the results obtained with the two methods showed that the new and completely automated two dimensional liquid chromatography method is more suitable for milk powder sample because of its online cleanup effect involved. Crown Copyright © 2013. Published by Elsevier B.V. All rights reserved.

  5. Reverse bistable effect in ferroelectric liquid crystal devices with ultra-fast switching at low driving voltage.

    Science.gov (United States)

    Guo, Qi; Zhao, Xiaojin; Zhao, Huijie; Chigrinov, V G

    2015-05-15

    In this Letter, reverse bistable effect with deep-sub-millisecond switching time is first reported in ferroelectric liquid crystal (FLC) devices using a homogeneous photo-alignment technique. It is indicated by our experimental results that both the anchoring energy and the dielectric property of the FLC's alignment layer is critical for the existence of the reverse bistable effect. In addition, with the derived criteria of the reverse bistable effect, we quantitatively analyze the switching dynamics of the reverse bistable FLC and the transition condition between the traditional bistability and our presented reverse bistability. Moreover, the fabricated FLC device exhibits an ultra-fast switching of ∼160  μs and a high contrast ratio of 1000:1, both of which were measured at a low driving voltage of 11 V. The featured deep-sub-millisecond switching time is really advantageous for our presented reverse bistable FLC devices, which enables a significant quality improvement of the existing optical devices, as well as a wide range of new applications in photonics and display areas.

  6. Automatic on-line solid-phase extraction with ultra-high performance liquid chromatography and tandem mass spectrometry for the determination of ten antipsychotics in human plasma.

    Science.gov (United States)

    Zhong, Qisheng; Shen, Lingling; Liu, Jiaqi; Yu, Dianbao; Li, Simin; Li, Zhiru; Yao, Jinting; Huang, Taohong; Kawano, Shin-Ichi; Hashi, Yuki; Zhou, Ting

    2016-06-01

    An automatic on-line solid-phase extraction with ultra-high performance liquid chromatography and tandem mass spectrometry method was developed for the simultaneous determination of ten antipsychotics in human plasma. The plasma sample after filtration was injected directly into the system without any pretreatment. A Shim-pack MAYI-C8 (G) column was used as a solid-phase extraction column, and all the analytes were separated on a Shim-pack XR-ODS III column with a mobile phase consisting of 0.1% v/v formic acid in water with 5 mM ammonium acetate and acetonitrile. The method features were systematically investigated, including extraction conditions, desorption conditions, the equilibration solution, the valve switching time, and the dilution for column-head stacking. Under the optimized conditions, the whole analysis procedure took only 10 min. The limits of quantitation were in the range of 0.00321-2.75 μg/L and the recoveries ranged from 75.9 to 122%. Compared with the off-line ultra-high performance liquid chromatography and the reported methods, this validated on-line method showed significant advantages such as minimal pretreatment, shortest analysis time, and highest sensitivity. The results indicated that this automatic on-line method was rapid, sensitive, and reliable for the determination of antipsychotics in plasma and could be extended to other target analytes in biological samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Method development for the quantitation of ABT-578 in rabbit artery tissue by 96-well liquid-liquid extraction and liquid chromatography/tandem mass spectrometric detection.

    Science.gov (United States)

    Ji, Qin C; Zhang, Jun; Rodila, Ramona; Watson, Pamela; El-Shourbagy, Tawakol

    2004-01-01

    Quantitative determination of drug concentrations in tissue samples can provide critical information for drug metabolism, kinetics, and toxicity evaluations. For analysis of tissue samples using liquid chromatography/tandem mass spectrometric (LC/MS/MS) detection, homogenization is a critical step in achieving good assay performance. Assay performance can be closely evaluated by spiking the drug directly into tissue samples prior to homogenization. It is especially important to include this assay evaluation for the analysis of artery tissue samples because artery tissue is very elastic, making it quite a challenge to develop an effective procedure for homogenization. An LC/MS/MS assay in 96-well format using liquid-liquid extraction was developed for analyzing ABT-578 in rabbit artery samples. Tissue quality control samples were prepared by spiking ABT-578 stock solutions directly into the tissue before homogenization. The usage of the tissue control samples gives a thorough evaluation of the sample preparation process that includes both homogenization and sample extraction. A 20% blood in saline solution was used as a homogenization solution. Calibration standards were made by spiking ABT-578 into rabbit whole blood. Blood quality control samples were also prepared by spiking ABT-578 into rabbit whole blood. These blood QC samples were used to confirm the validity of the calibration curve. A lower limit of quantitation of 0.050 ng/mL was achieved. The linear dynamic range of blood standards was from 0.050-30.3 ng/mL with the correlation coefficient (r) ranging from 0.9969-0.9996. Overall %CV was between 1.3 and 7.0%, and analytical recovery was between 98.2 and 105.8% for blood QC samples. The %CVs for tissue QC samples were between 6.7 and 13.0%, and analytical recovery after correction was between 93.5 and 114.3%. Copyright 2004 John Wiley & Sons, Ltd.

  8. Ultra-high performance liquid chromatography with fluorescence detection following salting-out assisted liquid-liquid extraction for the analysis of benzimidazole residues in farm fish samples.

    Science.gov (United States)

    Tejada-Casado, Carmen; Lara, Francisco J; García-Campaña, Ana M; Del Olmo-Iruela, Monsalud

    2018-03-30

    Ultra-high performance liquid chromatography (UHPLC) coupled with fluorescence detection (FL) has been proposed for the first time to determine thirteen benzimidazoles (BZs) in farmed fish samples. In order to optimize the chromatographic separation, parameters such as mobile phase composition and flow rate were carefully studied, establishing a gradient mode with a mobile phase consisted of water (solvent A) and acetonitrile (solvent B) at a flow rate of 0.4 mL/min. The separation was performed on a Zorbax Eclipse Plus RRHD C 18 column (50 × 2.1 mm, 1.8 μm), involving a total analysis time lower than 12 min. Salting-out assisted liquid-liquid extraction (SALLE) was applied as sample treatment to different types of farmed fish (trout, sea bream and sea bass). To obtain satisfactory extraction efficiencies for the studied analytes, several parameters affecting the SALLE procedure were optimized including the amount of sample, type and volume of the extraction solvent, and the nature and amount of the salt used. Characterization of the method in terms of performance characteristics was carried out, obtaining satisfactory results for the linearity (R 2  ≥ 0.997), repeatability (RSD ≤ 6.1%), reproducibility (RSD ≤ 10.8%) and recoveries (R ≥ 79%; RSD ≤ 7.8%). Detection limits between 0.04-29.9 μg kg -1 were obtained, demonstrating the applicability of this fast, simple and environmentally friendly method. Copyright © 2018 Elsevier B.V. All rights reserved.

  9. A new method for the determination of benzophenone-UV filters in human serum samples by dispersive liquid-liquid microextraction with liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Vela-Soria, F; Ballesteros, O; Zafra-Gómez, A; Ballesteros, L; Navalón, A

    2014-04-01

    Benzophenone-UV filters (BP-UV filters) are extensively used in cosmetics products to avoid damaging effects of UV radiation. Despite their low toxicity, many research papers indicate that BP-UV filters are weak endocrine disruptors (EDCs). There are clear relationships between BP-UV filters exposure and several health disorders such as carcinogenesis and malformations observed in animals. In the present work, a new sample treatment procedure by dispersive liquid-liquid microextraction (DLLME) is proposed for the extraction of six BPs, namely benzophenone-1 (BP-1), benzophenone-2 (BP-2), benzophenone-3 (BP-3), benzophenone-6 (BP-6), benzophenone-8 (BP-8) and 4-hydroxybenzophenone (4-OH-BP), in human serum samples, followed by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) analysis. The method involves an enzymatic treatment to quantify the total content (free plus conjugated species) of BP-UV filters in serum. The extraction parameters were accurately optimized using multivariate optimization approach. Benzophenone-d₁₀ (BP-d₁₀) was used as surrogate. Limits of quantification (LOQs) ranged from 0.4 to 0.9 ng mL(-1) and inter-day precision (evaluated as relative standard deviation) ranged from 1.9% to 13.1%. The method was validated using matrix-matched calibration and a recovery assay. Recovery rates for spiked samples ranged from 97% to 106%, and acceptable linearity was obtained up to concentrations of 40 ng mL(-1). The method was applied to the determination of the target compounds in human serum samples from 20 randomly selected anonymous individuals. Copyright © 2013 Elsevier B.V. All rights reserved.

  10. Simultaneous determination of pyrethroids and pyrethrins by dispersive liquid-liquid microextraction and liquid chromatography triple quadrupole mass spectrometry in environmental samples.

    Science.gov (United States)

    Ccanccapa-Cartagena, Alexander; Masiá, Ana; Picó, Yolanda

    2017-08-01

    A simple and environmentally friendly dispersive liquid-liquid microextraction (DLLME) method coupled with electrospray ionization liquid chromatography triple quadrupole mass spectrometry (LC-QqQ-MS/MS) was developed for the simultaneous determination of 17 synthetic and natural pyrethroids. A comparison of solid-phase extraction (SPE) versus DLLME for water samples and only "dilute and shoot" versus the additional extract cleanup by DLLME for sediment samples is reported. Chloroform was the extracting solvent in the DLLME technique for both water and sediment samples. Ultrasonic energy was applied to fully extract the analytes into fine droplets, providing high recoveries in short times. Method detection limits (MDLs) ranged from 0.12 to 0.62 ng L -1 and recoveries from 70 to 119% with RSD values 2-15% (n = 5) for water samples. In sediment samples, MDLs ranged from 0.50 to 2.50 ng g -1 and recoveries from 71 to 112% with RSDs 2-16% (n = 5). The proposed method showed a good linearity within the range of 10-500 ng mL -1 , with coefficients of determination (R 2 ) higher than 0.99. Matrix effects were observed for most compounds in water and sediment (ME% Albufera wetland and Turia River. Acrinathrin (48 ng g -1 ) and etofenprox (16 ng g -1 ) were detected in sediment samples. Graphical abstract Pyrethrins and pyrethroid determination in water and sediments by DLLME and LC-MS/MS.

  11. Determination of three natural pesticides in processed fruit and vegetables using high-performance liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Sannino, Anna

    2007-01-01

    This paper describes a method for the sensitive and selective determination of two macrocyclic lactones (abamectin and spinosad) and azadirachtin in apple purée, concentrated lemon juice, tomato purée and canned peas. The general sample extraction-partitioning method for our gas chromatography and liquid chromatography multiresidue methods has been used. The analytical procedure involves an extraction with acetone and liquid-liquid partitioning with ethyl acetate/cyclohexane combined in one step. The extracts are analyzed by liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) without any further clean-up step. The pesticides are separated on a reversed-phase C12 column using a gradient elution. Thirteen simultaneous MS/MS transitions of precursor ions were monitored. Studies at fortification levels of 2.5-10 microg/kg and 25-100 microg/kg gave mean recoveries ranging from 70-100% for all compounds with satisfactory precision (relative standard deviation (RSD) from 3-20%). The excellent selectivity and sensitivity allows quantification and identification of low levels of pesticides in canned peas, tomato and apple purées (limits of quantitation (LOQs) 1-5 microg/kg) and in concentrated lemon juice (LOQs 2-10 microg/kg). The quantification of analytes was carried out using the most sensitive transition for every compound and by 'matrix-matched' standards calibration. Copyright (c) 2007 John Wiley & Sons, Ltd.

  12. Urinary detection of conjugated and unconjugated anabolic steroids by dilute-and-shoot liquid chromatography-high resolution mass spectrometry.

    Science.gov (United States)

    Tudela, Eva; Deventer, Koen; Geldof, Lore; Van Eenoo, Peter

    2015-02-01

    Anabolic androgenic steroids (AAS) are an important class of doping agents. The metabolism of these substances is generally very extensive and includes phase-I and phase-II pathways. In this work, a comprehensive detection of these metabolites is described using a 2-fold dilution of urine and subsequent analysis by liquid chromatography-high resolution mass spectrometry (LC-HRMS). The method was applied to study 32 different metabolites, excreted free or conjugated (glucuronide or sulfate), which permit the detection of misuse of at least 21 anabolic steroids. The method has been fully validated for 21 target compounds (8 glucuronide, 1 sulfate and 12 free steroids) and 18 out of 21 compounds had detection limits in the range of 1-10 ng mL(-1) in urine. For the conjugated compounds, for which no reference standards are available, metabolites were synthesized in vitro or excretion studies were investigated. The detection limits for these compounds ranged between 0.5 and 18 ng mL(-1) in urine. The simple and straightforward methodology complements the traditional methods based on hydrolysis, liquid-liquid extraction, derivatization and analysis by gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-mass spectrometry (LC-MS). Copyright © 2014 John Wiley & Sons, Ltd.

  13. Profiling of drug binding proteins by monolithic affinity chromatography in combination with liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Zhang, Xuepei; Wang, Tongdan; Zhang, Hanzhi; Han, Bing; Wang, Lishun; Kang, Jingwu

    2014-09-12

    A new approach for proteome-wide profiling drug binding proteins by using monolithic capillary affinity chromatography in combination with HPLC-MS/MS is reported. Two immunosuppresive drugs, namely FK506 and cyclosporin A, were utilized as the experimental models for proof-of-concept. The monolithic capillary affinity columns were prepared through a single-step copolymerization of the drug derivatives with glycidyl methacrylate and ethylene dimethacrylate. The capillary chromatography with the affinity monolithic column facilitates the purification of the drug binding proteins from the cell lysate. By combining the capillary affinity column purification and the shot-gun proteomic analysis, totally 33 FK506- and 32 CsA-binding proteins including all the literature reported target proteins of these two drugs were identified. Among them, two proteins, namely voltage-dependent anion-selective channel protein 1 and serine/threonine-protein phosphatase PGAM5 were verified by using the recombinant proteins. The result supports that the monolithic capillary affinity chromatography is likely to become a valuable tool for profiling of binding proteins of small molecular drugs as well as bioactive compounds. Copyright © 2014 Elsevier B.V. All rights reserved.

  14. High efficiency polyethylene glycol diacrylate monoliths for reversed-phase capillary liquid chromatography of small molecules.

    Science.gov (United States)

    Aggarwal, Pankaj; Lawson, John S; Tolley, H Dennis; Lee, Milton L

    2014-10-17

    Highly cross-linked monolithic networks (i.e., polyethylene glycol diacrylate, PEGDA) synthesized from monomers containing varying ethylene oxide chain lengths were fabricated inside fused silica capillary columns for use in liquid chromatography (LC) of small molecules. Tergitol was used as a surfactant porogen in combination with other typical organic liquid porogens. Column performance was correlated with quantitative descriptors of the physical/chemical properties of the monomers and porogens using a statistical model. Solubility and viscosity values of the components were identified as important predictors of monolith morphology and efficiency. The chromatographic retention mechanism was determined to be principally reversed-phase (RP) with additional hydrogen bonding between the polar groups of the analytes and the ethylene oxide groups embedded in the monolith structure. The fabricated monolithic columns were evaluated under RPLC conditions using phenols, hydroxy benzoic acids, and alkyl parabens as test compounds. Isocratic elution of hydroxy benzoic acids at a linear velocity of 0.04 cm/s using a PEGDA-700 monolith gave chromatographic peaks with little tailing (i.e., tailing factorcolumn was 186,000 plates/m when corrected for injector dead volume. High resolution gradient separations of selected pharmaceutical compounds and phenylurea herbicides were achieved in less than 18 min. Optimized monoliths synthesized from all four crosslinking monomers exhibited high permeability and demonstrated little swelling or shrinking in different polarity solvents. Column preparation was highly reproducible, with relative standard deviation (RSD) values less than 2.1%, based on retention times of the phenol standards (3 different columns). Copyright © 2014 Elsevier B.V. All rights reserved.

  15. Evaluation of aminoacids in irradiated beans (Vigna unguiculata (L.) Walp) by high performance liquid chromatography (HPLC)

    Energy Technology Data Exchange (ETDEWEB)

    Lima, Keila S. Cople; Souza, Luciana B.; Coelho, Maysa J.; Lima, Antonio L. Santos; Hernandes, Nilber K. [Instituto Militar de Engenharia (IME), Rio de Janeiro, RJ (Brazil). Secao de Engenharia Nuclear]. E-mail: keila@ime.eb.br; Godoy, Ronoel L.O. [EMBRAPA Agroindustria de Alimentos, Rio de Janeiro, RJ (Brazil)]. E-mail: ronoel@ctaa.embrapa.br

    2007-07-01

    Fradinho-bean (Vigna unguiculata (L.) Walp) is originated from Africa and is known in Brazil as 'caupi', 'corda' or 'macassar'. It is grown in the interior of Northeast Brazil (semi-arid region) and can be found in parts of the North, being one of the most important components of people's diet in those regions. The Northeast area produces around 429,375 ton of fradinho-bean per year. Leguminous plants are very important sources of proteins, vitamins, carbohydrates and minerals. This kind of bean is an excellent source of proteins (around 23- 25% of its nutritional content), being superior to regular beans (Phaseolus vulgaris). The irradiation process is an alternative to avoid post-harvesting losses, without changing the nutritional value of food. This study has the objective to evaluate the effect of different gamma irradiation doses (0.0; 0.5; 1.0; 2.5; 5.0 and 10.0 kGy) on aminoacid content of fradinho-bean by high performance liquid chromatography (HPLC) and the accompanying of the grains during storage time of 6 months. After irradiation, the bean grains went through a milling process in order to make flour for posterior extraction. A liquid chromatographer Waters, model Alliance 2695, with fluorescent detector Waters 2475, having a mobile phase with gradient elution of sodium acetate. acetonitrile and Milli-Q water, was employed. The flux used was 1 mL/min and the injection volume of 10 {mu}L. The column (C 18 150.0 x 3.9 mm) was kept at 36 deg C. The results show that gamma irradiation is a promise process for fradinho bean during conservation storage time of 6 months, until the dose of 10.0 kGy. Even the most radio-sensitive aminoacids like aromatics and basic lateral chains were preserved. (author)

  16. Evaluation of aminoacids in irradiated beans (Vigna unguiculata (L.) Walp) by high performance liquid chromatography (HPLC)

    International Nuclear Information System (INIS)

    Lima, Keila S. Cople; Souza, Luciana B.; Coelho, Maysa J.; Lima, Antonio L. Santos; Hernandes, Nilber K.

    2007-01-01

    Fradinho-bean (Vigna unguiculata (L.) Walp) is originated from Africa and is known in Brazil as 'caupi', 'corda' or 'macassar'. It is grown in the interior of Northeast Brazil (semi-arid region) and can be found in parts of the North, being one of the most important components of people's diet in those regions. The Northeast area produces around 429,375 ton of fradinho-bean per year. Leguminous plants are very important sources of proteins, vitamins, carbohydrates and minerals. This kind of bean is an excellent source of proteins (around 23- 25% of its nutritional content), being superior to regular beans (Phaseolus vulgaris). The irradiation process is an alternative to avoid post-harvesting losses, without changing the nutritional value of food. This study has the objective to evaluate the effect of different gamma irradiation doses (0.0; 0.5; 1.0; 2.5; 5.0 and 10.0 kGy) on aminoacid content of fradinho-bean by high performance liquid chromatography (HPLC) and the accompanying of the grains during storage time of 6 months. After irradiation, the bean grains went through a milling process in order to make flour for posterior extraction. A liquid chromatographer Waters, model Alliance 2695, with fluorescent detector Waters 2475, having a mobile phase with gradient elution of sodium acetate. acetonitrile and Milli-Q water, was employed. The flux used was 1 mL/min and the injection volume of 10 μL. The column (C 18 150.0 x 3.9 mm) was kept at 36 deg C. The results show that gamma irradiation is a promise process for fradinho bean during conservation storage time of 6 months, until the dose of 10.0 kGy. Even the most radio-sensitive aminoacids like aromatics and basic lateral chains were preserved. (author)

  17. Reversed-phase liquid chromatography coupled on-line with capillary gas chromatography use of an anion-exchange membrane to remove an ion-pair reagent from the eluent.

    NARCIS (Netherlands)

    Brinkman, U.A.T.; Goosens, E.C.; de Jong, D.; de Jong, G.J.; Beerthuizen, I.M.

    1995-01-01

    In order to enable the coupling of reversed-phase liquid chromatography (RPLC) with capillary gas chromatography (GC), the performance of an anion-exchange micromembrane device has been studied to remove the ion-pair reagent methanesulphonic acid from an acetonitrile/water LC eluent. The regenerant

  18. The high pressure liquid chromatography and its application to the separation of polynuclear aromatic hydrocarbons in atmospheric dust and burning residues

    International Nuclear Information System (INIS)

    Lopez, M.-C.

    1975-09-01

    A new technique of analysis is described: the high speed liquid chromatography or more exactly the high performance liquid chromatography because of the progress achieved on the new packings of the columns. The main types of chromatography, according to the phenomena involved are described: adsorption, partition, ion-exchange and exclusion chromatography. A brief outline is given of the theory for determination of stationary and mobile phases in order to obtain the optimum conditions of separation. Some exemples of possible applications are given, particularly the use of this technique for the separation of polycyclic aromatic hydrocarbons in atmospheric pollution and burning residues [fr

  19. Analysis of the Constituents in “Zhu She Yong Xue Shuan Tong” by Ultra High Performance Liquid Chromatography with Quadrupole Time-of-Flight Mass Spectrometry Combined with Preparative High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Lin-Lin Wang

    2015-11-01

    Full Text Available “Zhu She Yong Xue Shuan Tong” lyophilized powder (ZSYXST, consists of a series of saponins extracted from Panax notoginseng, which has been widely used in China for the treatment of strokes. In this study, an ultra-high performance liquid chromatography with quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF/MS combined with preparative high performance liquid chromatography (PHPLC method was developed to rapidly identify both major and minor saponins in ZSYXST. Some high content components were removed through PHPLC in order to increase the sensitivity of the trace saponins. Then, specific characteristic fragment ions in both positive and negative mode were utilized to determine the types of aglycone, saccharide, as well as the saccharide chain linkages. As a result, 94 saponins, including 20 pairs of isomers and ten new compounds, which could represent higher than 98% components in ZSYXST, were identified or tentatively identified in commercial ZSYXST samples.

  20. Phytochemical and morphological characterization of hop (Humulus lupulus L.) cones over five developmental stages using high performance liquid chromatography coupled to time-of-flight mass spectrometry, ultrahigh performance liquid chromatography photodiode array detection, and light microscopy techniques.

    Science.gov (United States)

    Kavalier, Adam R; Litt, Amy; Ma, Chunhui; Pitra, Nicholi J; Coles, Mark C; Kennelly, Edward J; Matthews, Paul D

    2011-05-11

    Hop (Humulus lupulus L.) inflorescences, commonly known as "hop cones", are prized for their terpenophenolic contents, used in beer production and, more recently, in biomedical applications. In this study we investigated morphological and phytochemical characteristics of hop cones over five developmental stages, using liquid chromatography coupled to time-of-flight mass spectrometry (LC-TOF-MS), and ultrahigh performance liquid chromatography photodiode array detection (UHPLC-PDA) methods to quantitate 21 polyphenolics and seven terpenophenolics. Additionally, we used light microscopy to correlate phytochemical quantities with changes in the morphology of the cones. Significant increases in terpenophenolics, concomitant with glandular trichome development and associated gross morphological changes, were mapped over development to fluctuations in contents of polyphenolic constituents and their metabolic precursor compounds. The methods reported here can be used for targeted metabolic profiling of flavonoids, phenolic acids, and terpenophenolics in hops, and are applicable to quantitation in other crops.

  1. Diversity of the Lactic Acid Bacterium and Yeast Microbiota in the Switch from Firm- to Liquid-Sourdough Fermentation

    Science.gov (United States)

    Di Cagno, Raffaella; Pontonio, Erica; Buchin, Solange; De Angelis, Maria; Lattanzi, Anna; Valerio, Francesca; Calasso, Maria

    2014-01-01

    Four traditional type I sourdoughs were comparatively propagated (28 days) under firm (dough yield, 160) and liquid (dough yield, 280) conditions to mimic the alternative technology options frequently used for making baked goods. After 28 days of propagation, liquid sourdoughs had the lowest pH and total titratable acidity (TTA), the lowest concentrations of lactic and acetic acids and free amino acids, and the most stable density of presumptive lactic acid bacteria. The cell density of yeasts was the highest in liquid sourdoughs. Liquid sourdoughs showed simplified microbial diversity and harbored a low number of strains, which were persistent. Lactobacillus plantarum dominated firm sourdoughs over time. Leuconostoc lactis and Lactobacillus brevis dominated only some firm sourdoughs, and Lactobacillus sanfranciscensis persisted for some time only in some firm sourdoughs. Leuconostoc citreum persisted in all firm and liquid sourdoughs, and it was the only species detected in liquid sourdoughs at all times; it was flanked by Leuconostoc mesenteroides in some sourdoughs. Saccharomyces cerevisiae, Candida humilis, Saccharomyces servazzii, Saccharomyces bayanus-Kazachstania sp., and Torulaspora delbrueckii were variously identified in firm and liquid sourdoughs. A total of 197 volatile components were identified through purge and trap–/solid-phase microextraction–gas chromatography-mass spectrometry (PT–/SPME–GC-MS). Aldehydes, several alcohols, and some esters were at the highest levels in liquid sourdoughs. Firm sourdoughs mainly contained ethyl acetate, acetic acid, some sulfur compounds, and terpenes. The use of liquid fermentation would change the main microbial and biochemical features of traditional baked goods, which have been manufactured under firm conditions for a long time. PMID:24632249

  2. Accelerated solvent extraction combined with dispersive liquid-liquid microextraction before gas chromatography with mass spectrometry for the sensitive determination of phenols in soil samples.

    Science.gov (United States)

    Xing, Han-Zhu; Wang, Xia; Chen, Xiang-Feng; Wang, Ming-Lin; Zhao, Ru-Song

    2015-05-01

    A method combining accelerated solvent extraction with dispersive liquid-liquid microextraction was developed for the first time as a sample pretreatment for the rapid analysis of phenols (including phenol, m-cresol, 2,4-dichlorophenol, and 2,4,6-trichlorophenol) in soil samples. In the accelerated solvent extraction procedure, water was used as an extraction solvent, and phenols were extracted from soil samples into water. The dispersive liquid-liquid microextraction technique was then performed on the obtained aqueous solution. Important accelerated solvent extraction and dispersive liquid-liquid microextraction parameters were investigated and optimized. Under optimized conditions, the new method provided wide linearity (6.1-3080 ng/g), low limits of detection (0.06-1.83 ng/g), and excellent reproducibility (extraction with dispersive liquid-liquid microextraction as a sample pretreatment procedure coupled with gas chromatography and mass spectrometry is an excellent method for the rapid analysis of trace levels of phenols in environmental soil samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Flexoelectric effect in an in-plane switching (IPS) liquid crystal cell for low-power consumption display devices

    Science.gov (United States)

    Kim, Min Su; Bos, Philip J.; Kim, Dong-Woo; Yang, Deng-Ke; Lee, Joong Hee; Lee, Seung Hee

    2016-01-01

    Technology of displaying static images in portable displays, advertising panels and price tags pursues significant reduction in power consumption and in product cost. Driving at a low-frequency electric field in fringe-field switching (FFS) mode can be one of the efficient ways to save powers of the recent portable devices, but a serious drop of image-quality, so-called image-flickering, has been found in terms of the coupling of elastic deformation to not only quadratic dielectric effect but linear flexoelectric effect. Despite of the urgent requirement of solving the issue, understanding of such a phenomenon is yet vague. Here, we thoroughly analyze and firstly report the flexoelectric effect in in-plane switching (IPS) liquid crystal cell. The effect takes place on the area above electrodes due to splay and bend deformations of nematic liquid crystal along oblique electric fields, so that the obvious spatial shift of the optical transmittance is experimentally observed and is clearly demonstrated based on the relation between direction of flexoelectric polarization and electric field polarity. In addition, we report that the IPS mode has inherent characteristics to solve the image-flickering issue in the low-power consumption display in terms of the physical property of liquid crystal material and the electrode structure. PMID:27731372

  4. Determination of chlorobenzenes in textiles by pressurized hot water extraction followed by vortex-assisted liquid-liquid microextraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Lu, Yang; Zhu, Yan

    2013-12-06

    A method for quantitative determination of chlorobenzenes in textiles is developed, using pressurized hot water extraction (PHWE), vortex-assisted liquid-liquid microextraction (VALLME) and gas chromatography-mass spectrometry (GC-MS). VALLME serves as a trapping step after PHWE. The extraction conditions are investigated, as well as the quantitative features such as linearity, limits of detection (LODs), limits of quantification (LOQs), repeatabilities and reproducibilities between days. LOQs of 0.018-0.032mg/kg were achieved. The present method provides good repeatabilities (RSDtextiles. Copyright © 2013 Elsevier B.V. All rights reserved.

  5. Amphenicols stability in medicated feed – development and validation of liquid chromatography method

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    Pietro Wojciech Jerzy

    2014-12-01

    Full Text Available A liquid chromatography-ultraviolet detection method for the determination of florfenicol (FF and thiamphenicol (TAP in feeds is presented. The method comprises the extraction of analytes from the matrix with a mixture of methanol and acetonitrile, drying of the extract, and its dissolution in phosphate buffer. The analysis was performed with a gradient programme of the mobile phase composed of acetonitrile and buffer (pH = 7.3 on a Zorbax Eclipse Plus C18 (150 × 4.6 mm, 5 μm analytical column with UV (λ = 220 nm detection. The analytical procedure has been successfully adopted and validated for quantitative determination of florfenicol and thiamphenicol in feed samples. Sensitivity, specificity, linearity, repeatability, and intralaboratory reproducibility were included in the validation. The mean recovery of amphenicols was 93.5% within the working range of 50-4000 mg/kg. Simultaneous determination of chloramphenicol, which is banned in the feed, was also included within the same procedure of FF and TAP stability studies. Storing the medicated feed at room temperature for up to one month decreased concentration in the investigated drugs even by 45%. These findings are relevant to successful provision of therapy to animals.

  6. Determination of ractopamine in pig hair using liquid chromatography with tandem mass spectrometric detection.

    Science.gov (United States)

    Wu, Junlin; Liu, Xiaoyun; Peng, Yunping

    2014-01-01

    A quantitative analytical procedure for the determination of ractopamine in pig hair has been developed and validated. The hair samples were washed and incubated at 75°C with isoxuprine and hair extraction buffer. The drug present was quantified using mixed solid-phase extraction and liquid chromatography with tandem mass spectrometric detection. The limit of quantization (LOQ) was 10pg/mg and the intra-day precision at 25pg/mg and 750pg/mg was 0.49% and 2.8% respectively. Inter-day precision was 0.88% and 3.52% at the same concentrations. The hair extraction percentage recovery at 25pg/mg and 50ng/mL was 99.47% and 103.83% respectively. The extraction percentage recovery at 25pg/mg and 50ng/mg was 93.52% and 100.26% respectively. Our results showed that ractopamine residues persist in hair in 24days of withdrawal and also showed the possibility to test ractopamine from pig hair samples. Copyright © 2014 Elsevier Inc. All rights reserved.

  7. COMPARISON OF CAROTENOID CONTENT IN TOMATO, TOMATO PULP AND KETCHUP BY LIQUID CHROMATOGRAPHY

    Directory of Open Access Journals (Sweden)

    J. J. T. GAMA

    2009-01-01

    Full Text Available

    Although tomatoes are commonly consumed fresh, over 80 % the consumption of tomatoes is in the form of processed products such as tomato pulp, ketchup, juice and sauce. Research has indicated the potential health benefits of a diet rich in tomatoes and tomato products. The present study was carried out to determine the carotenoid content of fresh tomato, tomato pulp and ketchup by high performance liquid chromatography. The major differences among these products were in the concentration of some of the pigments. Tomato had all-trans-lycopene (1046-1099 μg/g DW, cislycopene (125-132 μg/g DW and all-trans- -carotene (45-59 μg/g DW as principal carotenoids. Tomato pulp and ketchup had all-trans-lycopene (951-999 μg/g DW and 455-476 μg/g DW, all-trans- -carotene (76-88 DW μg/g and 20-27 DW μg/g and cis-lycopene (71-83 μg/g DW and 14-25 μg/g DW as the main pigments, respectively. They also contained other carotenoids in much smaller amounts (lycoxanthin, zeaxanthin, anteraxanthin, lutein, -carotene, -carotene and phytofluene.

  8. Analysis of serotonin concentrations in human milk by high-performance liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Chiba, Takeshi; Maeda, Tomoji; Tairabune, Tomohiko; Tomita, Takashi; Sanbe, Atsushi; Takeda, Rika; Kikuchi, Akihiko; Kudo, Kenzo

    2017-03-25

    Serotonin (5-hydroxytryptamine, 5-HT) plays an important role in milk volume homeostasis in the mammary gland during lactation; 5-HT in milk may also affect infant development. However, there are few reports on 5-HT concentrations in human breast milk. To address this issue, we developed a simple method based on high-performance liquid chromatography with fluorescence detection (HPLC-FD) for measuring 5-HT concentrations in human breast milk. Breast milk samples were provided by four healthy Japanese women. Calibration curves for 5-HT in each sample were prepared with the standard addition method between 5 and 1000 ng/ml, and all had correlation coefficients >0.999. The recovery of 5-HT was 96.1%-101.0%, with a coefficient of variation of 3.39%-8.62%. The range of 5-HT concentrations estimated from the calibration curves was 11.1-51.1 ng/ml. Thus, the HPLC-FD method described here can effectively extract 5-HT from human breast milk with high reproducibility. Copyright © 2017 Elsevier Inc. All rights reserved.

  9. HDL proteome in hemodialysis patients: a quantitative nanoflow liquid chromatography-tandem mass spectrometry approach.

    Directory of Open Access Journals (Sweden)

    Alain Mangé

    Full Text Available Aside from a decrease in the high-density lipoprotein (HDL cholesterol levels, qualitative abnormalities of HDL can contribute to an increase in cardiovascular (CV risk in end-stage renal disease (ESRD patients undergoing chronic hemodialysis (HD. Dysfunctional HDL leads to an alteration of reverse cholesterol transport and the antioxidant and anti-inflammatory properties of HDL. In this study, a quantitative proteomics approach, based on iTRAQ labeling and nanoflow liquid chromatography mass spectrometry analysis, was used to generate detailed data on HDL-associated proteins. The HDL composition was compared between seven chronic HD patients and a pool of seven healthy controls. To confirm the proteomics results, specific biochemical assays were then performed in triplicate in the 14 samples as well as 46 sex-matched independent chronic HD patients and healthy volunteers. Of the 122 proteins identified in the HDL fraction, 40 were differentially expressed between the healthy volunteers and the HD patients. These proteins are involved in many HDL functions, including lipid metabolism, the acute inflammatory response, complement activation, the regulation of lipoprotein oxidation, and metal cation homeostasis. Among the identified proteins, apolipoprotein C-II and apolipoprotein C-III were significantly increased in the HDL fraction of HD patients whereas serotransferrin was decreased. In this study, we identified new markers of potential relevance to the pathways linked to HDL dysfunction in HD. Proteomic analysis of the HDL fraction provides an efficient method to identify new and uncharacterized candidate biomarkers of CV risk in HD patients.

  10. Comprehensive measurement of total nondigestible carbohydrates in foods by enzymatic-gravimetric method and liquid chromatography.

    Science.gov (United States)

    Nishibata, Toyohide; Tashiro, Kouichi; Kanahori, Sumiko; Hashizume, Chieko; Kitagawa, Machiko; Okuma, Kazuhiro; Gordon, Dennis T

    2009-09-09

    Total nondigestible carbohydrate (NDC) in foods was determined by combining, not modifications, AOAC Official Methods 991.43, 2001.03, and 2002.02. Total NDC included insoluble dietary fiber (IDF) + high-molecular-weight soluble dietary fiber (HMWSDF), nondigestible oligosaccharides (NDO) not precipitated in ethanol solution, and resistant starch (RS). Eight sources of NDC (cellulose, wheat bran, gum arabic, resistant maltodextrin, polydextrose, fructooligosaccharide, galactooligosaccharides, and RS) were incorporated in different combinations into standard formula bread samples. All of the NDC sources and bread samples were analyzed for their (1) IDF + HMWSDF content with corrections for residual RS amount using AOAC Official Method 991.43, (2) NDO by liquid chromatography (LC) in AOAC Official Method 2001.03, and (3) RS by AOAC Official Method 2002.02. The correlation coefficient (R(2)) comparing calculated amounts versus measured amounts of total NDC in 11 bread samples was 0.92. Analysis of commercial food samples was also well matched with the DF + NDO value on their nutritional label. Consequently, we confirmed a single measurement of LC can determine all NDO in foods, and total NDC in foods can be determined by unifying existing AOAC Official Methods.

  11. Characterization of impurities in tylosin using dual liquid chromatography combined with ion trap mass spectrometry.

    Science.gov (United States)

    Chopra, Shruti; Van Schepdael, Ann; Hoogmartens, Jos; Adams, Erwin

    2013-03-15

    Investigation of unknown impurities in a tylosin sample was performed using liquid chromatography coupled to mass spectrometry (LC/MS). Separation was performed according to the recently described LC-UV method of Ashenafi et al. (2011) [14]. This method was reported to have a good selectivity as it was able to separate the four main components of tylosin from the already known and 23 unknown impurities. However, as this method uses a mobile phase with non-volatile constituents, direct characterization of these impurities using LC/MS was not possible. The impurity fractions were therefore first collected and then desalted before sending them to the MS. Identification of the impurities in the tylosin sample was performed with a quadruple ion trap (IT) MS, with an electrospray ionization (ESI) source in the positive ion mode. The structure of the impurities was deduced by comparing their fragmentation pattern with those of the main components of tylosin. As several peaks in the LC-UV method contained multiple compounds, using this method in total 41 new impurities were (partly) characterized. Copyright © 2012 Elsevier B.V. All rights reserved.

  12. Cleanup procedure for determination of aflatoxins in major agricultural commodities by liquid chromatography.

    Science.gov (United States)

    Sobolev, Victor S; Dorner, Joe W

    2002-01-01

    A simple, fast, reliable, and inexpensive chemical cleanup procedure was developed for quantitation of aflatoxins in major important agricultural commodities by liquid chromatography (LC). Aflatoxins were extracted from a ground sample with methanol-water (80 + 20, v/v), and after a single cleanup step on a minicolumn packed with basic aluminum oxide, they were quantitated by LC equipped with a C18 column, photochemical reactor, and fluorescence detector. Water-methanol-1-butanol (1,400 + 720 + 25, v/v/v) served as the mobile phase. Recoveries of aflatoxins B1, B2, G1, and G2 from peanuts spiked at 5.0, 2.5, 7.5, and 2.5 microg/kg were 87.2 +/- 2.3, 82.0 +/- 0.8, 80.0 +/- 1.8, and 80.4 +/- 2.8%, respectively. Similar recoveries, precision, and accuracy were achieved for corn, cottonseed, almonds, Brazil nuts, pistachios, and walnuts. The quantitation limit for aflatoxin B1 was 1 microg/kg. The minimal cost of the minicolumn allows for substantial savings compared with available commercial aflatoxin cleanup devices.

  13. Simultaneous determination of organic acids and vitamin C in green beans by liquid chromatography.

    Science.gov (United States)

    Vazquez Oderiz, M L; Vazquez Blanco, M E; Lopez Hernandez, J; Simal Lozano, J; Romero Rodriguez, M A

    1994-01-01

    A method is described for determining and quantitating organic acids (oxalic, malic, citric, and fumaric) and vitamin C by liquid chromatography with a UV-visible detector that allows simultaneous monitoring at 2 wavelengths. The method was applied to samples of green beans (Phaseolus vulgaris L.). Recoveries were 97.8% for oxalic acid, 98.9% for malic acid, 98.7% for citric acid, 99.2% for fumaric acid, and 98.5% for vitamin C. Method precisions (coefficients of variation) were 1.7% for oxalic acid, 0.8% for malic acid, 0.9% for citric acid, 1.5% for fumaric acid, and 1.2% for vitamin C. Measurement precisions (coefficients of variation) were 1.32% for oxalic acid, 0.33% for malic acid, 0.62% for citric acid, 1.01% for fumaric acid, and 0.39% for vitamin C. Limits of detection were 0.025 mg/mL for oxalic acid, 0.022 mg/mL for malic acid, 0.024 mg/mL for citric acid, 1.0 x 10(-4) mg/mL for fumaric acid, and 2.7 x 10(-4) mg/mL for vitamin C.

  14. Simultaneous determination of 30 ginsenosides in Panax ginseng preparations using ultra performance liquid chromatography

    Science.gov (United States)

    Park, Hee-Won; In, Gyo; Han, Sung-Tai; Lee, Myoung-Woo; Kim, So-Young; Kim, Kyung-Tack; Cho, Byung-Goo; Han, Gyeong-Ho; Chang, Il-Moo

    2013-01-01

    A quick and simple method for simultaneous determination of the 30 ginsenosides (ginsenoside Ro, Rb1, Rb2, Rc, Rd, Re, Rf, Rg1, 20(S)-Rg2, 20(R)-Rg2, 20(S)-Rg3, 20(R)-Rg3, 20(S)-Rh1, 20(S)-Rh2, 20(R)-Rh2, F1, F2, F4, Ra1, Rg6, Rh4, Rk3, Rg5, Rk1, Rb3, Rk2, Rh3, compound Y, compound K, and notoginsenoside R1) in Panax ginseng preparations was developed and validated by an ultra performance liquid chromatography photo diode array detector. The separation of the 30 ginsenosides was efficiently undertaken on the Acquity BEH C-18 column with gradient elution with phosphoric acids. Especially the chromatogram of the ginsenoside Ro was dramatically enhanced by adding phosphoric acid. Under optimized conditions, the detection limits were 0.4 to 1.7 mg/L and the calibration curves of the peak areas for the 30 ginsenosides were linear over three orders of magnitude with a correlation coefficients greater than 0.999. The accuracy of the method was tested by a recovery measurement of the spiked samples which yielded good results of 89% to 118%. From these overall results, the proposed method may be helpful in the development and quality of P. ginseng preparations because of its wide range of applications due to the simultaneous analysis of many kinds of ginsenosides. PMID:24235860

  15. Measurement of hemoglobin A1 by liquid chromatography and by agar gel electrophoresis compared.

    Science.gov (United States)

    Hayes, E J; Gleason, R E; Soeldner, J S; Wacks, M; Blankstein, L

    1981-03-01

    We compare measurement of total fast hemoglobin (HbA1) by "high-performance" liquid chromatography and by electrophoresis on agar gel. Blood samples were obtained from a diverse population (n = 222): offspring of two diabetic parents, diabetic patients with and without retinopathy, diabetic and non-diabetic pregnant women, patients in the coronary-care unit, and normal persons. Precision studies with a normal and an above-normal A1 sample resulted in overall CVs of 9.0% and 4.6% for the electrophoretic method and 4.4% and 2% for the chromatographic method. Linear regression analysis of values for total fast hemoglobin for the complete sample population and for each subgroup showed results of the electrophoretic method to be in excellent agreement with those by the chromatographic method. We conclude that the agar gel electrophoretic method offers a reproducible means for HbA1 determination that is comparable to the HPLC method in terms of accuracy and is highly suited for routine laboratory use.

  16. Detection of honey adulteration with starch syrup by high performance liquid chromatography.

    Science.gov (United States)

    Wang, Shaoqing; Guo, Qilei; Wang, Linlin; Lin, Li; Shi, Hailiang; Cao, Hong; Cao, Baosen

    2015-04-01

    According to saccharide profile comparison between starch syrups and pure honeys analysed through high performance liquid chromatography (HPLC), a characteristic peak was found at 15.25 min retention time in HPLC chromatogram of syrup, but no peak was observed at the same retention time in chromatogram of pure honeys. This characteristic peak for syrup was identified as an overlapping peak of oligosaccharides with more than 5 degree of polymerisation (DP) based on HPLC chromatogram comparison between starch syrup and a series of standard mono-, di- and oligosaccharides of 3-7 DP. Additionally syrup content correlated linearly with the height of the characteristic peak of syrup under different slope in two ranges 2.5-7.5% and 10-100%, respectively. Therefore, the characteristic peak at 15.25 min retention time can serve as a syrup indicator in HPLC analysis of the adulterated honeys. This new HPLC method for honey adulteration detection was further applied in an authenticity inspection on more than 100 commercial honeys. In addition to the improved accuracy of honey adulteration detection, the proposed HPLC method was simple, low cost and easy practice for honey product quality control by government department considering the popularity of HPLC device and technology. Copyright © 2014 Elsevier Ltd. All rights reserved.

  17. Quantitative Determination of Compounds from Akebia quinata by High-Performance Liquid Chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Yen, Nguyen; Thu, Nguyen; Zhao, Bing Tian; Woo, Mi Hee; Min, Byung Sun [Catholic Univ. of Daegu, Gyeongsan (Korea, Republic of); Lee, Jae Hyun [Dongguk Univ., Yongin (Korea, Republic of); Kim, Jeong Ah [Kyungpook National Univ., Daegu (Korea, Republic of); Son, Jong Keun [Yeungnam Univ., Gyeongsan (Korea, Republic of); Choi, Jae Sui [Pukyung National Univ., Busan (Korea, Republic of); Woo, Eun Rhan [Chosun Univ., Gwangju (Korea, Republic of)

    2014-07-15

    To provide the scientific corroboration of the traditional uses of Akebia quinata (Thunb.) Decne., a detailed analytical examination of A. quinata stems was carried out using a reversed-phase high performance liquid chromatography (RP-HPLC) method coupled to photodiode array detector (PDA) for the simultaneous determination of four phenolic substances; cuneataside D, 2-(3,4-dihydroxyphenyl)ethyl-O-β-D-glucopyranoside, 3-caffeoylquinic acid and calceolarioside B. Particular attention was focused on the main compound, 3-caffeoylquinic acid, which has a range of biological functions. In addition, 2-(3,4-dihydroxyphenyl)ethyl-O-β-D-glucopyranoside was considered as a discernible marker of A. quinata from its easy confuse plants. The contents of compounds 2 and 3 ranged from 0.72 to 2.68 mg/g and from 1.66 to 5.64 mg/g, respectively. The validation data indicated that this HPLC/PDA assay was used successfully to quantify the four phenolic compounds in A. quinata from different locations using relatively simple conditions and procedures. The pattern-recognition analysis data from 53 samples classified them into two groups, allowing discrimination between A. quinata and comparable herbs. The results suggest that the established HPLC/PDA method is suitable for quantitation and pattern-recognition analyses for a quality evaluation of this medicinal herb.

  18. Determination of Diclofenac sodium by high-performance liquid chromatography in 0,1 % eyedrops

    International Nuclear Information System (INIS)

    Garcia Penna, Caridad Margarita; Pereda Rodriguez, Diana; Gonzalez Hortezon, Ania; Montes de Oca Porto, Yanet; Cannizares Arencibia, Yanara; Leon Guerrero, Gissel Maria

    2009-01-01

    Diclofenac sodium is a drug prescribed in eye anterior segment inflammation postoperative treatments, preoperative and postoperative cataract meiosis inhibition, symptomatic treatment of non-infectious chronic conjunctivitis, of ocular inflammation, of ocular pain, and of refractory postsurgical photophobia. In present paper we developed and validated an analytical method by high-performance liquid chromatography to quality control, and stability studies of Diclofenac sodium of 1 % eye drops. Method was based on active principle separation through endcapped 1 00RP-8 Lichrospher chromatographic column (5 μ) (250 x 4 mm) using UV detection to 254 nm, thus using a mobile phase including sodium a solution of hydrogen phosphate to a 2.5 pH: methanol in a 34:60 ratio. Calibration curve was plotted during the interval of 60 to 140 % where it was linear with a correlation coefficient equal to 0.9995; statistic test for interception and slope was considered as non-significant. We achieved a recovery rate of 100.25 % during study concentration interval, and Cochran (G) and Student (t) tests were not significant. Variation coefficient in repeating study was equal to 0.39 % for the 6 assayed replica, whereas in average precision analysis Fischer and Student tests were non-significant. Analytical method was linear, precise, specific and exact during the interval of study concentrations. (Author)

  19. 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.

  20. Surfactant-bound monolithic columns for separation of proteins in capillary high performance liquid chromatography.

    Science.gov (United States)

    Gu, Congying; He, Jun; Jia, Jinping; Fang, Nenghu; Simmons, Robert; Shamsi, Shahab A

    2010-01-22

    A surfactant-bound monolithic stationary phase based on the co-polymerization of 11-acrylamino-undecanoic acid (AAUA) is designed for capillary high performance liquid chromatography (HPLC). Using D-optimal design, the effect of the polymerization mixture (concentrations of monomer, crosslinker and porogens) on the chromatographic performance (resolution and analysis time) of the AAUA-EDMA monolithic column was evaluated. The polymerization mixture was optimized using three proteins as model test solutes. The D-optimal design indicates a strong dependence of chromatographic parameters on the concentration of porogens (1,4-butanediol and water) in the polymerization mixture. Optimized solutions for fast separation and high resolution separation, respectively, were obtained using the proposed multivariate optimization. Differences less than 6.8% between the predicted and the experimental values in terms of resolution and retention time indeed confirmed that the proposed approach is practical. Using the optimized column, fast separation of proteins could be obtained in 2.5 min, and a tryptic digest of myoglobin was successfully separated on the high resolution column. The physical properties (i.e., morphology, porosity and permeability) of the optimized monolithic column were thoroughly investigated. It appears that this surfactant-bound monolith may have a great potential as a new generation of capillary HPLC stationary phase. Copyright 2009 Elsevier B.V. All rights reserved.