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Sample records for simultaneous hptlc determination

  1. Simultaneous HPTLC Determination of Rabeprazole and Itopride Hydrochloride From Their Combined Dosage Form

    OpenAIRE

    Suganthi, A.; John, Sofiya; Ravi, T. K.

    2008-01-01

    A simple, precise, sensitive, rapid and reproducible HPTLC method for the simultaneous estimation of the rabeprazole and itopride hydrochloride in tablets was developed and validated. This method involves separation of the components by TLC on precoated silica gel G60F254 plate with solvent system of n-butanol, toluene and ammonia (8.5:0.5:1 v/v/v) and detection was carried out densitometrically using a UV detector at 288 nm in absorbance mode. This system was found to give compact spots for ...

  2. Simultaneous HPTLC determination of strychnine and brucine in strychnos nux-vomica seed

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    Abid Kamal

    2012-01-01

    Full Text Available Objective: A simple, sensitive, and specific thin layer chromatography (TLC densitometry method has been developed for the simultaneous quantification of strychnine and brucine in the seeds of Strychnos nux-vomica. Materials and Methods: The method involved simultaneous estimation of strychnine and brucine after resolving it by high performance TLC (HPTLC on silica gel plate with chloroform-methanol-formic acid (8.5:1.5:0.4 v/v/v as the mobile phase. Results: The method was validated as per the ICH guidelines for precision (interday, intraday, intersystem, robustness, accuracy, limit of detection, and limit of quantitation. The relationship between the concentration of standard solutions and the peak response was linear within the concentration range of 50-1000 ng/spot for strychnine and 100-1000 ng/spot for brucine. The method precision was found to be 0.58-2.47 (% relative standard deviation [RSD] and 0.36-2.22 (% RSD for strychnine and brucine, respectively. Accuracy of the method was checked by recovery studies conducted at three different concentration levels and the average percentage recovery was found to be 100.75% for strychnine and 100.52% for brucine, respectively. Conclusions: The HPTLC method for the simultaneous quantification of strychnine and brucine was found to be simple, precise, specific, sensitive, and accurate and can be used for routine analysis and quality control of raw material of S. nux-vomica and several unani and ayurvedic formulations containing this as an ingredient.

  3. Simultaneous HPTLC Determination of Rabeprazole and Itopride Hydrochloride From Their Combined Dosage Form.

    Science.gov (United States)

    Suganthi, A; John, Sofiya; Ravi, T K

    2008-01-01

    A simple, precise, sensitive, rapid and reproducible HPTLC method for the simultaneous estimation of the rabeprazole and itopride hydrochloride in tablets was developed and validated. This method involves separation of the components by TLC on precoated silica gel G60F254 plate with solvent system of n-butanol, toluene and ammonia (8.5:0.5:1 v/v/v) and detection was carried out densitometrically using a UV detector at 288 nm in absorbance mode. This system was found to give compact spots for rabeprazole (Rf value of 0.23 0.02) and for itopride hydrochloride (Rf value of 0.75+/-0.02). Linearity was found to be in the range of 40-200 ng/spot and 300-1500 ng/spot for rabeprazole and itopride hydrochloride. The limit of detection and limit of quantification for rabeprazole were 10 and 20 ng/spot and for itopride hydrochloride were 50 and 100 ng/spot, respectively. The method was found to be beneficial for the routine analysis of combined dosage form.

  4. A High-Performance Thin Layer Chromatography (HPTLC) Method for Simultaneous Determination of Diphenhydramine Hydrochloride and Naproxen Sodium in Tablets.

    Science.gov (United States)

    Bhole, R P; Shinde, S S; Chitlange, S S; Wankhede, S B

    2015-01-01

    A rapid and simple high-performance thin layer chromatography (HPTLC) method with densitometry at 230 nm was developed and validated for simultaneous determination of diphenhydramine hydrochloride (DPH) and naproxen sodium (NPS) from pharmaceutical preparation. The separation was carried out on aluminum plates precoated with silica gel 60 F254 using mobile phase toluene:methanol:glacial acetic acid (7.5:1:0.2, v/v/v). The linearity range lies between 200 and 1200 ng/band for DPH and 1760 and 10,560 ng/band for NPS with correlation coefficients of 0.994 and 0.995, respectively. The R f value for DPH is 0.20 ± 0.05 and for NPS is 0.61 ± 0.06. % Recoveries of DPH and NPS was in the range of 99.70%-99.95% and 99.63%-99.95%, respectively. Limit of detection value for DPH was 13.21 ng/band and for NPS was 8.03 ng/band. Limit of quantitation value for DPH was 40.06 ng/band and for NPS was 24.34 ng/band. The developed method was validated as per ICH guidelines. In stability testing, DPH was found unstable to acid and alkaline hydrolysis, and DPH and NPS were found unstable to oxidation, whereas both the drugs were stable to neutral and photodegradation. The proposed method was successfully applied for the routine quantitative analysis of dosage form containing DPH and NPS.

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

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    Kaliappan Ilango

    2013-01-01

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

  6. Simultaneous determination of hydrochlorothiazide and benazepril hydrochloride or amiloride hydrochloride in presence of hydrochlorothiazide impurities: chlorothiazide and salamide by HPTLC method.

    Science.gov (United States)

    Naguib, Ibrahim A; Abdelaleem, Eglal A; Zaazaa, Hala E; Draz, Mohammed E

    2015-01-01

    Simple, selective and sensitive high-performance thin layer chromatographic (HPTLC) method has been developed and validated for the simultaneous determination of hydrochlorothiazide (HCZ) in the presence of its impurities (chlorothiazide (CT) and salamide (DSA)), in two quaternary mixtures with benazepril hydrochloride (BZ) or amiloride hydrochloride (AM). The separation was carried out on HPTLC silica gel 60 F254 using ethyl acetate-methanol-glacial acetic acid (85:2:0.3 v/v/v) followed by densitometric measurement of bands at 240 nm for the first mixture containing HCZ, CT, DSA, BZ and by using ethyl acetate-methanol-water-ammonia (90:10:5:3 v/v/v) followed by densitometric measurement at 278 nm for the second mixture containing HCZ, CT, DSA, AM. Calibration curves were constructed in the range of (0.2-1.8 µg/band) and (0.4-2.2 µg/band) with good accuracy for HCZ and BZ, respectively, for the first mixture and in the range of (0.6-1.8 µg/band) and (0.4-2.4 µg/band) with good accuracy for HCZ and AM, respectively, for the second mixture. The developed method was validated according to ICH guidelines and demonstrated good accuracy and precision. Moreover, the methods were successfully applied for the determination of HCZ and BZ and AM in pure form and pharmaceutical dosage forms. The results were statically compared with the reported methods with no significant difference, indicating the ability of the proposed method to be used for routine analysis of drug product. © The Author [2014]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  7. Simultaneous determination of five active compounds in chimonanthus nitens by double-development HPTLC and scanning densitometry

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    Zhou Bin

    2012-05-01

    Full Text Available Abstract Background Chimonanthus nitens (family Calycanthaceae, Shanlamei in Chinese, is an unique species in China. The extract of dried leaves of Chimonanthus nitens has anti-inflammatory, antipyretic and antitussive effects. Terpenes, coumarins, and flavonoids are usually regarded as the main active components. Therefore, simultaneous determination of these compounds is very important to control the quality of Chimonanthus nitens. Results A double-development TLC method was developed for simultaneous analysis of five compounds in Chimonanthus nitens. The chromatography was performed on silica gel 60 plate with chloroform-methanol (9∶1, v/v and petroleum ether-ethyl acetate (10∶1, v/v as mobile phase for twice development. Their characteristic TLC profiles were observed under UV light at 365 nm and the bands were then revealed by reaction with 1% vanillin-H2SO4 solution. Quantification of three monoterpenes was achieved by densitometry at 545 nm (β-caryophyllene or 606 nm (cineole and linalool. Two coumarins (scopoletin and scoparone were determined by densitometry at 340 nm with filter wavelength of 370 nm. The investigated compounds had good linearity (R2 >0.99 within test ranges. Conclusions The developed double-development TLC method is helpful to control the quality of Chimonanthus nitens, which is simple and accurate.

  8. HPTLC determination of diosgenin in fenugreek seeds

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    Król-Kogus Barbara

    2018-03-01

    Full Text Available A new HPTLC-densitometric method for diosgenin determination in fenugreek seeds was established after optimization of the conditions for efficient saponin extraction and acid hydrolysis. Several procedures were tested, the best of which was a three-step Soxhlet extraction, followed by hydrolysis of the obtained methanolic extract with 2 mol L-1 H2SO4. Best diosgenin separation from other hydrolysis products was obtained on HPTLC Si60F254 plates u sing a mixture of n-heptane/ethyl acetate (7:3, V/V and modified anisaldehyde as a spraying reagent. The method was preliminarily validated and the determined amounts of diosgenin in fenugreek seeds of Polish and African origin were found to be similar and ranged from 0.12-0.18 %.

  9. Simultaneous densitometric determination of anthelmintic drug albendazole and its metabolite albendazole sulfoxide by HPTLC in human plasma and pharmaceutical formulations.

    Science.gov (United States)

    Pandya, Jui J; Sanyal, Mallika; Shrivastav, Pranav S

    2017-09-01

    A new, simple, accurate and precise high-performance thin-layer chromatographic method has been developed and validated for simultaneous determination of an anthelmintic drug, albendazole, and its active metabolite albendazole, sulfoxide. Planar chromatographic separation was performed on aluminum-backed layer of silica gel 60G F 254 using a mixture of toluene-acetonitrile-glacial acetic acid (7.0:2.9:0.1, v/v/v) as the mobile phase. For quantitation, the separated spots were scanned densitometrically at 225 nm. The retention factors (R f ) obtained under the established conditions were 0.76 ± 0.01 and 0.50 ± 0.01 and the regression plots were linear (r 2  ≥ 0.9997) in the concentration ranges 50-350 and 100-700 ng/band for albendazole and albendazole sulfoxide, respectively. The method was validated for linearity, specificity, accuracy (recovery) and precision, repeatability, stability and robustness. The limit of detection and limit of quantitation found were 9.84 and 29.81 ng/band for albendazole and 21.60 and 65.45 ng/band for albendazole sulfoxide, respectively. For plasma samples, solid-phase extraction of analytes yielded mean extraction recoveries of 87.59 and 87.13% for albendazole and albendazole sulfoxide, respectively. The method was successfully applied for the analysis of albendazole in pharmaceutical formulations with accuracy ≥99.32%. Copyright © 2017 John Wiley & Sons, Ltd.

  10. Validated high-performance thin-layer chromatographic (HPTLC method for simultaneous determination of nadifloxacin, mometasone furoate, and miconazole nitrate cream using fractional factorial design

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    Kalpana G. Patel

    2016-07-01

    Full Text Available A high-performance thin-layer chromatographic method for simultaneous determination of nadifloxacin, mometasone furoate, and miconazole nitrate was developed and validated as per International Conference on Harmonization guidelines. High-performance thin-layer chromatographic separation was performed on aluminum plates precoated with silica gel 60F254 and methanol:ethyl acetate:toluene: acetonitrile:3M ammonium formate in water (1:2.5:6.0:0.3:0.2, % v/v as optimized mobile phase at detection wavelength of 224 nm. The retardation factor (Rf values for nadifloxacin, mometasone furoate, and miconazole nitrate were 0.23, 0.70, and 0.59, respectively. Percent recoveries in terms of accuracy for the marketed formulation were found to be 98.35–99.76%, 99.36–99.65%, and 99.16–100.25% for nadifloxacin, mometasone furoate, and miconazole nitrate, respectively. The pooled percent relative standard deviation for repeatability and intermediate precision studies was found to be < 2% for three target analytes. The effect of four independent variables, methanol content in total mobile phase, wavelength, chamber saturation time, and solvent front, was evaluated by fractional factorial design for robustness testing. Amongst all four factors, volume of methanol in mobile phase appeared to have a possibly significant effect on retention factor of miconazole nitrate compared with the other two drugs nadifloxacin and mometasone furoate, and therefore it was important to be carefully controlled. In summary, a novel, simple, accurate, reproducible, and robust high-performance thin-layer chromatographic method was developed, which would be of use in quality control of these cream formulations.

  11. Determination of isopropylthioxanthone (ITX) in milk, yoghurt and fat by HPTLC-FLD, HPTLC-ESI/MS and HPTLC-DART/MS.

    Science.gov (United States)

    Morlock, Gertrud; Schwack, Wolfgang

    2006-06-01

    Two new HPTLC methods for quantification of isopropyl-9H-thioxanthen-9-one (ITX) in milk, yoghurt and fat samples have been developed. Extraction of ITX from milk and yoghurt was performed with a mixture of cyclohexane and ethyl acetate by employment of accelerated solvent extraction (ASE). For soy bean oil and margarine, a simple partitioning of ITX into acetonitrile was used. ITX and 2,4-diethyl-9H-thioxanthen-9-one (DTX) used as internal standard have been separated on silica gel 60 HPTLC plates with a mixture of toluene and n-hexane (4:1, v/v) and on RP18 HPTLC plates with a mixture of acetonitrile and water (9:1, v/v). Development was performed anti-parallel from both plate sides leading to a throughput of 36 separations in 7 min. Fluorescence measurement at 254/>400 nm was used for quantification. Limits of detection (S/N of 3) have been established to be 64 pg for ITX and DTX on both types of HPTLC plates. In fatty matrix (spiked butter) LOD of ITX was determined to be 1 mug kg(-1). In the working range monitored (20-200 microg kg(-1)) polynomial regression of ITX showed a relative standard deviation (sdv) of +/-1.51 % (r = 0.99981). Starting with the limit of quantification the response was linear (sdv = +/-2.18 %, r = 0.99893). Regarding repeatability (n = 9) a coefficient of variation (CV) of 1.1 % was obtained for ITX at 32 ng on silica gel plates and of 2.9 % on reversed-phase plates. Repeatabilities (n = 4) of ITX determination at 20, 50 and 100 microg kg(-1) in milk, yoghurt, soybean oil and margarine showed CVs between +/-1.0 and 6.4 %. The results prove that modern planar chromatography is a rapid and cost-efficient alternative method to quantify ITX in milk-based or fatty matrices. Only positive results are confirmed by online ESI/MS in the SIM mode (LOQ 128 pg) and by DART/MS involving a minimal employment of the MS device, which is a further advantage of HPTLC. Overall mean recovery rates of ITX at 20 or 50 and 100 microg kg(-1) (n = 8) were 41

  12. Development and validation of an HPTLC method for the simultaneous estimation of Clonazepam and Paroxetine hydrochloride using a DOE approach

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    Purvi Shah

    2017-01-01

    Full Text Available The present study examines simultaneous multiple response optimization using Derringer's desirability function for the development of an HPTLC method to detect Clonazepam and Paroxetine hydrochloride in pharmaceutical dosage form. Central composite design (CCD was used to optimize the chromatographic conditions for HPTLC. The independent variables used for the optimization were the n-butanol content in the mobile phase, the chamber saturation time and the distance travelled. HPTLC separation was performed on aluminium plates pre-coated with silica gel 60 F254 as the stationary phase using n-butanol:glacial acetic acid:water (9:2:0.5% v/v/v as the mobile phase. Quantification was achieved based on a densitometric analysis of Clonazepam and Paroxetine hydrochloride over the concentration range of 40–240 ng/band and 300–1800 ng/band, respectively, at 288 nm. The method yielded compact and well-resolved bands at Rf of 0.77 ± 0.02 and 0.34 ± 0.02 for Clonazepam and Paroxetine hydrochloride, respectively. The linear regression analysis for the calibration plots produced r2 = 0.9958 and r2 = 0.9989 for Clonazepam and Paroxetine hydrochloride, respectively. The precision, accuracy, robustness, specificity, limit of detection and limit of quantitation of the method were validated according to the ICH guidelines. The factors evaluated in the robustness test were determined to have an insignificant effect on the selected responses. The results indicate that the method is suitable for the routine quality control testing of marketed tablet formulations.

  13. Validated HPTLC methods for determination of some selected antihypertensive mixtures in their combined dosage forms

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    Rasha A. Shaalan

    2014-12-01

    Full Text Available Simple and selective HPTLC methods were developed for the simultaneous determination of the antihypertensive drugs; carvedilol and hydrochlorothiazide in their binary mixture (Mixture I and amlodipine besylate, valsartan, and hydrochlorothiazide in their combined ternary formulation (Mixture II. Effective chromatographic separation was achieved on Fluka TLC plates 20 × 20 cm aluminum cards, 0.2 mm thickness through linear ascending development. For Mixture I, the mobile phase composed of chloroform–methanol in the ratio 8:2 v/v. Detection was performed at 254 nm for both carvedilol and hydrochlorothiazide. For Mixture II, the mobile phase was chloroform–methanol–ammonia in the volume ratio 8:2:0.1. Detection was performed at 254 nm for valsartan and hydrochlorothiazide, and at 365 nm for amlodipine. Quantification was based on spectrodensitometric analysis. Analytical performance of the proposed HPTLC procedures was statistically validated with respect to linearity, ranges, precision, accuracy, specificity, robustness, detection and quantification limits. The linearity ranges were 0.05–1.0 and 0.1–2.0 μg/spot for carvedilol and hydrochlorothiazide, respectively in Mixture I, 0.1–2.0, 0.1–2.0 and 0.2–4.0 μg/spot for amlodipine, hydrochlorothiazide and valsartan, respectively in Mixture II, with correlation coefficients >0.9992. The validated HPTLC methods were applied to the analysis of the cited antihypertensive drugs in their combined pharmaceutical tablets. The proposed methods confirmed peak identity and purity.

  14. Phytochemical investigation and simultaneous estimation of bioactive lupeol and stigmasterol in Abutilon indicum by validated HPTLC method

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    Md. Sarfaraj Hussain

    2014-05-01

    Full Text Available Objective: To perform a simultaneous quantitative estimation of two biologically active triterpenoid compounds lupeol and a steroid compound, stigmasterol, in Abutilon indicum (A. indicum using high-performance thin-layer chromatography (HPTLC. Methods: TLC aluminum plates precoated with silica-gel 60 F254 (20 cm×10 cm were used with a mobile phase of toluene-methanol-formic acid (7.0:2.7:0.3, v/v/v and densitometric determination of these compounds was carried out at 530 nm in reflectance/absorbance mode. Results: Compact bands for lupeol and stigmasterol were obtained at Rf 0.52±0.02 and 0.28±0.05. The limit of detection (45 and 18 ng/band, limit of quantification (135 and 54 ng/band, recovery (98.2%-99.7% and 97.2%-99.6% and precision (≤2.18 and 1.91 were satisfactory for lupeol and stigmasterol respectively. Linearity range for lupeol and stigmasterol were 100-1000 (r 2 =0.999 4 and 50-500 ng/band (r 2 =0.994 1 and the contents were estimated as (0.59±0.10% and (0.83±0.10% w/ w respectively. The total phenolic, flavonoid, proanthocyanidin, alkaloidal and saponin contents of methanolic extract of A. indicum were also measured in this work. According to International Conference on Harmonization (ICH guidelines, the method was validated for linearity, precision, accuracy, and recovery, limit of detection, limit of quantification, specificity, and robustness. Conclusions: The HPTLC method was found to be reproducible, accurate, and precise and could detect these two compounds at nanogram level from the A. indicum.

  15. Separation and determination of PETN and TNT by HPTLC

    Energy Technology Data Exchange (ETDEWEB)

    Chaloosi, Marzieh; Nejad-Darzi, Seyed Karim Hassani; Ghoulipour, Vanik [Faculty of Chemistry, University of Tarbiat Moallem, Tehran (Iran)

    2009-02-15

    High-performance thin layer chromatography (HPTLC) has been used for the separation and quantification of 2,4,6-trinitrotoluene (TNT) and pentaerythritol tetranitrate (PETN). The compounds were separated on silica gel 60 F{sub 254} with a double development system of trichloroethylene-acetone 4:1 and petroleum ether-acetone 5.7:1. For obtaining chromatograms of these materials, UV detection was performed at 215 and 250 nm for PETN and TNT, respectively. The linear dynamic range was 0.835-83.50 {mu}g per spot for PETN and 0.045-1.44 {mu}g per spot for TNT. (Abstract Copyright [2009], Wiley Periodicals, Inc.)

  16. Novel HPTLC and UV-AUC analyses: For simple, economical, and rapid determination of Zileuton racemate

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    Saurabh B. Ganorkar

    2017-03-01

    Full Text Available Novel, simple, rapid and reliable High-Performance Thin-Layer Chromatographic (HPTLC and UV-spectroscopic area under curve (UV-AUC methods were developed and validated for the analysis of zileuton racemate in bulk and in in-house tablet formulation. HPTLC quantitation of zileuton was done by UV detection at 260 nm and analysis was performed on (20 × 10 cm aluminium sheets precoated with silica gel 60-F254 (E. Merck as stationary phase and toluene–methanol–glacial acetic acid (3.5:1.5:0.1 v/v as mobile phase. Quantitation by HPTLC method was performed over the concentration range of 200–1200 ng/band. The HPTLC method resulted into a compact and well resolved band for zileuton at retention factor (Rf of 0.51 ± 0.02. Linear regression analysis data for calibration of HPTLC method represented a good linear relationship with regression coefficient; r2 = 0.997. UV-AUC method was developed using sodium lauryl sulphate (0.05 M as a hydrotropic agent to enhance water solubility and area was determined at a wavelength range in between 248.40 and 271.0 nm. Correlation coefficient for UV-AUC analysis was found to be r2 = 0.999. The developed UV-AUC method depicted a fine linear relationship for zileuton racemate in a concentration range of 2–12 μg/mL. Both the developed methods were validated for precision, robustness, ruggedness, accuracy, sensitivity as per guidelines laid by the International Conference on Harmonisation (ICH. Statistical analysis proved that the developed methods were precise, robust, sensitive and accurate and can be used effectively for the analysis of zileuton in bulk and pharmaceutical formulations.

  17. Stability-Indicating HPTLC Method for Simultaneous Estimation of Flurbiprofen and Chloramphenicol in Ophthalmic Solution.

    Science.gov (United States)

    Sadakwala, Vaishnavi M; Chauhan, Renu S; Shah, Shailesh A; Shah, Dinesh R

    2016-01-01

    A specific, accurate and reproducible stability-indicating high performance thin layer chromatography (HPTLC) method was developed for the estimation of flurbiprofen and chloramphenicol in the presence of their degradation products. Degradation studies of both the drugs were carried out in acidic, alkaline, neutral, oxidative, photolytic and thermal stress conditions. Separation was performed on thin layer chromatography plate precoated with silica gel 60 F254 using ethyl acetate : n-hexane : methanol : tri-ethyl amine (5 : 4 : 2 : 0.5, v/v/v/v). Spots at retention factor 0.29 and 0.62 were recognized as flurbiprofen and chloramphenicol, respectively, and were quantified through densitometric measurements at wavelength 267 nm. Method was found to be linear over the concentration range 12-60 ng/spot with correlation coefficient of 0.9997 for flurbiprofen and 200-1,000 ng/spot with correlation coefficient of 0.9977 for chloramphenicol. The proposed method was applied to the estimation of flurbiprofen and chloramphenicol in commercial ophthalmic formulation. The developed HPTLC method can be applied for routine analysis of flurbiprofen and chloramphenicol in the presence of their degradation products in their individual as well as combined pharmaceutical formulations. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  18. Analytical methods for determination of alkaloids and saponins from roots of Caulophyllum thalictroids (L) Michx using UPLC HPLC and HPTLC

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    A comparison study of analytical methods including HPLC, UPLC and HPTLC are presented in this paper for the determination of major alkaloid and triterpene saponins from the roots of Caulophyllum thalictroides (L.) Michx. (blue cohosh) and dietary supplements claiming to contain blue cohosh. The meth...

  19. Determination of Sugar Composition of Polysaccharides in Caesalpinia pulcherrima Galactomannan Solution Using HPTLC

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    Nilima A. THOMBRE

    2015-04-01

    Full Text Available Galactomannans (GM, a group of neutral nontoxic polysaccharides naturally occurring in the seeds of some legumes, are used in the textile, pharmaceutical, biomedical, cosmetics and food industries. As to date there are no documented reports on determination of the sugar composition in polysaccharides by HPTLC and the following study is an attempt in this direction. GM from seeds of Caesalpinia pulcherrima L. (CP was isolated and purified by precipitation method using alcohol. A new, simple, sensitive, selective, precise, and robust HPTLC method for analysis of monosaccharides such as galactose, mannose, xylose and glucose in isolated CP GM has been developed and validated. Chromatograms were developed using a mobile phase of acetone: water (9:1 v/v on pre-coated plate of silica gel GF aluminium TLC plate and quantified by UV spectrophotometer at 254nm. The Rf values were 0.45, 0.34, 0.40 and 0.60 for mannose, galactose, xylose and glucose, respectively. The linearity of method was found to be within the concentration range of 2000-10000 ng/spot for all above monosaccharides. The limit of detection for mannose, galactose, xylose and glucose was found to be 0.14986 ng/spot, 0.31973 ng/spot, 0.27569 ng/spot, and 0.36808 ng/spot, respectively. The limit of quantification for mannose, galactose, xylose and glucose was found to be 1.498 ng/spot, 3.197 ng/spot, 2.756 ng/spot, and 3.680 ng/spot, respectively. The method was also validated for precision, specificity and recovery. This developed method was used to analyze CP GM for monosaccharides compositions

  20. A validated and densitometric HPTLC method for the simultaneous quantification of reserpine and ajmalicine in Rauvolfia serpentina and Rauvolfia tetraphylla

    OpenAIRE

    Pandey, Devendra Kumar; Radha,; Dey, Abhijit

    2016-01-01

    ABSTRACT High performance thin layer chromatographic method (HPTLC) has been developed for the quantification of reserpine and ajmalicine in root part of two different population of Rauvolfia serpentina (L.) Benth. ex Kurz and Rauvolfia tetraphylla L., Apocynaceae, collected from Punjab and Uttarakhand. HPTLC of methanolic extract of root containing indole alkaloids, i.e., reserpine and ajmalicine, was performed on TLC Silicagel 60 F254 (10 cm × 10 cm) plates with toluene:ethyl acetate:formic...

  1. Validation of the method for the simultaneous estimation of bioactive marker gallic acid and quercetin in Abutilon indicum by HPTLC

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    Md. Sarfaraj Hussain

    2012-05-01

    Full Text Available Objective: To establish and validate an simultaneous estimation of the two biomarker compounds gallic acid (GA and quercetin (QE from methanolic extract of Abutilon indicum (AI. Methods: Chromatography was performed on aluminium foil-backed silica gel 60 F254 HPTLC plates with the binary mobile phase toluene-ethyl acetate-formic acid (5:4:1, v/v/v. Ultraviolet detection was performed densitometrically at the maximum absorbance wavelength, 270nm. The method was validated for precision, recovery, robustness, specificity, and detection and quantification limits, in accordance with ICH guidelines. Results: The system was found to give compact spots for GA and QE (Rf value of 0.31 and 0.50, respectively. The limit of detection (23 and 41 ng band-1 limit of quantification (69 and 123 ng band-1, recovery (99.4-99.9 and 98.7-99.4%, and precision (≤ 1.98 and 1.97 were satisfactory for gallic acid and quercetin respectively. Linearity range for GA and QE were 100-1000 (r2= 0.9991 and 150-900 ng band-1 (r2= 0.9956 and the contents estimated as 0.69% ± 0.01% and 0.57% ± 0.01% w/w respectively. Conclusions: This simple, precise and accurate method gave good resolution from other constituents present in the extract. The method has been successfully applied in the analysis and routine quality control of herbal material and formulations containing AI.

  2. Screening and determination of sibutramine in adulterated herbal slimming supplements by HPTLC-UV densitometry.

    Science.gov (United States)

    Mathon, Caroline; Ankli, Anita; Reich, Eike; Bieri, Stefan; Christen, Philippe

    2014-01-01

    The adulteration of herbal supplements is of growing importance, especially when they contain undeclared compounds like sibutramine that are unsafe drugs. Sibutramine was withdrawn from US and European markets in 2010. In this study, an HPTLC-UV densitometric method was developed for the quantification of sibutramine in herbal diet foods. Sample extracts were directly applied onto HPTLC silica gel plates and separated with a mobile phase made of a toluene-methanol mixture. Sibutramine was quantified at 225 nm and its unequivocal identification was confirmed by MS using a TLC-MS interface. During two surveys, 52 weight loss supplements obtained via the Internet were screened. Half of those were adulterated with sibutramine at amounts reaching up to 35 mg per capsule. The results of this validated HPTLC method were compared with those obtained by HPLC-UV and HPLC-MS/MS. The results were not significantly different with the three methods.

  3. Two selective HPTLC methods for determination of some angiotensin II receptor antagonists in tablets and biological fluids.

    Science.gov (United States)

    Salah, Gamal A; Abd El-Wadood, Hanaa M; Khairy, Mohamed; Khorshed, Ahmed A

    2017-07-01

    Two simple, selective, precise and highly sensitive high-performance thin-layer chromatography (HPTLC) methods have been developed and validated for analysis of five angiotensin II receptor antagonists, namely losartan, irbesartan valsartan, candesartan and olmesartan, which are widely used in clinical practice. HPTLC of the drugs was performed on pre-coated silica gel HPTLC plates 60 F 254 by development using a mobile phase composed of chloroform-acetone-glacial acetic acid (7.8:1.5:0.7m v/v/v), which was suitable for all of the studied drugs. The first method depended on utilizing reflectance/fluorescence mode for detection while the second method depended on using 2,3,5,6-tetrachloro-1,4-benzoquinone as spraying reagent for the first time to form orange spots scanned at 460 nm. A good linear relationship was obtained over the concentration ranges of 1.2-60 and 360-3000 ng/band while detection and quantification limits were in the ranges of 0.07-0.43, 45.2-140.49 and 0.21-1.29, 137.05-425.74 ng/band for reflectance/fluorescence and reflectance/absorbance methods respectively. The developed methods were applied successfully for their determination in tablets and spiked human plasma for reflectance/fluorescence method with good accuracy and precision, and so can be applied in the pharmacokinetic and bioavailability studies. Copyright © 2016 John Wiley & Sons, Ltd.

  4. Occurrence of curcuminoids in Curcuma longa : A quality standardization by HPTLC

    Directory of Open Access Journals (Sweden)

    M Paramasivam

    2008-06-01

    Full Text Available A simple high performance thin layer chromatographic (HPTLC method has been developed for the simultaneous determination of the pharmacologically important active Curcuminoids viz. curcumin, demthoxycurcumin and bis-demethoxycurcumin in Curcuma longa L. The assay combines the separation and quantification of the analytes on silica gel 60 GF254 HPTLC plates with visualisation under UV and scanning at 425 nm. Using this technique, the alkaloidal content of different parts of the title plant has been determined.

  5. Quantitative determination of vitexin in Passiflora foetida Linn. leaves using HPTLC

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    Aussavashai Shuayprom

    2016-03-01

    Conclusions: The method was evaluated for sensitivity, accuracy, precision and reproducibility. Each analysis by HPTLC is less expensive than current methods. This method is suitable for routine quality control of raw material of the leaves of P. foetida extract and its products.

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

    Science.gov (United States)

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

    2012-05-01

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

  7. Uni-dimensional double development HPTLC-densitometry method for simultaneous analysis of mangiferin and lupeol content in mango (Mangifera indica) pulp and peel during storage.

    Science.gov (United States)

    Jyotshna; Srivastava, Pooja; Killadi, Bharti; Shanker, Karuna

    2015-06-01

    Mango (Mangifera indica) fruit is one of the important commercial fruit crops of India. Similar to other tropical fruits it is also highly perishable in nature. During storage/ripening, changes in its physico-chemical quality parameters viz. firmness, titrable acidity, total soluble solid content (TSSC), carotenoids content, and other biochemicals are inevitable. A uni-dimensional double-development high-performance thin-layer chromatography (UDDD-HPTLC) method was developed for the real-time monitoring of mangiferin and lupeol in mango pulp and peel during storage. The quantitative determination of both compounds of different classes was achieved by densitometric HPTLC method. Silica gel 60F254 HPTLC plates and two solvent systems viz. toluene/EtOAC/MeOH and EtOAC/MeOH, respectively were used for optimum separation and selective evaluation. Densitometric quantitation of mangiferin was performed at 390nm, while lupeol at 610nm after post chromatographic derivatization. Validated method was used to real-time monitoring of mangiferin and lupeol content during storage in four Indian cultivars, e.g. Bombay green (Bgreen), Dashehari, Langra, and Chausa. Significant correlations (pacidity and TSSC with mangiferin and lupeol in pulp and peel during storage were also observed. Copyright © 2014 Elsevier Ltd. All rights reserved.

  8. A validated and densitometric HPTLC method for the simultaneous quantification of reserpine and ajmalicine in Rauvolfia serpentina and Rauvolfia tetraphylla

    Directory of Open Access Journals (Sweden)

    Devendra Kumar Pandey

    Full Text Available ABSTRACT High performance thin layer chromatographic method (HPTLC has been developed for the quantification of reserpine and ajmalicine in root part of two different population of Rauvolfia serpentina (L. Benth. ex Kurz and Rauvolfia tetraphylla L., Apocynaceae, collected from Punjab and Uttarakhand. HPTLC of methanolic extract of root containing indole alkaloids, i.e., reserpine and ajmalicine, was performed on TLC Silicagel 60 F254 (10 cm × 10 cm plates with toluene:ethyl acetate:formic acid (7:2:1, as mobile phase. Quantification of the reserpine and ajmalicine was performed in the absorption–reflection mode at 268 nm. The recovery of reserpine and ajmalicine were 99.3 and 98.7% respectively. The calibration curves were linear for both the reserpine and ajmalicine, in the range of 200–1200 ng. HPTLC densitometry has been performed for the estimation of reserpine and ajmalicine in root part of R. serpentina and R. tetraphylla for the first time. The method is simple, rapid and cost effective and can be used for routine analysis of ajmalicine and reserpine in different Rauvolfia species as well as for quality control of herbal drugs containing Rauvolfia species.

  9. HPTLC and reverse phase HPLC methods for the simultaneous quantification and in vitro screening of antioxidant potential of isolated sesquiterpenoids from the rhizomes of Cyperus rotundus.

    Science.gov (United States)

    Priya Rani, M; Padmakumari, K P

    2012-09-01

    Three sesquiterpenoids solavetivone, aristolone and nootkatone were isolated from the acetone extract of Cyperus rotundus by silica gel column chromatography and identified by spectral studies. Solavetivone has been isolated for the first time from the species. Simple, sensitive and selective HPTLC and HPLC methods with ultraviolet detection (245 nm) were developed and validated for the simultaneous quantification. HPTLC method was validated in terms of their linearity, LOD, LOQ, precision, accuracy and compared with RP-HPLC-UV method. Among the three sesquiterpenoids isolated, nootkatone possessed the highest radical scavenging potential (IC(50) 4.81 μg/ml) followed by aristolone (IC(50) 5.28 μg/ml) and solavetivone (IC(50) 6.82 μg/ml) by DPPH radical scavenging assay. Total antioxidant activity against phosphomolybdenum reagent was also studied. The methods described in this paper were able to identify and quantify sesquiterpenoids from the complex mixtures of phytochemicals and could be extended to the marker based standardization of polyherbal formulations containing C. rotundus. Copyright © 2012 Elsevier B.V. All rights reserved.

  10. Optimization of Extraction Conditions and HPTLC - UV Method for Determination of Quinine in Different Extracts of Cinchona species Bark

    Directory of Open Access Journals (Sweden)

    Dharam C. Jain

    2008-10-01

    Full Text Available A simple, precise and accurate high-performance thin-layer chromatographic method has been established for quantitative determination of quinine. Conditions were also optimized for best possible extraction of quinine via varying concentrations of diethyl amine in different solvents (n-hexane, chloroform, ethyl acetate and methanol for maximum recovery of quinine. Methanol modified with 20 % DEA found to be best for highest possible recovery of target analyte quinine. Chromatographic separation of quinine was performed on silica gel 60 F 254 HPTLC plates with ethyl acetate : diethyl amine in the proportion 88 : 12 (v/v, as mobile phase. The determination was carried out using the densitometric absorbance mode at 236 nm. Quinine response was found to be linear over the range 4–24 μg spot −1. The HPTLC method was evaluated in terms of specificity, precision, reproducibility, LOD – LOQ and robustness. Beside these parameters, number of theoretical plates and flow constant were also included as a part of validation

  11. Rapid quantitative determination of maltose and total sugars in sweet potato (Ipomoea batatas L. [Lam.]) varieties using HPTLC.

    Science.gov (United States)

    Lebot, Vincent

    2017-03-01

    When a raw sweet potato root is analysed, only sucrose, glucose and fructose are present but during cooking, starch is hydrolysed into maltose giving the sweet flavour to cooked roots. This study aimed at developing an HPTLC protocol for the rapid quantitative determination of maltose and total sugars in four commercial varieties and to compare them to 243 hybrids grouped by flesh colour (white, orange, purple). In commercial varieties, mean maltose content varied from 10.26 to 15.60% and total sugars from 17.83 to 27.77% on fresh weight basis. Hybrids showed significant variation in maltose content within each group, with means ranging from 7.65% for white-fleshed, to 8.53% in orange- and 11.98% in purple-fleshed. Total mean sugars content was 20.24, 22.11 and 26.84% respectively for white, orange and purple flesh hybrids. No significant correlations were detected between individual sugars but maltose and total sugars content were highly correlated. Compared to the best commercial variety ( Baby ), 25 hybrids (10.3%) presented a higher maltose content and 40 (16.5%) showed a higher total sugars content. HPTLC was observed as an attractive, cost efficient, high-throughput technique for quantitating maltose and total sugars in sweet potatoes. Perspectives for improving sweet potato quality for consumers' requirements are also discussed.

  12. Solicitation of HPLC and HPTLC Techniques for Determination of Rutin from Polyalthia longifolia Thwaites

    Science.gov (United States)

    Doshi, Gaurav Mahesh; Zine, Sandeep Prabhakar; Chaskar, Pratip Kashinath; Une, Hemant Devidas

    2014-01-01

    Background: Polyalthia longifolia Thwaites is an important traditional plant in India. Rutin, an active constituent has been reported to possess good amount of pharmacological as well as therapeutic potential. Objective: The aim of the present study was to find out by analytical techniques how much percentage of rutin is present in the plant leaves’ ethanolic extract by analytical techniques. Materials and Methods: Shade dried leaves of Polyalthia longifolia were subjected to cold ethanolic extraction followed by monitoring the isolated rutin high-pressure liquid chromatography (HPLC) and high performance thin layer chromatography (HPTLC) after carrying out preliminary phytochemical screening. Results: Extraction yield was found to be 13.94% w/w. Phytochemical screening of the extract showed the presence of flavonoids, steroids, diterpenoids, alkaloids, saponins, tannins and phenolic compounds and mucilage. From the Rf value, the ethanolic extract was found to be having constituent identical to rutin. By HPTLC and HPLC the amount of rutin was found to be 11.60% w/w and 4.03% w/v, respectively. Conclusion: The active constituent isolated was found to be equal to rutin. PMID:25002804

  13. Validated HPTLC Method for Dihydrokaempferol-4'-O-glucopyranoside Quantitative Determination in Alcea Species.

    Science.gov (United States)

    Abdel Salam, Nabil A; Ghazy, Nabila M; Shawky, Eman; Sallam, Shimaa M; Shenouda, Mary L

    2018-07-01

    Dihydrokaempferol-4'-O-glucopyranoside, a flavanonol glucoside, is the major compound in the flower of Alcea rosea L. which possesses significant antioxidant and anticancer activity against HepG-2 cell line and thus can be considered a marker compound for A. rosea L. We attempted to establish a new simple, validated high-performance thin-layer chromatographic (HPTLC) method for the quantitation of dihydrokaempferol-4'-O-glucopyranoside to help in the standardization of the hydroalcoholic extracts of A. rosea L. flowers and to evaluate the best method for its extraction from the plant material. The separation was carried out on an HPTLC aluminum plate pre-coated with silica gel 60F-254, eluted with ethyl acetate-methanol-water-acetic acid (30:5:4:0.15 v/v). Densitometric scanning was performed using a Camag TLC scanner III, at 295 nm. A linear relationship was obtained between the concentrations (0.9-3.6 mg) and peak areas with the correlation coefficient (r) of 0.9971 ± 0.0002. The percentage relative standard deviations of intra-day and inter-day precisions were 0.22-1.45 and 0.49-1.66, respectively. The percentage w/w of dihydrokaempferol-4'-O-glucopyranoside in the flowers of A. rosea L. after maceration and sonication for 15 min was found to be 0.733 g/100 g and 0.928 g/100 g, respectively.

  14. A validated HPTLC method for determination of terbutaline sulfate in biological samples: Application to pharmacokinetic study

    OpenAIRE

    Faiyazuddin, Md.; Rauf, Abdul; Ahmad, Niyaz; Ahmad, Sayeed; Iqbal, Zeenat; Talegaonkar, Sushma; Bhatnagar, Aseem; Khar, Roop K.; Ahmad, Farhan J.

    2011-01-01

    Terbutaline sulfate (TBS) was assayed in biological samples by validated HPTLC method. Densitometric analysis of TBS was carried out at 366 nm on precoated TLC aluminum plates with silica gel 60F254 as a stationary phase and chloroform–methanol (9.0:1.0, v/v) as a mobile phase. TBS was well resolved at RF 0.34 ± 0.02. In all matrices, the calibration curve appeared linear (r2 ⩾ 0.9943) in the tested range of 100–1000 ng spot−1 with a limit of quantification of 18.35 ng spot−1. Drug recovery f...

  15. Determination of flutamide and two major metabolites using HPLC-DAD and HPTLC methods.

    Science.gov (United States)

    Abdelwahab, Nada S; Elshemy, Heba A H; Farid, Nehal F

    2018-01-25

    Flutamide is a potential antineoplastic drug classified as an anti-androgen. It is a therapy for men with advanced prostate cancer, administered orally after which it undergoes extensively first pass metabolism in the liver with the production of several metabolites. These metabolites are predominantly excreted in urine. One of the important metabolites in plasma is 4-nitro-3-(trifluoromethyl)phenylamine (Flu-1), while the main metabolite in urine is 2-amino-5-nitro-4-(trifluoromethyl)phenol (Flu-3). In this work the two metabolites, Flu-1 and Flu-3, have been synthesized, and then structural confirmation has been carried out by HNMR analysis. Efforts were exerted to develop chromatographic methods for resolving Flutamide and its metabolites with the use of acceptable solvents without affecting the efficiency of the methods. The drug along with its metabolites were quantitatively analyzed in pure form, human urine, and plasma samples using two chromatographic methods, HPTLC and HPLC-DAD methods. FDA guidelines for bio-analytical method validation were followed and USP recommendations were used for analytical method validation. Interference from excipients has been tested by application of the methods to pharmaceutical tablets. No significant difference was found between the proposed methods and the official one when they were statistically compared at p value of 0.05%.

  16. Bioanalytical method development and validation for determination of metoprolol tartarate and hydrochlorothiazide using HPTLC in human plasma

    Directory of Open Access Journals (Sweden)

    Ambadas Ranganath Rote

    2013-12-01

    Full Text Available A simple, sensitive, rapid and economic chromatographic method has been developed for determination of metoprolol tartarate and hydrochlorothiazide in human plasma using paracetamol as an internal standard. The analytical technique used for method development was high-performance thin-layer chromatography. HPTLC Camag with precoated silica gel Plate 60F254 (20 cm×10 cm at 250 µm thicknesses (E. Merck, Darmstadt, Germany was used as the stationary phase. The mobile phase used consisted of chloroform: methanol: ammonia (9:1:0.5v/v/v. Densitometric analysis was carried out at a wavelength of 239 nm. The rf values for hydrochlorothiazide, paracetamol and metoprolol tartarate were 0.13±0.04, 0.28±0.05, 0.48±0.04, respectively. Plasma samples were extracted by protein precipitation with methanol. Concentration ranges of 200, 400, 600, 800, 1000, 1200 ng/mL and 2000, 4000, 6000, 8000, 10000, 12000 ng/mL of hydrochlorothiazide and metoprolol tartarate, respectively, were used with plasma for the calibration curves. The percent recovery of metoprolol tartarate and hydrochlorothiazide was found to be 77.30 and 77.02 %, respectively. The stability of metoprolol tartarate and hydrochlorothiazide in plasma were confirmed during three freeze-thaw cycles (-20 ºC on a bench for 24 hours and post-preparatively for 48 hours. The proposed method was validated statistically and proved suitable for determination of metoprolol tartarate and hydrochlorothiazide in human plasma.

  17. Determination of bioactive marker glycyrrhizin in Glycyrrhiza glabra root and commercial formulation by validated HPTLC-densitometric method

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    Perwez Alam

    2014-11-01

    Full Text Available Objective: To develop a simple sensitive high performance thin layer chromatography (HPTLC- densitometric method for quantification of glycyrrhizin in the Glycyrrhiza glabra root methanol extract and licorice root capsule methanol extract. Methods: Chromatography was performed on glass-backed silica gel 60 F254 HPTLC plates with the green solvents ethyl acetate: glacial acetic acid: methanol: water in proportion of 6:2:1:0.5, v/v/ v/v as mobile phase. Scanning and quantification of developed plate was done densitometrically at 254 nm. The method was validated for detection and quantification limits, precision, recovery and robustness according to International Conference on Harmonization guidelines. Results: The system gave compact spot for glycyrrhizin (Rf =0.280±0.001. The regression curve of standard was found to be Y=4.213x+22.078. The limit of detection (15.7 ng per band, limit of quantification (47.1 ng per band, recovery (99.4%-99.8% and precision (≤1.62% and ≤1.84%; intraday and interday were satisfactory for glycyrrhizin. Linearity range for glycyrrhizin was 20- 200 ng (r 2 =0.996. The content of glycyrrhizin was estimated as 5.9% and 11.2% w/w in glycyrrhizin in the Glycyrrhiza glabra root methanol extract and licorice root capsule methanol extract, respectively. Conclusions: This estimation technique is very much useful for the estimation of glycyrrhizin present in various formulations as well as for quality control of crude drugs containing glycyrrhizin.

  18. Simultaneous HPTLC analysis of ursolic acid, betulinic acid, stigmasterol and lupeol for the identification of four medicinal plants commonly available in the Indian market as Shankhpushpi.

    Science.gov (United States)

    Sethiya, Neeraj Kumar; Mishra, Shrihari

    2015-01-01

    In this study, we investigated a new, simple, sensitive, selective and precise high-performance thin-layer chromatography (HPTLC) fingerprint and quantitative estimation method for the analysis of ursolic acid, betulinic acid, stigmasterol and lupeol in Shankhpushpi botanicals. Linear ascending development was carried out in a twin trough glass chamber saturated with petroleum ether-ethyl acetate-toluene (7:2:1, v/v/v). The plate was dried, sprayed with anisaldehyde reagent and analyzed by CAMAG TLC scanner III at 580 nm. The system was found to give compact spots for ursolic acid (0.21), betulinic acid (0.29), stigmasterol (0.33) and lupeol (0.50). The relationship between the concentration of standard solutions and the peak response is linear within the concentration range of 100-600 ng/spot for ursolic acid, betulinic acid, stigmasterol and lupeol. The concentration of 134.2 and 146.1 mg of ursolic acid per gram of Clitorea ternatea (CT) and Canscora decussata (CD); 110.6 mg of betulinic acid per gram of EA; 92.75, 154.95, 31.947 and 39.21 mg of stigmasterol per gram of Evolvulus alsinoides (EA), Convolvulus pluricaulis (CP), CT and CD; 30.12 mg of lupeol per gram of CT were found. The proposed HPTLC method may use for routine quality testing and identification of Shankhpushpi botanicals. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  19. TLC/HPTLC in Biomedical Applications

    Science.gov (United States)

    Mohammad, A.; Moheman, A.

    The main objective of this chapter is to encapsulate the applications of thin-layer chromatography (TLC) and high-performance thin-layer chromatography (HPTLC) as used in the analysis of compounds of pharmaceutical importance. The chapter discusses the advantages of using TLC or HPTLC for biomedical applications and summarizes important information on stationary and mobile phases, adopted methodology, sample application, zone detection, and identification and quantification of amino acids and proteins, carbohydrates, lipids, bile acids, drugs, vitamins, and porphyrins in biological matrices such as blood, urine, feces, saliva, cerebrospinal fluid, body tissues, etc. Among the stationary phases, silica gel has been the most preferred layer material in combination of mixed aqueous- organic or multicomponent organic solvent systems as mobile phase. For quantitative determination of analyte in various matrices, densitometry has been more commonly used. According to the literature survey, the interest of chromatographers in using the TLC/HPTLC has been in the following order: drugs > amino acids and proteins > lipids > bile acids > carbohydrates/vitamins > porphyrins.

  20. Validated HPTLC technique for simultaneous evaluation of biomarkers gallic acid and quercetin in Trichosanthes dioica Roxb.: A systematic approach for quality control of herbals

    Directory of Open Access Journals (Sweden)

    Md. Sarfaraj Hussain

    2017-06-01

    Full Text Available Objective: To investigate the simultaneous quantification of two biologically active elements, flavonoids gallic acid (GA and quercetin (QE, in methanolic extract of Trichosanthes dioica that was customarily used to lower blood sugar and cholesterol. Methods: Silica gel 60F254 having receded with aluminum plate was applied for the separation. We used toluene-ethyl acetate-formic acid (5:4:1, v/v/v as a solvent system for the separation. Results: At 270 nm in reflectance mode densitometric analysis was performed. Squeezed bands for GA and QE were achieved at Rf (0.31 ± 0.03 and (0.50 ± 0.02. The scheme was validated for sensitivity, specificity, limit of detection and quantification. Linear relationship was found between the concentration range of 100–1 000 ng spot–1 for GA and 150–900 ng spot–1 for GA and QE, respectively. The instrumental precision was noted to be 1.03–1.96 (% RSD and 1.09–1.98 (% RSD for GA and QE, separately. Methodology specificity was determined at three different study point with varying concentration for recovery studies. Mean % recovery was noted to be 99.4%–99.9% and 98.7%–99.3% and the content estimated as (31.00 ± 1.18% and (39.00 ± 1.24% for GA and QE, respectively. Conclusions: The developed high performance thin layer chromatography scheme can be used for routine quality control analysis of Trichosanthes dioica and several other formulations containing these markers.

  1. HPTLC in Herbal Drug Quantification

    Science.gov (United States)

    Shinde, Devanand B.; Chavan, Machindra J.; Wakte, Pravin S.

    For the past few decades, compounds from natural sources have been gaining importance because of the vast chemical diversity they offer. This has led to phenomenal increase in the demand for herbal medicines in the last two decades and need has been felt for ensuring the quality, safety, and efficacy of herbal drugs. Phytochemical evaluation is one of the tools for the quality assessment, which include preliminary phytochemical screening, chemoprofiling, and marker compound analysis using modern analytical techniques. High-performance thin-layer chromatography (HPTLC) has been emerged as an important tool for the qualitative, semiquantitative, and quantitative phytochemical analysis of the herbal drugs and formulations. This includes developing TLC fingerprinting profiles and estimation of biomarkers. This review has an attempt to focus on the theoretical considerations of HPTLC and some examples of herbal drugs and formulations analyzed by HPTLC.

  2. HPTLC Hyphenated with FTIR: Principles, Instrumentation and Qualitative Analysis and Quantitation

    Science.gov (United States)

    Cimpoiu, Claudia

    In recent years, much effort has been devoted to the coupling of high-performance thin-layer chromatography (HPTLC) with spectrometric methods because of the robustness and simplicity of HPTLC and the need for detection techniques that provide identification and determination of sample constituents. IR is one of the spectroscopic methods that have been coupled with HPTLC. IR spectroscopy has a high potential for the elucidation of molecular structures, and the characteristic absorption bands can be used for compound-specific detection. HPTLC-FTIR coupled method has been widely used in the modern laboratories for the qualitative and quantitative analysis. The potential of this method is demonstrated by its application in different fields of analysis such as drug analysis, forensic analysis, food analysis, environmental analysis, biological analysis, etc. The hyphenated HPTLC-FTIR technique will be developed in the future with the aim of taking full advantage of this method.

  3. Development and Validation of a HPTLC Method for Simultaneous Estimation of L-Glutamic Acid and γ-Aminobutyric Acid in Mice Brain.

    Science.gov (United States)

    Sancheti, J S; Shaikh, M F; Khatwani, P F; Kulkarni, Savita R; Sathaye, Sadhana

    2013-11-01

    A new robust, simple and economic high performance thin layer chromatographic method was developed for simultaneous estimation of L-glutamic acid and γ-amino butyric acid in brain homogenate. The high performance thin layer chromatographic separation of these amino acid was achieved using n-butanol:glacial acetic acid:water (22:3:5 v/v/v) as mobile phase and ninhydrin as a derivatising agent. Quantitation of the method was achieved by densitometric method at 550 nm over the concentration range of 10-100 ng/spot. This method showed good separation of amino acids in the brain homogenate with Rf value of L-glutamic acid and γ-amino butyric acid as 21.67±0.58 and 33.67±0.58, respectively. The limit of detection and limit of quantification for L-glutamic acid was found to be 10 and 20 ng and for γ-amino butyric acid it was 4 and 10 ng, respectively. The method was also validated in terms of accuracy, precision and repeatability. The developed method was found to be precise and accurate with good reproducibility and shows promising applicability for studying pathological status of disease and therapeutic significance of drug treatment.

  4. Simultaneous Determination of Seven Constituents in Herbal ...

    African Journals Online (AJOL)

    Simultaneous Determination of Seven Constituents in Herbal Prescription Jaeumganghwa-Tang Using HPLC-PDA. CS Seo, JH Kim, HK Shin. Abstract. A simple and accurate high-performance liquid chromatographic method was applied to the quantitative analysis of seven components of the traditional herbal prescription ...

  5. Simultaneous Spectrophotometric Determination of Valsartan and ...

    African Journals Online (AJOL)

    Purpose: To develop a direct, simple and extraction-free spectrophotometric method for the simultaneous estimation of valsartan and ezetimibe in pharmaceuticals. Methods: A spectrophotometric method for the determination of valsartan and ezetimibe was developed using acidic dyes, namely, bromophenol blue (BPB) ...

  6. Simultaneous Determination of Amlodipine and Valsartan

    OpenAIRE

    Mohamed, Nashwah Gadallah

    2011-01-01

    A spectrophotometric method was developed for simultaneous determination of amlodipine (Aml) and valsartan (Val) without previous separation. In this method amlodipine in methanolic solution was determined using zero order UV spectrophotometry by measuring its absorbency at 360.5 nm without any interference from valsartan. Valsartan spectrum in zero order is totally overlapped with that of amlodipine. First, second and third derivative could not resolve the overlapped peaks. The first derivat...

  7. Development and validation of High-performance Thin-layer Chromatography Method for Simultaneous Determination of Polyphenolic Compounds in Medicinal Plants.

    Science.gov (United States)

    Jayachandran Nair, C V; Ahamad, Sayeed; Khan, Washim; Anjum, Varisha; Mathur, Rajani

    2017-12-01

    Quantitative standardization of plant-based products is challenging albeit essential to maintain their quality. This study aims to develop and validate high-performance thin-layer chromatography (HPTLC) method for the simultaneous determination of rutin (Ru), quercetin (Qu), and gallic acid (Ga) from Psidium guajava Linn. (PG) and Aegle marmelos (L.) Correa. (AM) and correlate with antioxidant activity. The stock solution (1 mg/mL) of standard Ru, Qu, and Ga in methanol: Water (1:1) was serially diluted and spotted (5 μL) on slica gel 60 F 254 thin-layer chromatography plates. Toluene: Ethyl acetate: Formic acid: Methanol (3:4:0.8:0.7, v/v/v) was selected as mobile phase for analysis at 254 nm. Hydroalcoholic (1:1) extracts of leaves of PG and AM were fractionated and similarly analyzed. Antioxidant activity was also determined using 2, 2-diphenyl-1-picrylhydrazyl assay. The developed method was robust and resolved Ru, Qu, and Ga at R f 0.08 ± 0.02, 0.76 ± 0.01, and 0.63 ± 0.02, respectively. The intra-day, interday precision, and interanalyst were limit of detection and limit of quantification for Ru, Qu, and Ga were 4.51, 4.2, 5.27, and 13.67, 12.73, 15.98 ng/spot, respectively. Antioxidant activity (Log 50% inhibition) of PG and AM was 4.947 ± 0.322 and 6.498 ± 0.295, respectively. The developed HPTLC method was rapid, accurate, precise, reproducible, and specific for the simultaneous estimation of Ru, Qu, and Ga. HPTLC method for simultaneous determination and quantification of Rutin, Quercetin and Gallic acid, is reported for quality control of herbal drugs. Abbreviations Used: A: Aqueous fraction; AM: Aegle marmelos L. Correa; B: Butanol fraction; C: Chloroform fraction; EA: Ethyl acetate fraction; Ga: Gallic acid; H: Hexane fraction; HA: Hydroalcoholic extract; HPTLC: High-performance thin-layer chromatography; PG: Psidium guajava ; Qu: Quercetin; Ru: Rutin.

  8. HPTLC methods for the Rapid Determination of Adhatoda vasica L. Glycyrrhiza glabbra L., Phyllanthus embelica L. and Camellia sinensis L. in a polyherbal formulation (INSTY)

    International Nuclear Information System (INIS)

    Sheikh, Z. A.; Zahoor, A.; Shafiq, K.; Usmanghani, K.; Khan, S. S.; Khan, A.

    2015-01-01

    An Insty Granule is a polyherbal formulation, and it is widely used to treat upper respiratory tract infections. It contains expectorant, anti-inflammatory, mucolytic and anti-pyretic properties. The major active constituents are vasicine, gallic acid, caffeine and glycyrrhizin. Insty a poly herbal formulation of eight herbs were investigated for its phytochemical evaluation. Biomarkers of about four herbs both qualitatively and quantitatively were investigated. Methods: The solvent systems used were ethyl acetate, chloroform, ethanol, ammonia (6: 3: 1: 1) for vasicin, ethyl acetate, chloroform, formic acid (12: 15: 3) for gallic acid, ethyl acetate, methanol, water (100: 13.5: 10) for caffeine, and methanol, water, acetic acid (70: 30: 0.5) for glycyrrhizin. Results: The methods showed a good linear relationship (r/sup 2/ = 0.999) in the concentration range 25-1500 ng per spot. It was found to be linear, accurate, precise, specific, robust and can be applied for quality control and standardization. Conclusion: In present study rapid and inexpensive qualification methods for the quality control of Adhatoda vasica L. Glycyrrhiza glabbra L., Phyllanthus embelica L. and Camellia sinensis L. on thin layer chromatography (TLC) were developed and validated on silica gel. HPTLC is most suitable technique because of quantification of number of samples at low operating cost, easy sample preparation, short analysis time and analytical assurance. (author)

  9. Simultaneous determination of protein structure and dynamics

    DEFF Research Database (Denmark)

    Lindorff-Larsen, Kresten; Best, Robert B.; DePristo, M. A.

    2005-01-01

    at the atomic level about the structural and dynamical features of proteins-with the ability of molecular dynamics simulations to explore a wide range of protein conformations. We illustrate the method for human ubiquitin in solution and find that there is considerable conformational heterogeneity throughout......We present a protocol for the experimental determination of ensembles of protein conformations that represent simultaneously the native structure and its associated dynamics. The procedure combines the strengths of nuclear magnetic resonance spectroscopy-for obtaining experimental information...... the protein structure. The interior atoms of the protein are tightly packed in each individual conformation that contributes to the ensemble but their overall behaviour can be described as having a significant degree of liquid-like character. The protocol is completely general and should lead to significant...

  10. Simultaneous Mass Determination for Gravitationally Coupled Asteroids

    Energy Technology Data Exchange (ETDEWEB)

    Baer, James [Private address, 3210 Apache Road, Pittsburgh, PA 15241 (United States); Chesley, Steven R., E-mail: jimbaer1@earthlink.net [Jet Propulsion Laboratory, California Institute of Technology, 4800 Oak Grove Drive, Pasadena, CA 91109 (United States)

    2017-08-01

    The conventional least-squares asteroid mass determination algorithm allows us to solve for the mass of a large subject asteroid that is perturbing the trajectory of a smaller test asteroid. However, this algorithm is necessarily a first approximation, ignoring the possibility that the subject asteroid may itself be perturbed by the test asteroid, or that the encounter’s precise geometry may be entangled with encounters involving other asteroids. After reviewing the conventional algorithm, we use it to calculate the masses of 30 main-belt asteroids. Compared to our previous results, we find new mass estimates for eight asteroids (11 Parthenope, 27 Euterpe, 51 Neimausa, 76 Freia, 121 Hermione, 324 Bamberga, 476 Hedwig, and 532 Herculina) and significantly more precise estimates for six others (2 Pallas, 3 Juno, 4 Vesta, 9 Metis, 16 Psyche, and 88 Thisbe). However, we also find that the conventional algorithm yields questionable results in several gravitationally coupled cases. To address such cases, we describe a new algorithm that allows the epoch state vectors of the subject asteroids to be included as solve-for parameters, allowing for the simultaneous solution of the masses and epoch state vectors of multiple subject and test asteroids. We then apply this algorithm to the same 30 main-belt asteroids and conclude that mass determinations resulting from current and future high-precision astrometric sources (such as Gaia ) should conduct a thorough search for possible gravitational couplings and account for their effects.

  11. Simultaneous Mass Determination for Gravitationally Coupled Asteroids

    Science.gov (United States)

    Baer, James; Chesley, Steven R.

    2017-08-01

    The conventional least-squares asteroid mass determination algorithm allows us to solve for the mass of a large subject asteroid that is perturbing the trajectory of a smaller test asteroid. However, this algorithm is necessarily a first approximation, ignoring the possibility that the subject asteroid may itself be perturbed by the test asteroid, or that the encounter’s precise geometry may be entangled with encounters involving other asteroids. After reviewing the conventional algorithm, we use it to calculate the masses of 30 main-belt asteroids. Compared to our previous results, we find new mass estimates for eight asteroids (11 Parthenope, 27 Euterpe, 51 Neimausa, 76 Freia, 121 Hermione, 324 Bamberga, 476 Hedwig, and 532 Herculina) and significantly more precise estimates for six others (2 Pallas, 3 Juno, 4 Vesta, 9 Metis, 16 Psyche, and 88 Thisbe). However, we also find that the conventional algorithm yields questionable results in several gravitationally coupled cases. To address such cases, we describe a new algorithm that allows the epoch state vectors of the subject asteroids to be included as solve-for parameters, allowing for the simultaneous solution of the masses and epoch state vectors of multiple subject and test asteroids. We then apply this algorithm to the same 30 main-belt asteroids and conclude that mass determinations resulting from current and future high-precision astrometric sources (such as Gaia) should conduct a thorough search for possible gravitational couplings and account for their effects.

  12. Simultaneous Mass Determination for Gravitationally Coupled Asteroids

    International Nuclear Information System (INIS)

    Baer, James; Chesley, Steven R.

    2017-01-01

    The conventional least-squares asteroid mass determination algorithm allows us to solve for the mass of a large subject asteroid that is perturbing the trajectory of a smaller test asteroid. However, this algorithm is necessarily a first approximation, ignoring the possibility that the subject asteroid may itself be perturbed by the test asteroid, or that the encounter’s precise geometry may be entangled with encounters involving other asteroids. After reviewing the conventional algorithm, we use it to calculate the masses of 30 main-belt asteroids. Compared to our previous results, we find new mass estimates for eight asteroids (11 Parthenope, 27 Euterpe, 51 Neimausa, 76 Freia, 121 Hermione, 324 Bamberga, 476 Hedwig, and 532 Herculina) and significantly more precise estimates for six others (2 Pallas, 3 Juno, 4 Vesta, 9 Metis, 16 Psyche, and 88 Thisbe). However, we also find that the conventional algorithm yields questionable results in several gravitationally coupled cases. To address such cases, we describe a new algorithm that allows the epoch state vectors of the subject asteroids to be included as solve-for parameters, allowing for the simultaneous solution of the masses and epoch state vectors of multiple subject and test asteroids. We then apply this algorithm to the same 30 main-belt asteroids and conclude that mass determinations resulting from current and future high-precision astrometric sources (such as Gaia ) should conduct a thorough search for possible gravitational couplings and account for their effects.

  13. Experimental Aspects and Implementation of HPTLC

    Science.gov (United States)

    Patel, Rashmin B.; Patel, Mrunali R.; Batel, Bharat G.

    High-Performance Thin-Layer Chromatography (HPTLC) is a sophisticated instrumentation technique. It has been reported in many publications to provide excellent separation and qualitative and quantitative analysis of a wide range of compounds, such as herbal and botanical dietary supplements, nutraceuticals, traditional western medicines, traditional Chinese medicines, and Ayurvedic (Indian) medicines (Sharma 2008). Comparative studies have often found that HPTLC is superior to High-Performance Liquid Chromatography (HPLC) in terms of total cost and time required for analysis. HPTLC is an off-line process in which the various stages are carried out independently. Important features of HPTLC are the ability to analyze cruder samples containing multicomponents; application of large number of sample and a series of standards using the spray-on technique; choice of solvents for the HPTLC development is wide as the mobile phases are fully evaporated before the detection step; processing of standards and samples identically on the same plate, leading to better accuracy and precision of quantification; different and universal selective detection methods, and in situ spectra recording in sequence to obtain positive identification of fractions; storage of total sample on layer, without time constrains. In addition, it minimizes exposure risks and significantly reduces disposal problems of toxic organic effluents; thereby, reduce possibilities of environment pollution. In view of this, HPTLC-based methods could be considered as a good alternative as they are being explored as an important tool in routine analysis. This chapter provides detailed information regarding HPTLC-based analytical method development (Renger 1993; Renger 1998; Patel and Patel 2008; Patel et al. 2010).

  14. High-performance thin-layer chromatography (HPTLC)

    National Research Council Canada - National Science Library

    Srivastava, ManMohan

    2011-01-01

    ... on HPTLC fundamentals: principle, theory, understanding; instrumentation: implementation, optimization, validation, automation and qualitative and quantitative analysis; applications: phytochemical analysis, biomedical analysis, herbal drug quantification, analytical analysis, finger print analysis and potential for hyphenation: HPTLC future to combinat...

  15. Simultaneous Determination of Mutagenicity and Toxicity of ...

    African Journals Online (AJOL)

    A demonstration of cytotoxicity is required (measurement of cell number, culture confluency and inhibition of mitotic index) for in vitro cytogenetic assays. The study therefore investigated whether delayed cytotoxicity can be used to simultaneously predict mutagenicity and cytotoxicty. Chinese hamster lung cells were ...

  16. Simultaneous determination of isoniazid and pyrazinamide in ...

    African Journals Online (AJOL)

    Finally, 20 µL was injected into the HPLC system. HPLC analysis ... The method was accurate, and relative error ... Keywords: HPLC, Isoniazid, Pyrazinamide, Plasma, Simultaneous analysis. Tropical ... work, we describe a new HPLC method with UV ... pooled human plasma. ..... License, which permits unrestricted use,.

  17. Simultaneous Determination of Ciprofloxacin and Tinidazole in ...

    African Journals Online (AJOL)

    Purpose: To develop a simple, sensitive and specific liquid chromatographic method with PDA detection for the simultaneous estimation of ciprofloxacin and tinidazole in tablet dosage form. Methods: Separation was achieved with an Agilent XDB C18, 250 × 4.60 mm 5 μ column, low pressure gradient mode with a ambient ...

  18. Simultaneous determination of atorvastatin calcium and olmesartan medoxomil in a pharmaceutical formulation by reversed phase high-performance liquid chromatography, high-performance thin-layer chromatography, and UV spectrophotometric methods.

    Science.gov (United States)

    Soni, Hiral; Kothari, Charmy; Khatri, Deepak; Mehta, Priti

    2014-01-01

    Validated RP-HPLC, HPTLC, and UV spectrophotometric methods have been developed for the simultaneous determination of atorvastatin calcium (ATV) and olmesartan medoxomil (OLM) in a pharmaceutical formulation. The RP-HPLC separation was achieved on a Kromasil C18 column (250 x 4.6 mm, 5 microm particle size) using 0.01 M potassium dihydrogen o-phosphate (pH 4 adjusted with o-phosphoric acid)-acetonitrile (50 + 50, v/v) as the mobile phase at a flow rate of 1.5 mL/min. Quantification was achieved by UV detection at 276 nm. The HPTLC separation was achieved on precoated silica gel 60F254 plates using chloroform-methanol-acetonitrile (4 + 2+ 4, v/v/v) mobile phase. Quantification was achieved with UV detection at 276 nm. The UV-Vis spectrophotometric method was based on the simultaneous equation method that involves measurement of absorbance at two wavelengths, i.e., 255 nm (lambda max of OLM) and 246.2 nm (lambda max of ATV) in methanol. All three methods were validated as per International Conference on Harmonization guidelines. The proposed methods were simple, precise, accurate, and applicable for the simultaneous determination of ATV and OLM in a marketed formulation. The results obtained by applying the proposed methods were statistically analyzed and were found satisfactory.

  19. Densitometric HPTLC quantification of asiaticoside isolated from ...

    African Journals Online (AJOL)

    Asiaticoside isolated from Centella asiatica has been found through in vitro test to serve as an active agent of healing on wounds. To quantify this compound in Centella asiatica cultivated in Benin, a new, simple and rapid High-Performance Thin-Layer Chromatography (HPTLC) method was developed and validated for its ...

  20. Simultaneous Determination of Famotidine and Flurbiprofen by High ...

    African Journals Online (AJOL)

    Purpose: To develop a selective, sensitive and accurate simultaneous High Performance Liquid Chromatography (HPLC) method for the analysis of flurbiprofen and famotidine tablet dosage form and excipients. Methods: A simultaneous method for the determination of the two drugs was employed. The assay consisted of ...

  1. Simultaneous Determination of Two Isomers of Asarone in Piper ...

    African Journals Online (AJOL)

    Simultaneous Determination of Two Isomers of Asarone in Piper sarmentosum Roxburgh (Piperaceae) Extracts using Different Chromatographic Columns. Mohd Shahrul Ridzuan Hamil, Abdul Hakeem Memon, Amin Malik Shah Abdul Majid, Zhari Ismail ...

  2. Simultaneous determination of ten compounds in two main ...

    African Journals Online (AJOL)

    Simultaneous determination of ten compounds in two main medicinal plant parts of Tibetan herb, Pterocephalus hookeri (CB Clarke) Höeck, by ultra-high performance liquid chromatography-photodiode array.

  3. Development of Validated High-performance Thin-layer Chromatography Method for Simultaneous Determination of Quercetin and Kaempferol in Thespesia populnea.

    Science.gov (United States)

    Panchal, Hiteksha; Amin, Aeshna; Shah, Mamta

    2017-01-01

    Thespesia populnea L. (Family: Malvaceae) is a well-known medicinal plant distributed in tropical regions of the world and cultivated in South Gujarat and indicated to be useful in cutaneous affections, psoriasis, ringworm, and eczema. Bark and fruits are indicated in the diseases of skin, urethritis, and gonorrhea. The juice of fruits is employed in treating certain hepatic diseases. The plant is reported to contain flavonoids, quercetin, kaempferol, gossypetin, Kaempferol-3-monoglucoside, β-sitosterol, kaempferol-7-glucoside, and gossypol. T. populnea is a common component of many herbal and Ayurvedic formulation such as Kamilari and Liv-52. The present study aimed at developing validated and reliable high-performance thin layer chromatography (HPTLC) method for the analysis of quercetin and kaempferol simultaneously in T. populnea . The method employed thin-layer chromatography aluminum sheets precoated with silica gel as the stationary phase and toluene: ethyl acetate: formic acid (6:4:0.3 v/v/v) as the mobile phase, which gave compact bands of quercetin and kaempferol. Linear regression data for the calibration curves of standard quercetin and kaempferol showed a good linear relationship over a concentration range of 100-600 ng/spot and 500-3000 ng/spot with respect to the area and correlation coefficient (R2) was 0.9955 and 0.9967. The method was evaluated regarding accuracy, precision, selectivity, and robustness. Limits of detection and quantitation were recorded as 32.06 and 85.33 ng/spot and 74.055 and 243.72 ng/spot for quercetin and kaempferol, respectively. We concluded that this method employing HPTLC in the quantitative determination of quercetin and kaempferol is efficient, simple, accurate, and validated.

  4. Simultaneous determination of radium and uranium in soil

    International Nuclear Information System (INIS)

    Yamamoto, Takashi; Yuki, Eiji; Ishida, Tatsuo

    1977-01-01

    Radium and uranium contents in soil are the fundamental indexes for natural radioactivity. In this connection, the simultaneous determination of Ra and U has been studied. To a soil sample, 133 Ba is added and the mixture is dried. It is decomposed with sulfuric and nitric acids. Then a Ba-carrier is added, and the insoluble residue (Ra analysis sample) and the solution (U analysis sample) are obtained for simultaneous determination of Ra and U. The rates of recovery of Ra and U in soil are both over 90%. (Mori, K.)

  5. Simultaneous determination of plutonium and uranium in environmental samples

    International Nuclear Information System (INIS)

    Jiao Shufen

    1993-01-01

    Plutonium and uranium in a plant sample ash was simultaneously determined by using anion exchange resin columns, and concentrated hydrochloric acid and nitric acid. At the final stage of the determination of the nuclides, each of them was electrodeposited together with a little amount of molybdenum carrier onto a stainless steel plate and measured by α-ray spectrometer. The recoveries of uranium and plutonium from the plant samples determined by adding internal standard 236 Pu which was 100% and 63%, respectively

  6. Simultaneous Determination of Flavonols and Terpene Lactones in ...

    African Journals Online (AJOL)

    Purpose: To develop an ultra-performance liquid chromatography-tandem mass spectrometry (UPLCMS/MS) method for the simultaneous determination of 7 major components of Ginkgo leaf (kaempferol, quercetin, isorhamnetin, ginkgolides A, ginkgolides B, ginkgolides C and bilobalide) in dog plasma. Methods: Beagle ...

  7. Simultaneous Determination of Metals in Coal with Low-Resolution ...

    African Journals Online (AJOL)

    The setup including low-resolution spectrometer with the charge-coupled device (CCD) detector, continuum radiation source and filter furnace (FF) atomizer was employed for direct simultaneous determination of Al, Fe, Mg, Cu and Mn in coal slurry. In the FF, sample vapour entered absorption volume by filtering through ...

  8. Radioenzymatic simultaneous determination of epinephrine and norepinephrine in plasma

    International Nuclear Information System (INIS)

    Mueller, T.

    1978-01-01

    The high-pressure liquid chromatography (= HPLC) was used in simultaneous determinations of a few pg epinephrine and norepinephrine. This separation procedure improves the efficiency when compared with the conventional thin-layer chromatographic methods (TLC) and allows routine assays in plasma. (orig.) [de

  9. Comparison of methods by TLC and HPTLC for determination of aflatoxin M1 in milk and B1 in eggs Comparação de metodologia para análise de aflatoxina M1 em leite e aflatoxina B1 em ovos por CCD e CCDAE

    Directory of Open Access Journals (Sweden)

    V. M. Scussel

    2003-12-01

    Full Text Available Milk and egg matrixes were assayed for aflatoxin M1 (AFM1 and B1 (AFB1 respectively, by AOAC official and modified methods with detection and quantification by thin layer chromatography (TLC and high performance thin layer chromatography (HPTLC. The modified methods: Blanc followed by Romer, showed to be most appropriate for AFM1 analysis in milk. Both methods reduced emulsion formation, produced cleaner extracts, no streaking spots, precision and accuracy improved, especially when quantification was performed by HPTLC. The use of ternary mixture in the Blanc Method was advantageous as the solvent could extract AFM1 directly from the first stage (extraction, leaving other compounds in the binary mixture layer, avoiding emulsion formation, thus reducing toxin loss. The relative standard deviation (RSD% values were low, 16 and 7% when TLC and HPTLC were used, with a mean recovery of 94 and 97%, respectively. As far as egg matrix and final extract are concerned, both methods evaluated for AFB1 need further studies. Although that matrix leads to emulsion with consequent loss of toxin, the Romer modified presented a reasonable clean extract (mean recovery of 92 and 96% for TLC and HPTLC, respectively. Most of the methods studied did not performed as expected mainly due to the matrixes high content of triglicerides (rich on saturated fatty acids, cholesterol, carotene and proteins. Although nowadays most methodology for AFM1 is based on HPLC, TLC determination (Blanc and Romer modified for AFM1 and AFB1 is particularly recommended to those, inexperienced in food and feed mycotoxins analysis and especially who cannot afford to purchase sophisticated (HPLC,HPTLC instrumentation.Aflatoxinas M1 (AFM1 e B1 (AFB1 foram analisadas em leite e ovos respectivamente, por diferentes métodos oficiais da AOAC e modificações usando detecção por cromatografia em camada delgada (CCD e CCD de alta eficiência (CCDAE. Os métodos modificados: Blanc e Romer

  10. Box-Behnken design for optimum extraction of biogenetic chemicals from P. lanceolata with an energy audit (thermal × microwave × acoustic): a case study of HPTLC determination with additional specificity using on-line/off-line coupling with DAD/NIR/ESI-MS.

    Science.gov (United States)

    Srivastava, Pooja; Ajayakumar, P V; Shanker, Karuna

    2014-01-01

    The genus Pluchea comprises about 80 species distributed worldwide, out of them, only Pluchea lanceolata (DC.) Oliv. & Hiern, is used extensively in the traditional system of India. No chromatographic method is available for its quality. To perform the energy audit for the extraction of biogenetic pentacyclic triterpene, its acetate and sterol from P. lanceolata utilising organic and four alternative solvents. Additionally to resolve the uncertainty of TLC determination, on-line/off-line coupling with a diode-array detector (DAD), and near-infrared (NIR) and electrospray ionisation (ESI) MS was introduced. The extraction of taraxasterol (Tx), taraxasterol acetate (TxAc) and stigmasterol (St) from P. lanceolata was performed using three energy modes. The effects of different operating parameters were studied for optimum extraction yield using the design of experiments, that is, the central composite design and Box-Behnken design. In addition to the retention factor (Rf ) and visible spectral matching, two additional optical spectroscopic techniques, that is, NIR and ESI-MS, were applied for extended specificity. The method was developed for Tx, TxAc and St determination using HPTLC at 645 nm. The optimum extraction yield of targeted compounds was found to be higher with organic solvents than eco-friendly surfactants. The pulse ultrasonic assisted extraction (PUAE) has resulted in optimum extraction of compounds comparable to hot extraction. Both NIR and ESI-MS provided extended specificity in determination. The 5/1-PUAE was determined to be effective, reproducible, simple and energy efficient for the determination of Tx, TxAc and St in P. lanceolata. The offline coupling of NIR and ESI-MS with HPTLC led to considerable improvement in specificity. Copyright © 2014 John Wiley & Sons, Ltd.

  11. Analysis of passion fruit rinds (Passiflora edulis: isoorientin quantification by HPTLC and evaluation of antioxidant (radical scavenging capacity

    Directory of Open Access Journals (Sweden)

    Maria Luiza Zeraik

    2012-01-01

    Full Text Available The content of isoorientin in passion fruit rinds (Passiflora edulis fo. flavicarpa O. Degener was determined by HPTLC (high performance thin layer chromatography with densitometric analysis. The results revealed a higher amount of isoorientin in healthy rinds of P. edulis (92.275 ± 0.610 mg L-1 than in rinds with typical symptoms of PWV (Passion fruit Woodiness Virus infection (28.931 ± 0.346 mg L-1. The HPTLC data, allied to assays of radical scavenging activity, suggest the potential of P. edulis rinds as a natural source of flavonoids or as a possible functional food.

  12. Simultaneous spectrophotometric determination of tungsten and molybdenum with dithiol

    International Nuclear Information System (INIS)

    Navale, A.S.

    1987-01-01

    Toluene-3,4-dithiol is a very sensitive reagent for the spectrophotometric determination of tungsten and molybdenum. Since the absorption spectra of the dithiol complexes of these two elements overlap, a separation of the two elements is carried out. This leads to time consuming extraction procedures. Measuring the absorption of the mixed complexes at two wavelengths and solving a set of simultaneous equations is also not favorable because a lot of time and effort is required for solving the simultaneous equations for each sample. A faster and simpler method is described here for the simultaneous determination of the two elements. The method is based on measurement of absorbance of the mixed complexes at three pre-selected wavelengths and simple calculations involving the absorbance differences. The criteria for selecting the three wavelengths and the theory are described. Application of the method for the determination of tungsten and molybdenum in ore samples is presented. The method is applicable to any similar system consisting of two interfering components. 4 figures, 2 tables, 6 refs. (author)

  13. Simultaneous Determination of Glass Transition Temperatures of Several Polymers.

    Science.gov (United States)

    He, Jiang; Liu, Wei; Huang, Yao-Xiong

    2016-01-01

    A simple and easy optical method is proposed for the determination of glass transition temperature (Tg) of polymers. Tg was determined using the technique of microsphere imaging to monitor the variation of the refractive index of polymer microsphere as a function of temperature. It was demonstrated that the method can eliminate most thermal lag and has sensitivity about six fold higher than the conventional method in Tg determination. So the determined Tg is more accurate and varies less with cooling/heating rate than that obtained by conventional methods. The most attractive character of the method is that it can simultaneously determine the Tg of several polymers in a single experiment, so it can greatly save experimental time and heating energy. The method is not only applicable for polymer microspheres, but also for the materials with arbitrary shapes. Therefore, it is expected to be broadly applied to different fundamental researches and practical applications of polymers.

  14. Method for the simultaneous determination of nitrogen, phosphorus and potassium

    International Nuclear Information System (INIS)

    Srapeniants, R.A.; Saveliev, I.B.; Kovtun, J.L.; Sidorov, A.V.; Tsagolov, K.S.

    1980-01-01

    A method for the simultaneous determination of the nitrogen, phosphorus and potassium contents of materials containing them, such as vegetable materials and fertilisers, comprises exposing samples to be analysed and standard samples to neutron irradiation, recording the spectra of gamma radiation induced in the samples, laying the samples aside for a period of time determined by the half-life of the gamma ray-emitting isotopes, again recording the spectra of the samples being analysed and those of the standard samples, superimposing the first and second spectra of the samples being analysed and standard samples and shifting them relative to each other along the energy axis, and determining the content of the elements being analysed by comparing the spectra of the samples being analysed with those of the standard samples. (author)

  15. Simultaneous determination of inorganic and organic anions by ion chromatography

    International Nuclear Information System (INIS)

    Park, Yang Soon; Joe, Ki Soo; Han, Sun Ho; Park, Soon Dal; Choi, Kwang Soon

    1999-06-01

    Four methods were investigated for the simultaneous determination of several inorganic and organic anions in aqueous solution by ion chromatography. The first is two columns coupled system. The second is the gradient elution system with an anion exchange column. The third is the system with a mixed-mode stationary phase. The fourth is the system with an anion exchange column and the eluant of low conductivity without ion suppressor. The advantages and disadvantages of individual systems were discussed. The suitable methods were proposed for the application to the samples of the nuclear power industry and the environment. (author)

  16. Simultaneous determination of left ventricular perfusion and function

    International Nuclear Information System (INIS)

    Gremillet, E.; Champailler, A.; Esquerre, J.P.; Ouhayoun, E.; Coca, F.; Furber, A.; Le Jeune, J.J.

    1997-01-01

    Myocardial perfusion scintigraphy is a very useful tool for the diagnosis and prognosis of coronary artery disease. The evaluation of left ventricular function during stress testing in also very useful to determine the prognosis of coronary artery disease. This chapter highlights three different imaging methods to assess left ventricular function and myocardial perfusion/ The first one consists of sequential dual isotope myocardial SPECT with ECG-gating. The second concerns magnetic resonance imaging and the third explores first pass exercise ventriculography and myocardial perfusion scintigraphy simultaneously evaluated by means of 99m Tc-sestamibi. (authors)

  17. Free radical scavenging potential and HPTLC analysis of Indigofera tinctoria linn (Fabaceae

    Directory of Open Access Journals (Sweden)

    Sakthivel Srinivasan

    2016-04-01

    Full Text Available The objective of this study was to evaluate the free radical scavenging potential and high performance thin layer chromatography (HPTLC fingerprinting of Indigofera tinctoria (I. tinctoria. Phytochemical analysis was carried out using standard methods, and free radical scavenging activity of the plant was determined using 2,2-diphenyl-1-picrylhydrazy (DPPH, nitric oxide (NO and superoxide anion (O2− radical scavenging capacities. HPTLC plate was kept in CAMAG TLC Scanner 3 and the Rf values at fingerprint data were recorded by WINCATS software. Aqueous extract of I. tinctoria reliably showed the total phenolics (267.2±2.42 mg/g, flavonoids (75.43±3.36 mg/g and antioxidants (349.11±8.04 mg/g. The extract was found to have DPPH (52.08%, NO (23.12% and O2− (26.79% scavenging activities at the concentration of 250 μg/mL and the results were statistically significant compared with ascorbic acid standard (p<0.05. HPTLC results confirmed that the extract contained several potential active components such as phenols, flavonoids, saponins and terpenoids as the slides revealed multi-colored bands of varying intensities. This study confirmed that the plant had multipotential antioxidant and free radicals scavenging activities.

  18. Simultaneous determination of actinides by x-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Cohen, V.H.

    1990-01-01

    The x-ray spectrometric simultaneous determination of uranium and plutonium in simulated Purex Process solutions is described. The method is accomplished by intensity measurements of the L α sub(1) lines. The thin film technique for sample preparation and thorium as an internal standard had been used. An evaporation technique had been also tested for low concentration uranium solutions. In the measurement range 0,05 - 130 U g/L, 0,5 - 20 Pu g/L linear calibration curves were effected. The standard deviation in the concentration range 10 to 130 g/L was 3,5%, 4% in the 1 to 10 g/L and 13% in 0,05 to 1 g/L for uranium determination and 4% for plutonium determination in the range of 1 to 20 g/L. The sensitivity of the method was about 3,62 μg to U and 3,95 μg to Pu. Uranium and plutonium do not reciprocally interfere with one another until U/Pu ≅ 90 m/m. The fission product as interfering elements were also verified. Finally, uranium and plutonium were determined in simulated Purex Process solutions within the requested accuracy for control method. (author)

  19. Simultaneous determination of U and Pu isotopes by alpha spectrometry

    International Nuclear Information System (INIS)

    Equillor, H.E.; Campos, J.M.

    2011-01-01

    Determination of actinides by alpha spectrometry is usually carried out after full separation of each of the components of the sample. The procedure presented in this paper permits U and Pu isotopes to be measured together allowing faster sample processing and measurement. The method consists in the extraction with tributyl phosphate of U and Pu isotopes from the rest of the matrix, followed by a cathodic electrodeposition to obtain alpha spectrometry suitable pieces. It can be applied to various environmental samples, such as water, filters and soil (about 0.5 g of solid sample for the described conditions). High-quality electroplated discs are essential for simultaneous processing, so a technique to achieve this requirement is also explained. (authors) [es

  20. Simultaneous wide-range stopping power determination for several ions

    Energy Technology Data Exchange (ETDEWEB)

    Alanko, T. E-mail: tommi.alanko@phys.jyu.fi; Trzaska, W.H.; Lyapin, V.; Raeisaenen, J.; Tiourine, G.; Virtanen, A

    2002-05-01

    A new procedure to extract simultaneously continuous stopping power curves for several ions and several absorbers over a wide energy range and with statistical errors reduced to negligible level is presented. The method combines our novel time-of-flight based method with the capability of our K130 cyclotron and ECR ion-source to produce the so-called ion cocktails. The potential of the method is demonstrated with a 6.0 MeV/u cocktail consisting of {sup 16}O{sup 4+}, {sup 28}Si{sup 7+} and {sup 40}Ar{sup 10+} ions. The stopping power in polycarbonate in the energy range of 0.35-5 MeV/u has been determined with absolute uncertainty of less than 2.3% and with relative below 0.2%. The results are compared with literature data and with SRIM2000 parameterisation including cores and bonds corrections.

  1. Simultaneous determination of actinide and strontium nuclides by extraction chromatography

    International Nuclear Information System (INIS)

    Vajda, N.; Molnar, Zs.

    1999-01-01

    A relatively fast and simple separation procedure has been developed for the simultaneous determination of thorium, uranium, neptunium, plutonium, americium, curium and strontium radionuclides. Most of the isotopes of these elements are long-lived, pure alpha and beta emitters regarded as 'difficult to determine' ones in the literature. Our major goal was to develop a combined procedure capable for the analysis of all these nuclides in the same sample aliquot so that correlations can be revealed without the errors arising due to inhomogeneity of samples when the radionuclides are determined from different sub-samples. The combined procedure has the advantage that sample destruction becomes simpler and faster, too. The chemical procedure consists of co-precipitations for the pre-concentration of groups of chemically similar elements and extraction chromatographic separations for the purification of individual elements. By means of pre-concentration relatively big samples can be treated offering the possibility of low activity measurements that cannot be performed by analysing small sample amounts. Pre-concentration techniques were always chosen in order to improve the selectivity of the following separation steps. (authors)

  2. HPTLC Method Development and Validation of Zolpidem Tartrate in Bulk and Marketed Formulation

    OpenAIRE

    Abhay R. Shirode; Bharti G. Jadhav; Vilasrao J. Kadam

    2015-01-01

    High performance thin layer chromatography (HPTLC) offers many advantages over HPLC. It reduces the cost of analysis as compare to HPLC. The mobile phase consumption per sample is extremely low in HPTLC, hence reducing the acquisition and disposal cost. Considering the cost and suitability of analysis for estimation of zolpidem tartrate in bulk and its marketed formulation, HPTLC method was developed and validated. The Camag HPTLC system, employed with software winCATS (ver.1.4.1.8) was used ...

  3. [Role and functional spectrum of HPTLC in a hospital pharmaceutical quality control program].

    Science.gov (United States)

    Bourget, P; Perello, L; Demirdjian, S

    2001-02-01

    As part of the development of a quality assurance program (QAP), a high performance thin layer chromatography (HPTLC) analysis unit was installed in the pharmacy department at Gustave-Roussy. The HPTLC-CAMAG consists of: 1) an HPTLC-Vario development chamber for optimization of the mobile phases; 2) TLC Sampler III automated sample applicators; 3) solid teflon migration chambers, i.e., horizontal tanks that enable separation to be carried out either in sandwich or in saturation mode; 4) a TLC Scanner 3 densitometer controlled by CATS 4 software; and 5) a Pentium MMX 233 MHz personal computer with an external backup unit. HPTLC quantitative and qualitative analysis has now reached a remarkably high level of development and performance. The samples (aqueous or non-aqueous solutions) that are to be processed are automatically applied by spraying (50-300 nl) in calibrated bands of a few mm (with up to 64 3-mm bands per 10 x 20 cm plate) on high-performance stationary phases and of wide technological diversity. The chromatogram is obtained in 10 min, and run over a migration pathway of 5-6 cm. The plates are read by absorption-reflection or fluorescence-reflection at an ad hoc wavelength (190-800 nm), then the peak areas which have been scanned are calculated by the trapezoid method. The calibration curves are generated by Michaelis-Menten non-linear regression, and validated by internal quality control. The analytical yield is high, i.e., up to 50 assays and 250 determinations per day. HPTLC analysis covers a wide functional range, and can be used in the following ways: 1) as a teaching tool for separative analysis and GLP; 2) it is an invaluable method for the optimization of mobile phases and for the determination of absorption spectra and absorption maxima, with a view to developing HPLC methods in complex matrices; 3) it provides major support for post-production quality control of prescribed hospital preparations of all types, e.g., those connected with parenteral

  4. What's in the box? Authentication of Echinacea herbal products using DNA metabarcoding and HPTLC.

    Science.gov (United States)

    Raclariu, Ancuta Cristina; Ţebrencu, Carmen Elena; Ichim, Mihael Cristin; Ciupercǎ, Oana Teodora; Brysting, Anne Krag; de Boer, Hugo

    2018-05-15

    Differences in regulatory policies between countries as well as a lack of appropriate standardized methods for the authentication and quality control of herbal products directly impact their quality and safety. Echinacea products are among the top-selling herbal products in Europe and the United States with indications for a broad range of ailments. The increased use of Echinacea species has led to concerns about adulterated products resulting from challenges in morphology-based identification, due to overlapping morphological variation, frequent hybridization between species, and deliberate adulteration. This study addressed the need for a novel analytical strategy in the authentication of herbal products. A combination of high performance thin layer chromatography (HPTLC) and DNA metabarcoding was employed. Fifty-three Echinacea herbal products marketed across Europe were tested to evaluate the accuracy of these methods in plant identification and their potential for detecting substitutes, adulterants and other unreported plant constituents. HPTLC provides high resolution in the detection of Echinacea phytochemical target compounds, but does not offer information on the other species within the product. Alternatively, we showed that the limitation of HPTLC in detecting non-targeted species can be overcome by the complementary use of DNA metabarcoding. Using DNA metabarcoding, Echinacea species were detected in 34 out of the 38 retained products (89%), but with a lack of discriminatory resolution at the species level due to the low level of molecular divergence within the Echinacea genus. All of the tested herbal products showed considerable discrepancies between ingredients listed on the label and the ones detected using DNA metabarcoding, registering an overall ingredient fidelity of only 43%. The results confirm that DNA metabarcoding can be used to test for the presence of Echinacea species and simultaneously to detect other species present in even highly

  5. Simultaneous determination of glycols based on fluorescence anisotropy

    International Nuclear Information System (INIS)

    Garcia Sanchez, F.; Navas Diaz, A.; Lopez Guerrero, M.M.

    2007-01-01

    Simultaneous determination of non-fluorescent glycols in mixtures without separation or chemical transformation steps is described. Two methods based in the measure of fluorescence anisotropy of a probe such as fluorescein dissolved in the analyte or analyte mixtures are described. In the first method, the anisotropy spectra of pure and mixtures of analytes are used to quantitative determination (if the fluorophor concentration is in a range where fluorescence intensity is proportional to concentration). In the second method, a calibration curve anisotropy-concentration based on the application of the Perrin equation is established. The methods presented here are capable of directly resolving binary mixtures of non-fluorescent glycols on the basis of differences on the fluorescence anisotropy of a fluorescence tracer. Best analytical performances were obtained by application of the method based on Perrin equation. This method is simple, rapid and allows the determination of mixtures of glycols with reasonable accuracy and precision. Detection limits are limited by the quantum yield and anisotropy values of the tracer in the solvents. Recovery values are related to the differences in anisotropy values of the tracer in the pure solvents. Mixtures of glycerine/ethylene glycol (GL/EG), ethylene glycol/1,2-propane diol (EG/1,2-PPD) and polyethylene glycol 400/1,2-propane diol (PEG 400/1,2-PPD) were analysed and recovery values are within 95-120% in the Perrin method. Relative standard deviation are in the range 1.3-2.9% and detection limits in the range 3.9-8.9%

  6. Multidimensional and Multimodal Separations by HPTLC in Phytochemistry

    Science.gov (United States)

    Ciesla, Lukasz; Waksmundzka-Hajnos, Monika

    HPTLC is one of the most widely applied methods in phytochemical analysis. It is due to its numerous advantages, e.g., it is the only chromatographic method offering the option of presenting the results as an image. Other advantages include simplicity, low costs, parallel analysis of samples, high sample capacity, rapidly obtained results, and possibility of multiple detection. HPTLC provides identification as well as quantitative results. It also enables the identification of adulterants. In case of complex samples, the resolving power of traditional one-dimensional chromatography is usually inadequate, hence special modes of development are required. Multidimensional and multimodal HPTLC techniques include those realized in one direction (UMD, IMD, GMD, BMD, AMD) as well as typical two-dimensional methods realized on mono- or bi-layers. In this manuscript, an overview on variable multidimensional and multimodal methods, applied in the analysis of phytochemical samples, is presented.

  7. Simultaneous determination of a binary mixture: kinetic method for determination of uranium and vanadium

    International Nuclear Information System (INIS)

    Jianhua, W.; Ronghuan, H.

    1993-01-01

    A kinetic method for simultaneous determination of a binary mixture is proposed, and a procedure for simultaneous determination of uranium (IV) and vanadium (IV) is established based on their inductive effect on chromium (VI)-iodide redox reaction in a weak acidic medium. The reaction was monitored by FIA-spectrophotometry using the I 3 - -starch complex as indicator. The calibration graphs are linear for uranium (IV) and vanadium (IV) within the range of 0 ∼ 3.6 μg/ml and 0 ∼ 2.5 μg/ml respectively. Most foreign ions, except for iron (II) and antimony (III), do not interfere with the determination. The uranium and vanadium content in different samples was determined, and the results were satisfactory. (author). 2 tabs., 2 figs., 9 refs

  8. Simultaneous determination of atorvastatin calcium and ramipril in capsule dosage forms by high-performance liquid chromatography and high-performance thin layer chromatography.

    Science.gov (United States)

    Panchal, Hiral J; Suhagia, Bhanubhai N

    2010-01-01

    Two simple and accurate methods to determine atorvastatin calcium and ramipril in capsule dosage forms were developed and validated using HPLC and HPTLC. The HPLC separation was achieved on a Phenomenex Luna C18 column (250 x 4.6 mm id, 5 microm) in the isocratic mode using 0.1% phosphoric acid-acetonitrile (38 + 62, v/v), pH 3.5 +/- 0.05, mobile phase at a flow rate of 1 ml/min. The retention times were 6.42 and 2.86 min for atorvastatin calcium and ramipril, respectively. Quantification was achieved with a photodiode array detector set at 210 nm over the concentration range of 0.5-5 microg/mL for each, with mean recoveries (at three concentration levels) of 100.06 +/- 0.49% and 99.95 +/- 0.63% RSD for atorvastatin calcium and ramipril, respectively. The HPTLC separation was achieved on silica gel 60 F254 HPTLC plates using methanol-benzene-glacial acetic acid (19.6 + 80.0 + 0.4, v/v/v) as the mobile phase. The Rf values were 0.40 and 0.20 for atorvastatin calcium and ramipril, respectively. Quantification was achieved with UV densitometry at 210 nm over the concentration range of 50-500 ng/spot for each, with mean recoveries (at three concentration levels) of 99.98 +/- 0.75% and 99.87 +/- 0.83% RSD for atorvastatin calcium and ramipril, respectively. Both methods were validated according to International Conference on Harmonization guidelines and found to be simple, specific, accurate, precise, and robust. The mean assay percentages for atorvastatin calcium and ramipril were 99.90 and 99.55% for HPLC and 99.91 and 99.47% for HPTLC, respectively. The methods were successfully applied for the determination of atorvastatin calcium and ramipril in capsule dosage forms without any interference from common excipients.

  9. Simultaneous determination of radioactive halogen isotopes and 99Tc

    International Nuclear Information System (INIS)

    Kabai, E.; Vajda, N.; Gaca, P.

    2003-01-01

    The purpose of this study was to develop a simplified method for simultaneous determination of radiologically important halogen isotopes and 99 Tc from different types of samples like environmental, biological and waste samples. Due to their long half-lives (longer than 10 5 years) they play important role in the nuclear cycle, especially in environmental monitoring and protection. For a rapid response in the evaluation of 129 I, 36 Cl and 99 Tc contamination levels of these samples it is advantageous to combine the existing individual methods. According to the present procedure, iodine, chlorine and technetium are separated selectively from the same sample aliquot followed by the β spectrometry of the purified fractions. Increased sensitivities can be achieved by neutron activation (NA) especially in the case of 129 I. Our work intends to solve the problem by combining the well-known hot acidic distillation method for iodine separation with the organic extraction process characteristic for technetium separation. The major objective of the work was to separate the disturbing halides from iodine. For this purpose a selective oxidant was applied. For the sample destruction and fractionated distillation an air flow-through installation was used with hot concentrated sulphuric and nitric acids. The trap for iodine contained 3 M NaOH solution. After iodine separation the trap was exchanged for a new one containing the same solution for trapping chlorine or bromine with an addition of 0.01 M KMnO 4 solution as an oxidative agent. As expected, the main part of technetium was contained in the acidic residue after distillation. Tc purification was performed by organic extraction with TBP and TEVA column. (author)

  10. Antiglycation and Antioxidant Activities and HPTLC Analysis of ...

    African Journals Online (AJOL)

    Furthermore, high performance thin layer chromatography (HPTLC) analysis of Boswellia sacra resins was also carried out. Results: Polar fractions of the extract obtained exhibited the highest antiglycation activity while nonpolar fractions showed more than 50 % inhibition in superoxide anion scavenging assay.

  11. QUALITY CONTROL OF HAWTHORN TINCTURE BY HPTLC METHOD

    Directory of Open Access Journals (Sweden)

    Khokhlova KO

    2016-09-01

    Full Text Available Introduction. Hawthorn tincture is one of the most used herbal drugs at the domestic pharmaceutical market. According to the State register of drugs at the pharmaceutical market of Ukraine, there are 13 commercial offers of Hawthorn tincture from home-produced manufactures. The initial herbal raw materials for Hawthorn tincture are Hawthorn fruits, which are widespread at the territory of Ukraine. These are pharmacopoeial herbal raw material. Thus, 12 different species of Hawthorn fruits are included into monograph of Ukrainian State Pharmacopoeia (SPhU and State Pharmacopoeia of USSR XI ed. On the territory of Ukraine there are near 30 different species of Hawthorn, and the quantity of species is much arises due to its forms and hybrids. The ‘natural variability’ of bioactive substances of Hawthorn fruits of the same species and possibility of usage of many different species during manufacturing process of herbal drugs lead to the pitfalls in standardization of herbal drugs in general, and Hawthorn tincture particularly, and should be taken in mind while development of its quality control methods. For development of specific and reproducible identification method, it is necessary to ensure the number of parameters: usage of method and equipment that give reproducible results; big selections of different samples; rigorously observation of method’s procedure of implementation. The modern, automated HPTLC method of analysis was chosen for identification purpose. If standardize procedure and suitable equipment are used, the reproducible results of the method have to be obtained. The aim of this paper was development of HPTLC method for identification of Hawthorn tincture, which could be appropriated for stability study and establishment of its expire date. Materials and Methods. In research 13 samples of Hawthorn tinctures from 8 manufactures from Ukraine and Russia were analyzed. These samples were manufactured in 2010, 2014, 2015 years. The

  12. [HPTLC fingerprint analysis of andrographolides from Andrographis paniculata].

    Science.gov (United States)

    Shao, Yan-Hua; Wang, Jian-Gang; Lai, Xiao-Ping; Wu, Xiang-Wei; Ding, Ping

    2014-02-01

    To establish the high-performance thin layer chromatography (HPTLC) fingerprint of andrographolides from Andrographis paniculata, and to valuate the fingerprint similarity of samples from different habitats, markets, used parts and so on. Chromatographic conditions were as follows: stationary phase: precoated HPTLC GF254 silica-gel plate (20 cm x 10 cm); developing solvent system: chloroform-toluene-methanol (80:10:15); Relative humidity: 42%; Color development reagent: 5% H2SO4 ethanolic solution, heating at 105 degrees C and observing the fluorescent chromatogram in a UV cabinet at 366 nm. The common patterns of HPTLC fingerprint were obtained through CHROMAP 1.5 solution software. The HPTLC fingerprint of andrographolides was consisted of 9 characteristic peaks (fluorescent bands) including andrographolide, neoandrographolide and dehydroandrographolide which were chemical reference substances. The investigation and analysis of 51 batches of Andrographis paniculata showed that there were remarkable differences among different samples, so was the content of andrographolide and total lactones. This method is simple and rapid, which can serve as an effective identification and quality assessment method for Andrographis paniculata.

  13. Estimation of individual sennosides in plant materials and marketed formulations by an HPTLC method.

    Science.gov (United States)

    Shah, S A; Ravishankara, M N; Nirmal, A; Shishoo, C J; Rathod, I S; Suhagia, B N

    2000-04-01

    Senna is a well-known drug, used in the Ayurvedic and Allopathic systems of medicine, and is a treatment for constipation. The purgative action of senna and its formulations is due to the presence of sennosides A and B. An HPTLC method has been developed for the determination of individual sennosides (A, B, C, D) without any derivatization in marketed formulations (three tablet formulations, two granule formulations and one liquid formulation) and plant materials (senna leaf and pod). The methanolic solution of a sample was applied on a pre-coated silica gel G60 F254 TLC plate (E. Merck.) and was developed using n-propanol : ethyl acetate : water : glacial acetic acid (3 : 3 : 2 : 0.1 v/v) as the mobile phase. The relative band speeds (Rf values) obtained were 0.35, 0.25, 0.61, 0.46 for sennosides A, B, C and D, respectively. The densitometric response was monitored at 366nm. Calibration curves were found to be linear in the concentration ranges 193-1356, 402-2817, 71-497 and 132-927 ng per spot for sennosides A, B, C, and D, respectively. The correlation coefficients were found to be 0.9978, 0.9987, 0.9939 and 0.9983 respectively for sennosides A, B, C and D. The result obtained with the HPTLC method for total sennoside content was compared with the results using the pharmacopoeial methods (spectrophotometric (British Pharmacopoeia) and spectrofluorimetric (United States Pharmacopeia) using the 'F' test). The results revealed no significant difference in the three different methods for estimation of total sennoside. The proposed HPTLC method was found to be simple, specific, precise, accurate and rapid. It can be used for routine quality control of sennosides or senna-containing formulations for individual sennosides.

  14. Rapid validated HPTLC method for estimation of piperine and piperlongumine in root of Piper longum extract and its commercial formulation

    Directory of Open Access Journals (Sweden)

    Anagha A. Rajopadhye

    2012-12-01

    Full Text Available Piperine and piperlongumine, alkaloids having diverse biological activities, commonly occur in roots of Piper longum L., Piperaceae, which have high commercial, economical and medicinal value. In present study, rapid, validated HPTLC method has been established for the determination of piperine and piperlongumine in methanolic root extract and its commercial formulation 'Mahasudarshan churna®' using ICH guidelines. The use of Accelerated Solvent Extraction (ASE as an alternative to conventional techniques has been explored. The methanol extracts of root, its formulation and both standard solutions were applied on silica gel F254 HPTLC plates. The plates were developed in Twin chamber using mobile phase toluene: ethyl acetate (6:4, v/v and scanned at 342 and 325 nm (λmax of piperine and piperlongumine, respectively using Camag TLC scanner 3 with CATS 4 software. A linear relationship was obtained between response (peak area and amount of piperine and piperlongumine in the range of 20-100 and 30-150 ng/spot, respectively; the correlation coefficient was 0.9957 and 0.9941 respectively. Sharp, symmetrical and well resolved peaks of piperine and piperlongumine spots resolved at Rf 0.51 and 0.74, respectively from other components of the sample extracts. The HPTLC method showed good linearity, recovery and high precision of both markers. Extraction of plant using ASE and rapid HPTLC method provides a new and powerful approach to estimate piperine and piperlongumine as phytomarkers in the extract as well as its commercial formulations for routine quality control.

  15. Status of sennosides content in various Indian herbal formulations: Method standardization by HPTLC

    Directory of Open Access Journals (Sweden)

    Md.Wasim Aktar

    2008-12-01

    Full Text Available Several poly-herbal formulations containing senna (Cassia angustifolia leaves are available in the Indian market for the treatment of constipation. The purgative effect of senna is due to the presence of two unique hydroxy anthracene glycosides sennosides A and B. A HPTLC method for the quantitative analysis of sennosides A and B present in the formulation has been developed. Methanol extract of the formulations was analyzed on a silica gel 60 GF254 HPTLC plates with spot visualization under UV and scanning at 350 nm in absorption/ reflection mode. Calibration curves were found to be linear in the range 200-1000 ηg. The correlation coefficients were found to be 0.991 for sennoside A and 0.997 for sennoside B. The average recovery rate was 95% for sennoside A and 97% for sennoside B showing the reliability and reproducibility of the method. Limit of detection and quantification were determined as 0.05 and 0.25 μg/g respectively. The validity of the method with respect to analysis was confirmed by comparing the UV spectra of the herbal formulations with that of the standard within the same Rf window. The analysis revealed a significant variation in sennosides content.

  16. Standardization of Berberis aristata extract through conventional and modern HPTLC techniques

    Directory of Open Access Journals (Sweden)

    Dinesh K. Patel

    2012-05-01

    Full Text Available Objective: Berberis aristata (Berberidaceae is an important medicinal plant, found in the different region of the world. It has significant medicinal value in the traditional Indian and Chinese system of medicine. The aim of the present investigation includes qualitative and quantitative analysis of Berberis aristata extract. Methods: Present study includes determination of phytochemical analysis, solubility test, heavy metal analysis, antimicrobial study and quantitative analysis by HPTLC method. Results: Preliminary phytochemical analysis showed the presence of carbohydrate, glycoside, alkaloid, protein, amino acid, saponin, tannin and flavonoid. Solubility in water and alcohal were found to be 81.90% in water and 84.52% in 50% in alcohal. Loss on drying was found to be 5.32%. Total phenol and flavonoid content were found to be 0.11% and 2.8%. Level of lead, arsenic, mercury and cadmium complies the standard level. E. coli and salmonella was found to be absent whereas total bacterial count, yeast and moulds contents were found to be under the limit. Content of berberine was found to be 13.47% through HPTLC techniques. Conclusions: The results obtained from the present studies could be used as source of valuable information which can play an important role for the food scientists, researchers and even the consumers for its standards.

  17. Simultaneous determination of aluminium and phosphorus by neutron activation analysis

    International Nuclear Information System (INIS)

    Gatschke, W.; Gawlik, D.

    1980-01-01

    With the use of the pneumatic tube system of the BER II reactor, the irradiation position of which is equipped with a movable cadmium shield, the aluminium and phosphorus levels in bone powder and in human bone biopsies were determined. The contribution of aluminium and phosphorus to the 28 Al activity could be separated mathematically after the samples had been irradiated with and without cadmium shielding. The sensitivity and limit of quantitative determination of the analytical procedure were determined using the addition method and the fact that the levels of each element measured was independent of the amount of the other element was proved. (author)

  18. Preconcentration NAA for simultaneous multielemental determination in water sample

    International Nuclear Information System (INIS)

    Chatt, A.

    1999-01-01

    Full text: Environment concerns with water, air, land and their interrelationship viz., human beings, fauna and flora. One of the important environmental compartments is water. Elements present in water might face a whole lot of physico-chemical conditions. This poses challenges to measure their total concentrations as well as different species. Preconcentration of the elements present in water samples is a necessary requisites in water analysis. For multi elements concentration measurements, Neutron Activation Analysis (NAA) is one of the preferred analytical techniques due to its sensitivity and selectivity. In this talk preconcentration NAA for multielemental determination in water sample determination will be discussed

  19. Simultaneous Determination of Co-formulated Matrine and ...

    African Journals Online (AJOL)

    Purpose: To develop and validate a new, simple, sensitive and accurate high performance liquid chromatographic (HPLC) method for the simulataneous determination of matrine and secnidazole in suppositories. Methods: The method involved using a SinoChoom ODS-BP C18 column (5 ƒÊm, 4.6 mm ~ 200 mm) and ...

  20. Simultaneous Determination of Co-formulated Matrine and ...

    African Journals Online (AJOL)

    HP

    of 6.69 min and linearity for the quantification of the drug was obtained in the concentration range of ... biological samples. To the best of our knowledge, few HPLC methods have been developed in the literature for the determination of matrine and secnidazole in ... Chromatographic analysis was performed using.

  1. Simultaneous Estimation of Sitagliptin and Metformin in ...

    African Journals Online (AJOL)

    A rapid, simple, specific and precise high-performance thin-layer chromatography (HPTLC) method was developed for the simultaneous estimation of sitagliptin (STG) and metformin (MET) content in a fixed dose pharmaceutical formulation and also in bulk drug. In the developed method, aluminium backed silica gel 60 ...

  2. Simultaneous Atomic Absorption Spectrometry for Cadmium and Lead Determination in Wastewater: A Laboratory Exercise

    Science.gov (United States)

    Correia, Paulo R. M.; Oliveira, Pedro V.

    2004-01-01

    The simultaneous determination of cadmium and lead by multi-element atomic absorption spectrometry with electrochemical atomization is proposed by employing a problem-based approach. The reports indicate that the students assimilated the principles of the simultaneous atomic absorption spectrometry (SIMAAS), the role of the chemical modifier, the…

  3. Simulating shelf life determination by two simultaneous criteria.

    Science.gov (United States)

    Peleg, Micha; Normand, Mark D

    2015-12-01

    The shelf life of food and pharmaceutical products is frequently determined by a marker's concentration or quality index falling below or surpassing an assigned threshold level. Naturally, different chosen markers would indicate different shelf life for the same storage temperature history. We demonstrate that if there are two markers, such as two labile vitamins, the order in which their concentrations cross their respective thresholds may depend not only on their degradation kinetic parameters but also on the particular storage temperature profile, be it isothermal or non-isothermal. Thus, at least theoretically, the order observed in accelerated storage need not be always indicative of the actual order at colder temperatures, except where the two degradation reactions follow the same kinetic order and their temperature-dependence rate parameter is also the same. This is shown with simulated hypothetical degradation reactions that follow first or zero order kinetics and whose rate constant's temperature-dependence obeys the exponential model. It is also demonstrated with simulated hypothetical Maillard reaction's products whose synthesis rather than their degradation follows pseudo zero order kinetics. The software developed to do the simulations and calculate the thresholds crossing points has been posted on the Internet as a freely downloadable interactive Wolfram Demonstration, which can be used as a tool in storage studies and shelf life prediction. In principle, the methodology can be extended from two to any number of markers. Copyright © 2015 Elsevier Ltd. All rights reserved.

  4. The fractioning factor and the number of theorical plates in isotopic enrichment columns determined simultaneously

    International Nuclear Information System (INIS)

    Ducatti, Carlos

    1997-01-01

    Using an analytical approach and an analytical graphical method, it was determined simultaneously the fractioning factor and the number of theoretical plates in isotopic enrichment columns during the conditions of dinamical isotopic equilibrium. (author). 5 refs., 2 figs., 2 tabs

  5. Simultaneous determination of Albendazol and Triclabendazol in Triclazol 22 suspension for veterinary purposes

    International Nuclear Information System (INIS)

    Garcia Penna, Caridad M.; Gafas Leyva, Maite; Rosales Bosch, Karina

    2013-01-01

    Triclazol 22 suspension containing triclabendazol and albendazol is used as parasiticide for veterinary purposes. to validate the analytical method for simultaneous determination of triclabendazol and albendazol in triclazol 22 suspension for quality control

  6. Estimation of yohimbine base in complex mixtures by quantitative HPTLC application.

    Science.gov (United States)

    Adel-Kader, Maged Saad; Alwahebi, Naif Wahebi Hamadan; Alam, Prawez

    2017-01-01

    The indole alkaloid Yohimbine has been used for over two centuries in the treatment of erectly dysfunction. Several formulations containing yohimbine salts, yohimbe bark power or extract are marketed worldwide. Determination of the amount of yohimbine in such formulation is a challenging task due to their complex nature. Extraction followed by acid-base purification resulted in a relatively pure alkaloids containing fractions. The exact amounts of yohimbine free base in different formulations were determined by densitometric HPTLC validated methods using silica gel TLC plates. Standard curve for yohimbine was generated using yohimbine hydrochloride subjected to the same acid-base treatment as the used samples. All formulations found to contain yohimbine though some with less concentration than the labeled amount.

  7. Combining surface enhanced Raman scattering (SERS) and high-performance thin-layer chromatography (HPTLC)

    Science.gov (United States)

    Koglin, E.

    A new method for preparing SERS active surfaces using silver colloidal spheres deposited on HPTLC plates, used for thin-layer chromatography, is discussed in detail. The sensitivity of these activated HPTLC plates is so high that in-situ vibrational investigations of chromatogram spots are possible at the nanogram level. The HPTLC/SERS spectra of purine, benzoic acid and 1-nitro-pyrene adsorbed on silver colloidal activated silica gel plates are measured in the nanogram region. In addition we also report in this paper on the results of a feasibility study performed to evaluate the analytical potential of micro-Raman spectroscopy (triple monochromator, multichannel detection system) in SERS/HPTLC spot characterization. It permits the acquisition of Raman spectra from HPTLC spots down to 1 μm in size or other forms of microsamples approaching the picogram level in mass.

  8. Extraction as a source of additional information when concentrations in multicomponent systems are simultaneously determined

    International Nuclear Information System (INIS)

    Perkov, I.G.

    1988-01-01

    Using as an example photometric determination of Nd and Sm in their joint presence, the possibility to use the influence of extraction on analytic signal increase is considered. It is shown that interligand exchange in extracts in combination with simultaneous determination of concentrations can be used as a simple means increasing the accuracy of determination. 5 refs.; 2 figs.; 3 tabs

  9. Simultaneous determination of uranium and thorium with Arsenazo III by second-derivative spectrophotometry

    International Nuclear Information System (INIS)

    Kuroda, Rokuro; Kurosaki, Mayumi; Hayashibe, Yutaka; Ishimaru, Satomi

    1990-01-01

    A derivative spectrophotometric method has been developed for the simultaneous determination of microgram quantities of uranium and thorium with Arsenazo III in hydrochloric acid medium. The second-derivative absorbances of the uranium and thorium Arsenazo III complexes at 679.5 and 684.4 nm are used for their quantification. Uranium and thorium, both in the range 0.1-0.7 μg/ml have been determined simultaneously with good precision. The procedure does not require separation of uranium and thorium, and allows the determination of both metals in the presence of alkaline-earth metals and zirconium, but lanthanides interfere. (author)

  10. HPTLC-aptastaining - Innovative protein detection system for high-performance thin-layer chromatography

    Science.gov (United States)

    Morschheuser, Lena; Wessels, Hauke; Pille, Christina; Fischer, Judith; Hünniger, Tim; Fischer, Markus; Paschke-Kratzin, Angelika; Rohn, Sascha

    2016-05-01

    Protein analysis using high-performance thin-layer chromatography (HPTLC) is not commonly used but can complement traditional electrophoretic and mass spectrometric approaches in a unique way. Due to various detection protocols and possibilities for hyphenation, HPTLC protein analysis is a promising alternative for e.g., investigating posttranslational modifications. This study exemplarily focused on the investigation of lysozyme, an enzyme which is occurring in eggs and technologically added to foods and beverages such as wine. The detection of lysozyme is mandatory, as it might trigger allergenic reactions in sensitive individuals. To underline the advantages of HPTLC in protein analysis, the development of innovative, highly specific staining protocols leads to improved sensitivity for protein detection on HPTLC plates in comparison to universal protein derivatization reagents. This study aimed at developing a detection methodology for HPTLC separated proteins using aptamers. Due to their affinity and specificity towards a wide range of targets, an aptamer based staining procedure on HPTLC (HPTLC-aptastaining) will enable manifold analytical possibilities. Besides the proof of its applicability for the very first time, (i) aptamer-based staining of proteins is applicable on different stationary phase materials and (ii) furthermore, it can be used as an approach for a semi-quantitative estimation of protein concentrations.

  11. Simultaneous determination of oxygen and cadmium in cadmium and cadmium compounds

    International Nuclear Information System (INIS)

    Imaeda, K.; Kuriki, T.; Ohsawa, K.; Ishii, Y.

    1977-01-01

    Cadmium and its compounds were analysed for oxygen and cadmium by a modification of the Schutze-Unterzaucher method. Oxygen in some compounds such as cadmium oxide, nitrate and sulphate could not be determined by the usual method. The method of adding carbon was employed for the determination of total oxygen. Total oxygen could be determined by the addition of 5 mg of carbon to a sample boat and heating at 950 0 . The determination was also carried out by addition of naphthalene (2 mg). It was found that the cadmium powder and cadmium flake used contained ca. 1 and 0.15% oxygen, respectively. Oxygen and cadmium in cadmium and its compounds were simultaneously determined by the addition of 2 mg of naphthalene. Cadmium was determined colorimetrically by use of glyoxal-bis-(2-hydroxyanil). Oxygen and cadmium in the samples could be determined simultaneously with an average error of -0.02 and -0.22%, respectively. (author)

  12. Simultaneous spectrophotometric determination of binary mixtures of surfactants using continuous wavelet transformation

    International Nuclear Information System (INIS)

    Afkhami, Abbas; Nematollahi, Davood; Madrakian, Tayyebeh; Abbasi-Tarighat, Maryam; Hajihadi, Mitra

    2009-01-01

    This work presents a simple, rapid, and novel method for simultaneous determination of binary mixtures of some surfactants using continuous wavelet transformation. The method is based on the difference in the effect of surfactants Cetyltrimethylammoniumbromide (CTAB), dodecyl trimethylammonium bromide (DTAB), cetylpyridinium bromide (CPB) and TritonX-100 (TX-100) on the absorption spectra of complex of Beryllium with Chrome Azurol S (CAS) at pH 5.4. Binary mixtures of CTAB-DTAB, DTAB-CPB and CTAB-TX-100 were analyzed without prior separation steps. Different mother wavelets from the family of continuous wavelet transforms were selected and applied under the optimal conditions for simultaneous determinations. The proposed methods, under the working conditions, were successfully applied to simultaneous determination of surfactants in hair conditioner and mouthwash samples.

  13. SIMULTANEOUS SPECTROPHOTOMETRIC DETERMINATION OF MONTELUKAST SODIUM AND BAMBUTEROL HYDROCHLORIDE IN TABLETS

    OpenAIRE

    Patel Satish A; Patel Dhara J; Patel Natavarlal J.

    2011-01-01

    The present manuscript describe simple, sensitive, rapid, accurate, precise and economical first derivative spectrophotometric method for the simultaneous determination of montelukast sodium and bambuterol hydrochloride in combined tablet dosage form. The derivative spectrophotometric method was based on the determination of both the drugs at their respective zero crossing point (ZCP). The first order derivative spectra was obtained in chloroform and the determinations were made at 241 nm (ZC...

  14. Rapid Multisample Analysis for Simultaneous Determination of Anthropogenic Radionuclides in Marine Environment

    DEFF Research Database (Denmark)

    Qiao, Jixin; Shi, Keliang; Hou, Xiaolin

    2014-01-01

    An automated multisample processing flow injection (FI) system was developed for simultaneous determination of technetium, neptunium, plutonium, and uranium in large volume (200 L) seawater. Ferrous hydroxide coprecipitation was used for the preliminary sample treatment providing the merit of sim...... reliable data with reduced analytical cost in both radioecology studies and nuclear emergency preparedness....

  15. Simultaneous Determination of Arsenic, Manganese, and Selenium in Biological Materials by Neutron-Activation Analysis

    DEFF Research Database (Denmark)

    Heydorn, Kaj; Damsgaard, Else

    1973-01-01

    A new method was developed for the simultaneous determination of arsenic, manganese, and selenium in biological material by thermal-neutron activation analysis. The use of 81 mSe as indicator for selenium permitted a reduction of activation time to 1 hr for a 1 g sample, and the possibility of loss...

  16. A universal gamma-gamma method for simultaneous determination of rock and ore properties

    International Nuclear Information System (INIS)

    Charbucinski, J.

    1983-01-01

    A method for the simultaneous determination of heavy element content, density, borehole diameter and grain size is described, which is based on investigation of the changes in spectrum shape. By analysing these changes in a quantitative manner, information regarding the physical parameters of the medium can be obtained. The results of laboratory tests of the method are presented. (author)

  17. Simultaneous Determination of Binding Constants for Multiple Carbohydrate Hosts in Complex Mixtures

    DEFF Research Database (Denmark)

    Meier, Sebastian; Beeren, Sophie

    2014-01-01

    We describe a simple method for the simultaneous determination of association constants for a guest binding to seven different hosts in a mixture of more than 20 different oligosaccharides. If the binding parameters are known for one component in the mixture, a single NMR titration suffices...

  18. Simultaneous determination of ochratoxin A, mycophenolic acid and fumonisin B-2 in meat products

    DEFF Research Database (Denmark)

    Sørensen, Louise Marie; Mogensen, Jesper; Nielsen, Kristian Fog

    2010-01-01

    Here we present a method for simultaneous determination of the fungal metabolites mycophenolic acid, ochratoxin A (OTA) and fumonisin B-2 (FB2) in meat products. Extraction was performed with water-acetonitrile, followed by acetone-induced precipitation of salts and proteins. Purification...

  19. Bioanalytical HPTLC Method for Estimation of Zolpidem Tartrate from Human Plasma

    OpenAIRE

    Abhay R. Shirode; Bharti G. Jadhav; Vilasrao J. Kadam

    2016-01-01

    A simple and selective high performance thin layer chromatographic (HPTLC) method was developed and validated for the estimation of zolpidem tartrate from human plasma using eperisone hydrochloride as an internal standard (IS). Analyte and IS were extracted from human plasma by liquid liquid extraction (LLE) technique. The Camag HPTLC system, employed with software winCATS (ver.1.4.1.8) was used for the proposed bioanalytical work. Planar chromatographic development was carried out with the h...

  20. Status of sennosides content in various Indian herbal formulations: Method standardization by HPTLC

    OpenAIRE

    Md.Wasim Aktar; Rajlakshmi Poi; Anjan Bhattacharyya

    2008-01-01

    Several poly-herbal formulations containing senna (Cassia angustifolia) leaves are available in the Indian market for the treatment of constipation. The purgative effect of senna is due to the presence of two unique hydroxy anthracene glycosides sennosides A and B. A HPTLC method for the quantitative analysis of sennosides A and B present in the formulation has been developed. Methanol extract of the formulations was analyzed on a silica gel 60 GF254 HPTLC plates with spot visualization under...

  1. Simultaneous Determination of Four Preservatives in Foodstuffs by High Performance Liquid Chromatography

    OpenAIRE

    Mohammad Faraji; Farzaneh Rahbarzare

    2016-01-01

    Background and objectives:  High concentration of preservatives in food may result in gastrointestinal disturbances whereby some patients suffering from asthma, rhinitis, or urticaria. The aim of this study is the introduction and optimization a new method for simultaneous determination of four preservatives (SB, PS, MP, PP) in foodstuff by high performance liquid chromatography. Materials and methods: Important factors in extraction, separation and determination process were optimiz...

  2. Spectrophotometric simultaneous determination of Rabeprazole Sodium and Itopride Hydrochloride in capsule dosage form

    Science.gov (United States)

    Sabnis, Shweta S.; Dhavale, Nilesh D.; Jadhav, Vijay. Y.; Gandhi, Santosh V.

    2008-03-01

    A new simple, economical, rapid, precise and accurate method for simultaneous determination of rabeprazole sodium and itopride hydrochloride in capsule dosage form has been developed. The method is based on ratio spectra derivative spectrophotometry. The amplitudes in the first derivative of the corresponding ratio spectra at 231 nm (minima) and 260 nm were selected to determine rabeprazole sodium and itopride hydrochloride, respectively. The method was validated with respect to linearity, precision and accuracy.

  3. Simultaneous determination of size and refractive index of red blood cells by light scattering measurements

    International Nuclear Information System (INIS)

    Ghosh, N.; Buddhiwant, P.; Uppal, A.; Majumder, S.K.; Patel, H.S.; Gupta, P.K.

    2006-01-01

    We present a fast and accurate approach for simultaneous determination of both the mean diameter and refractive index of a collection of red blood cells (RBCs). The approach uses the peak frequency of the power spectrum and the corresponding phase angle obtained by performing Fourier transform on the measured angular distribution of scattered light to determine these parameters. Results on the measurement of two important clinical parameters, the mean cell volume and mean cell hemoglobin concentration of a collection of RBCs, are presented

  4. Development of a new, rapid and sensitive HPTLC method for estimation of Milnacipran in bulk, formulation and compatibility study

    Directory of Open Access Journals (Sweden)

    Gautam Singhvi

    2017-05-01

    Full Text Available A simple, sensitive and rapid high performance thin layer chromatographic (HPTLC method has been developed and validated for quantitative determination of Milnacipran Hydrochloride (MIL in bulk and formulations. The chromatographic development was carried out on HPTLC plates precoated with silica gel 60 F254 using a mixture of acetonitrile, water and ammonia (6:0.6:1.6 (v/v/v as mobile phase. Detection was carried out densitometrically at 220 nm. The Rf value of drug was found to be 0.63 ± 0.02. The method was validated as per ICH guideline with respect to linearity, accuracy, precision, robustness etc. The calibration curve was found to be linear over a range of 100–1000 ng μL−1 with a regression coefficient of 0.999. The accuracy was found to be very high (99.12–100.87%. %RSD values for intra-day and inter-day variation were not more than 1.43. The method has demonstrated high sensitivity and specificity. The method was applied for compatibility studies also. The method is new, simple and economic for routine estimation of MIL in bulk, preformulation studies and pharmaceutical formulation to help the industries as well as researchers for their sensitive determination of MIL rapidly at low cost in routine analysis.

  5. Densitometric HPTLC analysis of 8-gingerol in Zingiber officinale extract and ginger-containing dietary supplements, teas and commercial creams.

    Science.gov (United States)

    Alam, Prawez

    2013-08-01

    To develop and validate a simple, accurate HPTLC method for the analysis of 8-gingerol and to determine the quantity of 8-gingerol in Zingiber officinale extract and ginger-containing dietary supplements, teas and commercial creams. The analysis was performed on 10×20 cm aluminium-backed plates coated with 0.2 mm layers of silica gel 60 F254 (E-Merck, Germany) with n-hexane: ethyl acetate 60: 40 (v/v) as mobile phase. Camag TLC Scanner III was used for the UV densitometric scanning at 569. This system was found to give a compact spot of 8-gingerol at retention factor (Rf) value of (0.39±0.04) and linearity was found in the ranges 50-500 ng/spot (r (2)=0.9987). Limit of detection (12.76 ng/spot), limit of quantification (26.32 ng/spot), accuracy (less than 2 %) and recovery (ranging from 98.22-99.20) were found satisfactory. The HPTLC method developed for quantification of 8-gingerol was found to be simple, accurate, reproducible, sensitive and is applicable to the analysis of 8-gingerol in Zingiber officinale extract and ginger-containing dietary supplements, teas and commercial creams.

  6. Estimation of L-dopa from Mucuna pruriens LINN and formulations containing M. pruriens by HPTLC method.

    Science.gov (United States)

    Modi, Ketan Pravinbhai; Patel, Natvarlal Manilal; Goyal, Ramesh Kishorilal

    2008-03-01

    A selective, precise, and accurate high-performance thin-layer chromatographic (HPTLC) method has been developed for the analysis of L-dopa in Mucuna pruriens seed extract and its formulations. The method involves densitometric evaluation of L-dopa after resolving it by HPTLC on silica gel plates with n-butanol-acetic acid-water (4.0+1.0+1.0, v/v) as the mobile phase. Densitometric analysis of L-dopa was carried out in the absorbance mode at 280 nm. The relationship between the concentration of L-dopa and corresponding peak areas was found to be linear in the range of 100 to 1200 ng/spot. The method was validated for precision (inter and intraday), repeatability, and accuracy. Mean recovery was 100.30%. The relative standard deviation (RSD) values of the precision were found to be in the range 0.64-1.52%. In conclusion, the proposed TLC method was found to be precise, specific and accurate and can be used for identification and quantitative determination of L-dopa in herbal extract and its formulations.

  7. Forensic Analysis of Blue Ball point Pen Inks on Questioned Documents by High Performance Thin Layer Chromatography Technique (HPTLC)

    International Nuclear Information System (INIS)

    Lee, L.C.; Siti Mariam Nunurung; Abdul Aziz Ishak

    2014-01-01

    Nowadays, crimes related to forged documents are increasing. Any erasure, addition or modification in the document content always involves the use of writing instrument such as ball point pens. Hence, there is an evident need to develop a fast and accurate ink analysis protocol to solve this problem. This study is aimed to determine the discrimination power of high performance thin layer chromatography (HPTLC) technique for analyzing a set of blue ball point pen inks. Ink samples deposited on paper were extracted using methanol and separated via a solvent mixture of ethyl acetate, methanol and distilled water (70: 35: 30, v/ v/ v). In this method, the discrimination power of 89.40 % was achieved, which confirm that the proposed method was able to differentiate a significant number of pen-pair samples. In addition, composition of blue pen inks was found to be homogeneous (RSD < 2.5 %) and the proposed method showed good repeatability and reproducibility (RSD < 3. 0%). As a conclusion, HPTLC is an effective tool to separate blue ball point pen inks. (author)

  8. Radioactivation method for simultaneous determination of nitrogen, phosphorus and potassium content in plants and fertilizers

    International Nuclear Information System (INIS)

    Srapeniants, R.A.; Saveliev, I.B.; Kovtun, J.L.; Sidorov, A.V.; Tsagolov, K.S.; Miroshnikova, N.N.

    1982-01-01

    A radioactivation method for the simultaneous determination of the nitrogen, phosphorus and potassium content in plants and fertilizers is described. Samples to be analyzed and standard samples are exposed to neutron irradiation, and the spectra of gamma radiation induced in the samples are recorded. The samples laid aside for a period of time determined by the half-life of interfering isotopes, and the spectra of the samples and standards are recorded again. The first and second spectra are superposed and shifted relative to each other along the energy axis, and the content of the elements being analyzed is determined by comparing the spectra of the samples and standards

  9. Simultaneous determination of three herbicides by differential pulse voltammetry and chemometrics.

    Science.gov (United States)

    Ni, Yongnian; Wang, Lin; Kokot, Serge

    2011-01-01

    A novel differential pulse voltammetry method (DPV) was researched and developed for the simultaneous determination of Pendimethalin, Dinoseb and sodium 5-nitroguaiacolate (5NG) with the aid of chemometrics. The voltammograms of these three compounds overlapped significantly, and to facilitate the simultaneous determination of the three analytes, chemometrics methods were applied. These included classical least squares (CLS), principal component regression (PCR), partial least squares (PLS) and radial basis function-artificial neural networks (RBF-ANN). A separately prepared verification data set was used to confirm the calibrations, which were built from the original and first derivative data matrices of the voltammograms. On the basis relative prediction errors and recoveries of the analytes, the RBF-ANN and the DPLS (D - first derivative spectra) models performed best and are particularly recommended for application. The DPLS calibration model was applied satisfactorily for the prediction of the three analytes from market vegetables and lake water samples.

  10. Simultaneous determination of rifampicin, isoniazid and pyrazinamide in tablet preparations by multivariate spectrophotometric calibration.

    Science.gov (United States)

    Goicoechea, H C; Olivieri, A C

    1999-08-01

    The use of multivariate spectrophotometric calibration is presented for the simultaneous determination of the active components of tablets used in the treatment of pulmonary tuberculosis. The resolution of ternary mixtures of rifampicin, isoniazid and pyrazinamide has been accomplished by using partial least squares (PLS-1) regression analysis. Although the components show an important degree of spectral overlap, they have been simultaneously determined with high accuracy and precision, rapidly and with no need of nonaqueous solvents for dissolving the samples. No interference has been observed from the tablet excipients. A comparison is presented with the related multivariate method of classical least squares (CLS) analysis, which is shown to yield less reliable results due to the severe spectral overlap among the studied compounds. This is highlighted in the case of isoniazid, due to the small absorbances measured for this component.

  11. Simultaneous determination of Magnolol and Honokiol by amino acid ionic liquid synchronous fluorescence spectrometry

    Science.gov (United States)

    Liu, Wei; Zhu, Xiashi

    2018-05-01

    A novel method based on amino acid ionic liquids (AAILs) as an additive synchronous fluorescence spectrometry is proposed for simultaneous determination of magnolol (MN) and honokiol (HN) in traditional Chinese medicine Houpu. The overlapping fluorescence spectrum of MN and HN could be completely separated in the AAILs medium. Experiment parameters (the type and concentration of AAILs, pH values and temperature) were discussed. The detection limits of MN and HN reached 1.46 ng/mL, 0.92 ng/mL and the recovery rates ranged from 98.6%-100.7%, 99.7%-100.6%, respectively. This methods was successfully employed for simultaneously determination of MN and HN in real samples. No significant differences could be found in the results of this method and the pharmacopoeia of People's Republic of China 2015 (Ch.P.2015). The experiment mechanisms were discussed by the Gaussian simulation and fluorescence quantum yield.

  12. Simultaneous determination of nitrogen and phosphorus in cereals using 14 MeV Neutron Activation Analysis

    International Nuclear Information System (INIS)

    Bejarano, R.

    1992-01-01

    A method using 14 MeV neutron activation analysis was developed form non-destructive simultaneous determination of N and P in cereals. The samples were irradiated 5 min. after 0,5 min. decay time. The induced activities were measured using gamma spectrometry with Nal(Tl) well type detector. The accuracy, precision and detection limits obtained are discussed as well as the analytical results for different types of cereals. (Author) 10 refs., 8 tab., 1 fig

  13. Simultaneous determination of sulfamethoxazole and trimethoprim residues on manufacturing equipment surfaces

    OpenAIRE

    Coutinho, Roberto C.; Barbosa, Elder T.; Sena, Marcelo M.; Pérez, Caridad Noda

    2009-01-01

    A cleaning validation method was developed and validated, based on swabbing sampling and simultaneous chromatographic determination of sulfamethoxazole (SMX) and trimethoprim (TMP) residues. The method presented limits of detection of 0.06 mg mL-1 for SMX and 0.09 mg mL-1 for TMP. It was considered selective, precise, accurate and robust according to the guidelines from ANVISA, the Brazilian regulatory agency, and International Conference on Harmonization. Mean swab recovery factors of 98.5% ...

  14. Simultaneous determination of two active components of pharmaceutical preparations by sequential injection method using heteropoly complexes

    Directory of Open Access Journals (Sweden)

    Mohammed Khair E. A. Al-Shwaiyat

    2014-12-01

    Full Text Available New approach has been proposed for the simultaneous determination of two reducing agents based on the dependence of their reaction rate with 18-molybdo-2-phosphate heteropoly complex on pH. The method was automated using the manifold typical for the sequential analysis method. Ascorbic acid and rutin were determined by successive injection of two samples acidified to different pH. The linear range for rutin determination was 0.6-20 mg/L and the detection limit was 0.2 mg/L (l = 1 cm. The determination of rutin was possible in the presence of up to a 20-fold excess of ascorbic acid. The method was successfully applied to the determination of ascorbic acid and rutin in ascorutin tablets. The applicability of the proposed method for the determination of total polyphenol content in natural plant samples was shown.

  15. Simultaneous determination of hydroquinone and catechol at gold nanoparticles mesoporous silica modified carbon paste electrode

    Energy Technology Data Exchange (ETDEWEB)

    Tashkhourian, J., E-mail: tashkhourian@susc.ac.ir [Department of Chemistry, College of Sciences, Shiraz University, Shiraz 71456 (Iran, Islamic Republic of); Daneshi, M.; Nami-Ana, F. [Department of Chemistry, College of Sciences, Shiraz University, Shiraz 71456 (Iran, Islamic Republic of); Behbahani, M.; Bagheri, A. [Department of Chemistry, Shahid Beheshti University, G.C., Evin, Tehran (Iran, Islamic Republic of)

    2016-11-15

    Highlights: • An electrochemical sensor based on gold nanoparticles mesoporous silica modified carbon paste electrode was developed. • The electrode provides an accessible surface for simultaneous determination of hydroquinone and catechol. • Hydroquinone and catechol are highly toxic to both environment and human even at very low concentrations. - Abstract: A new electrochemical sensor based on gold nanoparticles mesoporous silica modified carbon paste electrode (AuNPs-MPS) was developed for simultaneous determination of hydroquinone and catechol. Morphology and structure of the AuNPs-MPS were characterized by transmission electron microscopy, X-ray diffraction and Fourier transform infrared spectroscopy. The electrochemical behavior of hydroquinone and catechol were investigated using square wave voltammetry and the results indicate that the electrochemical responses are improved significantly at the modified electrode. The observed oxidative peaks separation of about 120 mV made possible the simultaneous determination of hydroquinone and catechol in their binary-mixture. Under the optimized condition, a linear dynamic range of 10.0 μM–1.0 mM range for hydroquinone with the detection limit of 1.2 μM and from 30.0 μM–1.0 mM for catechol with the detection limit of 1.1 μM were obtained. The applicability of the method was demonstrated by the recovery studies of hydroquinone and catechol in spiked tap water samples.

  16. Application of different spectrophotometric methods for simultaneous determination of elbasvir and grazoprevir in pharmaceutical preparation

    Science.gov (United States)

    Attia, Khalid A. M.; El-Abasawi, Nasr M.; El-Olemy, Ahmed; Abdelazim, Ahmed H.

    2018-01-01

    The first three UV spectrophotometric methods have been developed of simultaneous determination of two new FDA approved drugs namely; elbasvir and grazoprevir in their combined pharmaceutical dosage form. These methods include simultaneous equation, partial least squares with and without variable selection procedure (genetic algorithm). For simultaneous equation method, the absorbance values at 369 (λmax of elbasvir) and 253 nm (λmax of grazoprevir) have been selected for the formation of two simultaneous equations required for the mathematical processing and quantitative analysis of the studied drugs. Alternatively, the partial least squares with and without variable selection procedure (genetic algorithm) have been applied in the spectra analysis because the synchronous inclusion of many unreal wavelengths rather than by using a single or dual wavelength which greatly increases the precision and predictive ability of the methods. Successfully assay of the drugs in their pharmaceutical formulation has been done by the proposed methods. Statistically comparative analysis for the obtained results with the manufacturing methods has been performed. It is noteworthy to mention that there was no significant difference between the proposed methods and the manufacturing one with respect to the validation parameters.

  17. Validated spectrophotometric methods for simultaneous determination of troxerutin and carbazochrome in dosage form

    Science.gov (United States)

    Khattab, Fatma I.; Ramadan, Nesrin K.; Hegazy, Maha A.; Al-Ghobashy, Medhat A.; Ghoniem, Nermine S.

    2015-03-01

    Four simple, accurate, sensitive and precise spectrophotometric methods were developed and validated for simultaneous determination of Troxerutin (TXN) and Carbazochrome (CZM) in their bulk powders, laboratory prepared mixtures and pharmaceutical dosage forms. Method A is first derivative spectrophotometry (D1) where TXN and CZM were determined at 294 and 483.5 nm, respectively. Method B is first derivative of ratio spectra (DD1) where the peak amplitude at 248 for TXN and 439 nm for CZM were used for their determination. Method C is ratio subtraction (RS); in which TXN was determined at its λmax (352 nm) in the presence of CZM which was determined by D1 at 483.5 nm. While, method D is mean centering of the ratio spectra (MCR) in which the mean centered values at 300 nm and 340.0 nm were used for the two drugs in a respective order. The two compounds were simultaneously determined in the concentration ranges of 5.00-50.00 μg mL-1 and 0.5-10.0 μg mL-1 for TXN and CZM, respectively. The methods were validated according to the ICH guidelines and the results were statistically compared to the manufacturer's method.

  18. Simultaneous all-optical determination of molecular concentration and extinction coefficient.

    Science.gov (United States)

    Cho, Byungmoon; Tiwari, Vivek; Jonas, David M

    2013-06-04

    Absolute molecular number concentration and extinction coefficient are simultaneously determined from linear and nonlinear spectroscopic measurements. This method is based on measurements of absolute femtosecond pump-probe signals. Accounting for pulse propagation, we present a closed form expression for molecular number concentration in terms of absorbance, fluorescence, absolute pump-probe signal, and laser pulse parameters (pulse energy, spectrum, and spatial intensity profile); all quantities are measured optically. As in gravimetric and coulometric determinations of concentration, no standard samples are needed for calibration. The extinction coefficient can then be determined from the absorbance spectrum and the concentration. For fluorescein in basic methanol, the optically determined molar concentrations and extinction coefficients match gravimetric determinations to within 10% for concentrations from 0.032 to 0.540 mM, corresponding to absorbance from 0.06 to 1. In principle, this photonumeric method is extensible to transient chemical species for which other methods are not available.

  19. Simultaneous extractive-photometric determination of Zr and Mo in multicomponent alloys

    International Nuclear Information System (INIS)

    Kutyrev, I.M.; Chernysheva, G.M.; Chebotnikovz, Yu.A.; Basargin, N.N.

    2000-01-01

    Nonaqueous buffer solutions of different acidity are developed for simultaneous photometric determination of Zr and Mo in the extract. Trioctylamine extraction system in toluene - sulfuric acid - molybdenum, zirconium provides selective isolation of the aforementioned elements in one extraction and makes it possible to remove the interfering effect of Fe(2,3), Co(2), Ni(2), Cu(2), Al(3), Ti(4), Cr(3), Mn(2), V(4), Si(4). The reliability of the method is confirmed by determination of the elements in SS123v standard sample [ru

  20. Process monitored spectrophotometric titration coupled with chemometrics for simultaneous determination of mixtures of weak acids.

    Science.gov (United States)

    Liao, Lifu; Yang, Jing; Yuan, Jintao

    2007-05-15

    A new spectrophotometric titration method coupled with chemometrics for the simultaneous determination of mixtures of weak acids has been developed. In this method, the titrant is a mixture of sodium hydroxide and an acid-base indicator, and the indicator is used to monitor the titration process. In a process of titration, both the added volume of titrant and the solution acidity at each titration point can be obtained simultaneously from an absorption spectrum by least square algorithm, and then the concentration of each component in the mixture can be obtained from the titration curves by principal component regression. The method only needs the information of absorbance spectra to obtain the analytical results, and is free of volumetric measurements. The analyses are independent of titration end point and do not need the accurate values of dissociation constants of the indicator and the acids. The method has been applied to the simultaneous determination of the mixtures of benzoic acid and salicylic acid, and the mixtures of phenol, o-chlorophenol and p-chlorophenol with satisfactory results.

  1. Simultaneous in-line concentration for spectrophotometric determination of cations and anions

    Directory of Open Access Journals (Sweden)

    Rocha Fábio R. P

    2004-01-01

    Full Text Available A flow system is proposed for simultaneous in-line concentration of cations and anions. A sliding-bar commutator was employed to insert an anion and a cation exchange column into a flowing sample stream for serial retention of the analytes. In the injector alternative position, different solutions flowed through the columns for parallel elution of the species in different analytical paths. Three-way solenoid valves allowed the intermittent reagent introduction in the sample zones. Signals were measured by employing two flow-through LED-based detectors. The simultaneous retention of the sample zones in coiled reactors can be also performed to increase the residence time and the analyte conversion rate. The analytical potentiality was demonstrated by the in-line concentration of ammonium and phosphate followed by spectrophotometric detection. For a 90 s loading time, the sampling rate was estimated as 40 determinations per hour, which is three-fold higher than the obtained without performing the tasks simultaneously. Enrichment factors of 8.0 and 18 were estimated for phosphate and ammonium, respectively, yielding detection limits of 1 mg L-1 PO4(3- and 1 mg L-1 NH4+ (99.7% confidence level. The reagent consumption was lower than 2 mg per determination. Results for freshwater samples agreed with the obtained by reference APHA procedures at the 95% confidence level.

  2. Simultaneous determination of four food allergens using compact disc immunoassaying technology.

    Science.gov (United States)

    Badran, Ahmed Ali; Morais, Sergi; Maquieira, Ángel

    2017-03-01

    A multiplex competitive microimmunoassay for the simultaneous determination of gliadin, casein, β-lactoglobulin, and ovalbumin is presented. The assay in microarray format is performed on a DVD where the allergens are physisorbed on the polycarbonate surface of the disc. The immunointeraction is detected using a mixture of specific gold-labeled antibodies and the signal amplified with the silver enhancement method. The optical density of the precipitate, read by a DVD drive, is related to the concentration of the four allergens in sample. An optimized protocol for the simultaneous extraction of the allergen proteins from food samples is also addressed. The suitability of the method is demonstrated for the simultaneous quantitative extraction and determination of the targeted allergens in spiked baby foods, juices, and beers. The sensitivity (EC50) of the multiplexed assay was 0.04, 0.40, 0.08, and 0.16 mg L -1 for gliadin, casein, β-lactoglobulin, and ovalbumin, respectively, and the recovery results from the analysis of food samples ranged from 72 to 117%. A portable, easy-to-use, array-based bioanalytical method is developed for quantification of food allergens with a limit of detection below the accepted levels of the international legislations, which allows promotion of food safety and quality. Graphical abstract GLI Gliadin, CAS Casein, β-LAC β-lactoglobulin, OVA Ovalbumin.

  3. Simultaneous Absorptance and Thermal-Diffusivity Determination of Optical Components with Laser Calorimetry Technique

    Science.gov (United States)

    Wang, Yanru; Li, Bincheng

    2012-11-01

    The laser calorimetry (LCA) technique is used to determine simultaneously the absorptances and thermal diffusivities of optical components. An accurate temperature model, in which both the finite thermal conductivity and the finite sample size are taken into account, is employed to fit the experimental temperature data measured with an LCA apparatus for a precise determination of the absorptance and thermal diffusivity via a multiparameter fitting procedure. The uniqueness issue of the multiparameter fitting is discussed in detail. Experimentally, highly reflective (HR) samples prepared with electron-beam evaporation on different substrates (BK7, fused silica, and Ge) are measured with LCA. For the HR-coated sample on a fused silica substrate, the absorptance is determined to be 15.4 ppm, which is close to the value of 17.6 ppm, determined with a simplified temperature model recommended in the international standard ISO11551. The thermal diffusivity is simultaneously determined via multiparameter fitting to be approximately 6.63 × 10-7 m2 · s-1 with a corresponding square variance of 4.8 × 10-4. The fitted thermal diffusivity is in reasonably good agreement with the literature value (7.5 × 10-7 m2 · s -1). Good agreement is also obtained for samples with BK7 and Ge substrates.

  4. Simultaneous determination of butyltin and phenyltin species in sediments using ultrasound-assisted leaching

    Energy Technology Data Exchange (ETDEWEB)

    Carpinteiro, J.; Rodriguez, I.; Cela, R. [Dpto. Quimica Analitica, Nutricion y Bromatologia, Universidad de Santiago de Compostela (Spain)

    2001-08-01

    A fast and simple procedure is presented for the simultaneous leaching of butyl (mono, di and tributyl) and phenyl organotin species from sediment samples. Leached compounds are further ethylated with sodium tetraethylborate in aqueous medium, and analyzed by gas chromatography. After testing the stability of triphenyltin under different extraction conditions, ultrasound-assisted leaching at room temperature in the presence of acetic acid was been proposed as an extraction procedure compatible with the simultaneous determination of phenyl- and butyltin compounds in sediments. Recoveries between 70 and 90% were obtained for phenyl species in spiked samples prepared in the laboratory. Results for butyltin species were validated by use of the reference material PACS-2. Quantification limits, using GC-MIP-AES as measurement technique, were approximately 5-10 ng g{sup -1}. Precision in the consecutive analysis of three sediment samples varied between 3 and 10%. (orig.)

  5. Simultaneous Determination of Cobalt (II and Nickel (II By First Order Derivative Spectrophotometry in Micellar Media

    Directory of Open Access Journals (Sweden)

    Rajni Rohilla

    2012-01-01

    Full Text Available A first-derivative spectrophotometry method for the simultaneous determination of Co (II and Ni (II with Alizarin Red S in presence of Triton X-100 is described. Measurements were made at the zero-crossing wavelengths at 549.0 nm for Co (II and 546.0 nm for Ni (II. The linearity is obtained in the range of 0.291- 4.676 μg/ml of Ni (II and 0.293- 4.124 μg/ml of Co (II in the presence of each other by using first derivative spectrophotometric method. The possible interfering effects of various ions were studied. The validity of the method was examined by using synthetic mixtures of Co (II and Ni (II. The developed derivative procedure, using the zero crossing technique, has been successfully applied for the simultaneous analysis of Co (II and Ni (II in spiked water samples.

  6. New highly sensitive method of simultaneous instrumental neutron activation determination of 12 microelements in vine

    International Nuclear Information System (INIS)

    Shoniya, N.I.

    1977-01-01

    The main principles and methods of simultaneous multi-element instrumental neutron activation determination of microelements in vine seeds are presented. The methods permit to carry out quantitative evaluation for every single corn of the seeds. It is shown that the method of instrumental neutron activation analysis with the utilization of a semiconductor spectrometer of high resolution and mini electronic computer permit to carry out serial determinations of 12 microelements in the individual corns of vine seeds of different sorts. This method will permit to determine the missing or excess content of this or that biologically important microelement in soils, plants, fruit and genetic material - seeds, and so to determine the optimum conditions of growing plants by applying microelement fertilizers as extra nutrient means

  7. Sensitive double-antibody method for simultaneous determination of insulin and growth hormone

    International Nuclear Information System (INIS)

    Koparanova, O.; Sotirov, G.; Tyrkolev, N.

    1982-01-01

    A method is described for simultaneous determination of insulin and growth hormone in one sample, using double-antibody technique. The method is characterized by appreciable sensitivity (2.5 μE/ml for insulin and a.2 ng/ml for growth hormone), exactness (variation quotient 6-16 per cent) and reproducibility (96.9-117 per cent). There was no statistically significant difference in the insulin and growth hormone values of the same sera, determined by the here suggested and the standard methods. The necessary test material for examination of either hormone is minimal (0.2 ml). One may thus extend the possibilities for radioimmunologic determination of insulin and growth hormone, when only minor amounts of serum or other biological fluid are available. The method is also less time consuming. Results are reported of statistical processing of an experimental model and different sera determined by the standard method and the one described by the authors. (author)

  8. Precise simultaneous determination of zirconium and hafnium in silicate rocks, meteorites and lunar samples. [Neutron reactions

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, P A; Garg, A N; Ehmann, W D [Kentucky Univ., Lexington (USA). Dept. of Chemistry

    1977-01-01

    A precise, sensitive and rapid analytical technique has been developed for the simultaneous determination of Zr and Hf in natural silicate matrices. The technique is based on radiochemical neutron activation analysis and employs a rapid fusion dissolution of the sample and simultaneous precipitation of the Zr-Hf pair with p-hydroxybenzene arsenic acid in an acidic medium. The indicator radionuclides, /sup 95/Zr and /sup 181/Hf, are counted and the /sup 95/Zr activity is corrected for the contribution from U fission. The chemical yields of the radiochemical separation are based on Hf carrier. The yield is determined by reactivation of the processed samples and standards with a /sup 252/Cf isotopic neutron source and by counting the 18.6 sec half-life sup(179m)Hf. The RNAA procedure for Zr and Hf has been shown to be precise and accurate for natural silicate samples, based on replicate analyses of samples containing Zr in the range of 1 ..mu..g/g to over 600 ..mu..g/g. The procedure is relatively rapid with a total chemical processing time of approximately 3 hours. At least 4 samples are processed simultaneously. Ten additional elements (Fe, Cr, Co, Sc, Eu, La, Lu, Ce, Th and Tb) can be determined by direct Ge(Li) spectrometry (INAA) on the samples prior to dissolution for the RNAA determination of Zr and Hf. Corrections for the U fission contribution can be made on the basis of the known U content or from the INAA Th content, based on the relatively constant natural Th/U ratio.

  9. Amplified nanostructure electrochemical sensor for simultaneous determination of captopril, acetaminophen, tyrosine and hydrochlorothiazide

    Energy Technology Data Exchange (ETDEWEB)

    Karimi-Maleh, Hassan, E-mail: h.karimi.maleh@gmail.com [Department of Chemistry, Graduate University of Advanced Technology, Kerman (Iran, Islamic Republic of); Ganjali, Mohammad R.; Norouzi, Parviz; Bananezhad, Asma [Center of Excellence in Electrochemistry, Faculty of Chemistry, University of Tehran, Tehran (Iran, Islamic Republic of)

    2017-04-01

    A novel nanomaterial-based voltammetric sensor has been developed for use a highly sensitive tool for the simultaneous determination of captopril (CA), acetaminophen (AC), tyrosine (TY) and hydrochlorothiazide (HCTZ). The device is based on the application of NiO/CNTs and (2-(3,4-dihydroxyphenethyl)isoindoline-1,3-dione) (DPID) to modify carbon paste electrodes. The NiO/CNTs nanocomposite was synthesized through a direct chemical precipitation approach and was characterized with X-ray powder diffraction (XRD), and scanning electron microscopy (SEM). The NiO/CNTs/DPID/CPEs were found to facilitate the analysis of CA, AC, TY and HCTZ in the concentration ranges of 0.07–200.0, 0.8–550.0, 5.0–750.0 and 10.0–600.0 μM with the respective detection limits of 9.0 nM, 0.3 μM, 1.0 μM and 5.0 μM. The developed NiO/CNTs/DPID/CPEs were used for the determination of the mentioned analytes in pharmaceutical and biological real samples. - Graphical abstract: In this study a novel sensor based on NiO/CNTs and (2-(3,4-dihydroxyphenethyl)isoindoline-1,3-dione) (DPID) modified carbon paste electrode fabricated for simultaneous determination of captopril, acetaminophen, tyrosine and hydrochlorothiazide for the first time. - Highlights: • Fabrication of NiO/CNTs and new catechol derivative modified carbon paste electrode • Good ability of proposed sensor for biological and pharmaceutical analysis • Simultaneous determination captopril, acetaminophen, tyrosine and hydrochlorothiazide.

  10. Fast determination of strontium-89 and strontium-90 by simultaneous Cerencov- and Proportional-Counting; Schnelle Bestimmung von Strontium-89 und Strontium-90 mittels simultaner Cerenkov- und Proportionalzaehlrohrmessung

    Energy Technology Data Exchange (ETDEWEB)

    Laerbusch, Karin; Wiezorek, Claus [Chemisches und Veterinaeruntersuchungsamt MEL, Muenster (Germany)

    2014-01-20

    The presented method for simultaneous determination of Sr 89 and Sr 90 combines the techniques of Cerencov- and Proportional-Counting. Due to the low limit of detection of the latter technique, the method is very sensitive for the total radiostrontium. The distribution among two measurement devices offers the advantage of time saving.

  11. Simultaneous determination of copper, lead and cadmium by cathodic adsorptive stripping voltammetry using artificial neural network

    International Nuclear Information System (INIS)

    Ensafi, Ali A.; Khayamian, T.; Benvidi, A.; Mirmomtaz, E.

    2006-01-01

    In this work, simultaneous determination of two groups of elements consisting of Pb(II)-Cd(II) and Cu(II)-Pb(II)-Cd(II) using adsorptive cathodic stripping voltammetry are described. The method is based on accumulation of these metal ions on mercury electrode using xylenol orange as a suitable complexing agent. The potential was scanned to the negative direction and the differential pulse stripping voltammograms were recorded. The instrumental and chemical factors were optimized using artificial neural network. The optimized conditions were obtained in pH of 5.5, xylenol orange concentration of 4.0 μM, accumulation potential of -0.50 V, accumulation time of 30 s, scan rate of 10 mV/s and pulse height of 70 mV. The relationship between the peak current versus concentration was linear over the range of 5.0-150.0 ng ml -1 for cadmium and 5.0-150.0 ng ml -1 for lead. The limits of detection were 0.98 and 1.18 ng ml -1 for lead and cadmium ions, respectively. In simultaneous determination of Cu(II), Pb(II) and Cd(II) there are inter-metallic interactions, which result a non-linear relationship between the peak current and the ionic concentration for each of the element. Therefore, an artificial neural network was used as the multivariate calibration method. The ANN was constructed with three neurons as the output layer for the simultaneous determination of the three elements. The constructed model was able to predict the concentration of the elements in the ranges of 1.0-50.0, 5.0-200.0 and 10.0-200.0 ng ml -1 , for Cu(II), Pb(II) and Cd(II), respectively

  12. Determinants of long-term outcome in patients undergoing simultaneous resection of synchronous colorectal liver metastases.

    Directory of Open Access Journals (Sweden)

    Qi Lin

    Full Text Available BACKGROUND: It remains unclear which patients can benefit from simultaneous resection of synchronous colorectal liver metastases (SCRLMs. This study aimed to examine the prognostic value of patient- and tumor-related factors in predicting long-term outcomes of patients undergoing simultaneous resection of SCRLMs and to help patients select a suitable therapeutic regimen and proper surveillance. METHODS: Clinicopathological and outcome data of 154 consecutive SCRLM patients who underwent simultaneous resection between July 2003 and July 2013 were collected from our prospectively established SCRLM data and analyzed with univariate and multivariate methods, and the prognostic index (PI was formulated based on the regression coefficients (β of the Cox model. The patients were classified into high- and low-risk groups according to the PI value; the cut-off point was the third quartile. RESULTS: The 5-year overall survival rate was 46%, and the 5-year disease-free survival rate was 35%. Five factors were found to be independent predictors of poor overall survival (OS by multivariate analysis: positive lymph node status, vascular invasion, BRAF mutation, the distribution of bilobar liver metastases (LMs and non-R0 resection of LMs. Compared to low PI (≤5.978, high PI (>5.978 was highly predictive of shorter OS. Three factors were found to be independent predictors of poor disease-free survival (DFS by multivariate analysis: tumor deposits, BRAF mutation and bilobar LM distribution. We also determined the PI for DFS. Compared to low PI (≤2.945, high PI (>2.945 was highly predictive of shorter DFS. CONCLUSIONS: Simultaneous resection of SCRLM may lead to various long-term outcomes. Patients with low PI have longer OS and DFS, while those with high PI have shorter OS and DFS. Thus, patients with high PI may receive more aggressive treatment and intensive surveillance, This model needs further validation.

  13. Status of sennosides content in various Indian herbal formulations: Method standardization by HPTLC

    Directory of Open Access Journals (Sweden)

    Md. Wasim Aktar

    2008-06-01

    Full Text Available Several poly-herbal formulations containing senna (Cassia angustifolia leaves are available in the Indian market for the treatment of constipation. The purgative effect of senna is due to the presence of two unique hydroxy anthracene glycosides sennosides A and B. A HPTLC method for the quantitative analysis of sennosides A and B present in the formulation has been developed. Methanol extract of the formulations was analyzed on a silica gel 60 GF254 HPTLCplates with spot visualization under UV and scanning at 350 nm in absorption/ reflection mode. Calibration curves were found to be linear in the range 200-1000 ηg. The correlation coefficients were found to be 0.991 for sennoside A and 0.997 for sennoside B. The average recovery rate was 95% for sennoside A and 97% for sennoside B showing the reliability and reproducibility of the method. Limit of detection and quantification were determined as 0.05 and 0.25 μg/g respectively. The validity of the method with respect to analysis was confirmed by comparing the UV spectra of the herbal formulations with that of the standard within the same Rf window. The analysis revealed a significant variation in sennosides content.

  14. Phytochemical analysis and standardization of Strychnos nux-vomica extract through HPTLC techniques

    Directory of Open Access Journals (Sweden)

    Dinesh Kumar Patel

    2012-05-01

    Full Text Available Objective: The objective is to develop a noval qualitative and quantitative method by which we can determine different phytoconstituents of Strychnos nux-vomica L. Methods: To profile the phyconstituents of Strychnos nux-vomica, in the present study hydroalcoholic extract of Strychnos nux-vomica was subjected to preliminary phytochemical analysis, antimicrobial activities against certain pathogenic microorganisms, solubility test, loss on drying and pH value. Extract was also subjected to the quantitative analysis including total phenol, flavonoid and heavy metal analysis. Quantitative analysis was performed through HPTLC methods using strychnine and brucine as a standard marker. Results: Phytochemical analysis revealed the presence of alkaloid, carbohydrate, tannin, steroid, triterpenoid and glycoside in the extract. Total flavonoid and phenol content of Strychnos nux-vomica L extract was found to be 0.40 % and 0.43%. Result showed that the level of heavy metal (lead, arsenic, mercury and cadmium complie the standard level. Total bacterial count, yeast and moulds contents were found to be under the limit whereas E. coli and salmonella was found to be absent in the extract. Content of strychnine and brucine were found to be 4.75% and 3.91%. Conclusions: These studies provide valluable information for correct identification and selection of the drug from various adulterations. In future this study will be helpful for the quantitative analysis as well as standardization of the Strychnos nux-vomica L.

  15. Radium 226 and uranium isotopes simultaneously determination in water samples using liquid scintillation counter

    International Nuclear Information System (INIS)

    Al-Masri, M.S.; Al-Akel, B.; Saaid, S.; Nashawati, A.

    2007-04-01

    In this work a method has been developed to determine simultaneously Radium 226 and Uranium isotopes in water samples by low back ground Liquid Scintillation Counter. Radium 226 was determined by its progeny Polonium 214 after one month of sample storage in order to achieve the equilibrium between Radium 226 and Polonium 214. Uranium isotopes were determined by subtracting Radium 226 activity from total alpha activity. The method detection limits were 0.049 Bq/L and 0.176 Bq/L for Radium 226 and Uranium isotopes respectively. The repeatability limits were ± 0.32 Bq/L and ± 0.9 Bq/L for Radium 226 and Uranium isotopes respectively. While relative errors were % 9.5 and %18.2 for Radium 226 and Uranium isotopes respectively. On the other hand, the report presented the results of different standard and natural samples.(author)

  16. Simultaneous and rapid determination of multiple component concentrations in a Kraft liquor process stream

    Science.gov (United States)

    Li, Jian [Marietta, GA; Chai, Xin Sheng [Atlanta, GA; Zhu, Junyoung [Marietta, GA

    2008-06-24

    The present invention is a rapid method of determining the concentration of the major components in a chemical stream. The present invention is also a simple, low cost, device of determining the in-situ concentration of the major components in a chemical stream. In particular, the present invention provides a useful method for simultaneously determining the concentrations of sodium hydroxide, sodium sulfide and sodium carbonate in aqueous kraft pulping liquors through use of an attenuated total reflectance (ATR) tunnel flow cell or optical probe capable of producing a ultraviolet absorbency spectrum over a wavelength of 190 to 300 nm. In addition, the present invention eliminates the need for manual sampling and dilution previously required to generate analyzable samples. The inventive method can be used in Kraft pulping operations to control white liquor causticizing efficiency, sulfate reduction efficiency in green liquor, oxidation efficiency for oxidized white liquor and the active and effective alkali charge to kraft pulping operations.

  17. Radioactivation method for simultaneous determination of nitrogen, phosphorus and potassium content in plants and fertilizers

    International Nuclear Information System (INIS)

    Kovtun, J.L.; Miroshnikova, N.N.; Saveliev, I.B.; Sidorov, A.V.; Srapeniants, R.A.; Tsagolov, K.S.

    1981-01-01

    According to the invention, the radioactivation method for simultaneous determination of the nitrogen, phosphorus and potassium content in plants and fertilizers consists in exposing samples to be analyzed and standard samples to neutron irradiation and recording the spectra of the gamma radiation induced in said samples, whereupon the samples are laid aside for a period of time determined by the half-life of the interfering isotope. This is followed by again recording the spectra of the samples being analyzed and of the standard samples and superposing the first and second spectra of the samples being analyzed and of the standard samples. These spectra are then shifted relative to each other along the energy axis, and the contents of the elements being analyzed are determined by thus comparing the spectra of the samples being analyzed and of the standard samples

  18. Simultaneous determination of 56 Mn and 187W in neutron activated steels

    International Nuclear Information System (INIS)

    Melo, M.C. de

    1982-01-01

    The simultaneous determination of the count rates due to 56 Mn and 187 W in the activation analysis of steel samples was carried out through exponential regression using least square fitting. The regression coefficients obtained corresponded to the initial count rates of 56 Mn and 187 W. Later on, the count rates of 56 Mn were correlated to the manganese content in the samples and to the count rates of the same radionuclide, obtained in a region of the gamma spectrum where only 56 Mn was apparent. The correlation coefficients were respectively .968 and .99997, thus demonstrating the applicability of the methodology adopted herein. (Author) [pt

  19. Simultaneous Determination of Ciprofloxacin Hydrochloride and Dexamethasone Sodium Phosphate in Eye Drops by HPLC

    OpenAIRE

    Katakam, Prakash; Sireesha, Karanam R.

    2012-01-01

    A liquid chromatographic method was developed and validated for the simultaneous determination of ciprofloxacin hydrochloride and dexamethasone sodium phosphate in bulk and pharmaceutical formulations. Optimum separation was achieved in less than 5 min using a C18 column (250 mmx4.6 mm i.d, 5μ particle size) by isocratic elution. The mobile phase consisting of a mixture of mixed phosphate buffer (pH 4) and acetonitrile (65:35, v/v) was used. Column effluents were monitored at 254 nm at a flow...

  20. Simultaneous determination of 18 pyrethroids in indoor air by gas chromatography/mass spectrometry.

    Science.gov (United States)

    Yoshida, Toshiaki

    2009-06-26

    An analytical method was developed for the simultaneous measurement of 18 pyrethroids (allethrin, bifenthrin, cyfluthrin, cypermethrin, cyphenothrin, deltamethrin, empenthrin, fenpropathrin, furamethrin, imiprothrin, metofluthrin, permethrin, phenothrin, prallethrin, profluthrin, resmethrin, tetramethrin and transfluthrin) in indoor air. The pyrethroids were collected for 24 h using a combination of adsorbents (quartz fiber filter disk and Empore C18 disk), with protection from light, and then extracted with acetone, concentrated, and analyzed by GC/MS. They could be determined accurately and precisely (detection limits: ca. 1 ng/m(3)). The collected pyrethroid samples could be stored for up to one month at 4 degrees C in a refrigerator.

  1. Derivative spectrophotometric method for simultaneous determination of clindamycin phosphate and tretinoin in pharmaceutical dosage forms.

    Science.gov (United States)

    Barazandeh Tehrani, Maliheh; Namadchian, Melika; Fadaye Vatan, Sedigheh; Souri, Effat

    2013-04-10

    A derivative spectrophotometric method was proposed for the simultaneous determination of clindamycin and tretinoin in pharmaceutical dosage forms. The measurement was achieved using the first and second derivative signals of clindamycin at (1D) 251 nm and (2D) 239 nm and tretinoin at (1D) 364 nm and (2D) 387 nm.The proposed method showed excellent linearity at both first and second derivative order in the range of 60-1200 and 1.25-25 μg/ml for clindamycin phosphate and tretinoin respectively. The within-day and between-day precision and accuracy was in acceptable range (CVpharmaceutical dosage form.

  2. Simultaneous determination of Albendazol and Triclabendazole in Triclazol 22 suspension for veterinary purposes

    International Nuclear Information System (INIS)

    Garcia Penna, Caridad Margarita; Gafas Leyva, Maite; Rosales Bosch, Karina

    2013-01-01

    To validate the analytical method for simultaneous determination of triclabendazole and al bendazole in triclazol 22 suspension for quality control. For quantitation of the active principle in the final product, the separation was performed through a liquid chromatographic column Lichrosorb RP-18 (5 μm) (250 x 4 mm), with ultraviolet detection range of 298 nm, by using a mobile phase of acetonitrile: ammonium acetate buffer solution of ph 6.6 (70:30); the quantitation was made against a reference sample by means of the external standard method

  3. Simultaneous determination of aliphatic hydrocarbons, PCBs and PCTs in pork liver by gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Gonzalez-Barros, C [Dept. de Quimica Analitica, Nutricion y Bromatologia, Area Nutricion y Bromatologia, Facultad de Farmacia, Santiago de Compostela (Spain); Alvarez Pineiro, M E [Inst. de Investigacion y Analisis Alimentarios, Lab. de Bromatologia, Facultad de Farmacia, Santiago de Compostela (Spain); Simal Lozano, J [Dept. de Quimica Analitica, Nutricion y Bromatologia, Area Nutricion y Bromatologia, Facultad de Farmacia, Santiago de Compostela (Spain); Lage Yusty, M A [Inst. de Investigacion y Analisis Alimentarios, Lab. de Bromatologia, Facultad de Farmacia, Santiago de Compostela (Spain)

    1996-10-01

    A multicomponent extraction/concentration procedure has been developed for the enrichment of PCBs, PCTs and aliphatic hydrocarbons (pristane, C{sub 18}, C{sub 19}, C{sub 20}, C{sub 22}, C{sub 24}, C{sub 28}, C{sub 32} and C{sub 36}) in pork liver. These components of the enriched extract were then simultaneously determined by gas chromatography. Mean recoveries ranged from 81.5% for pristane to 93% for PCBs; CV % (0.9-6.7) indicated the method to be both precise and reproducible. (orig.)

  4. H-point standard additions method for simultaneous determination of sulfamethoxazole and trimethoprim in pharmaceutical formulations and biological fluids with simultaneous addition of two analytes

    Science.gov (United States)

    Givianrad, M. H.; Saber-Tehrani, M.; Aberoomand-Azar, P.; Mohagheghian, M.

    2011-03-01

    The applicability of H-point standard additions method (HPSAM) to the resolving of overlapping spectra corresponding to the sulfamethoxazole and trimethoprim is verified by UV-vis spectrophotometry. The results show that the H-point standard additions method with simultaneous addition of both analytes is suitable for the simultaneous determination of sulfamethoxazole and trimethoprim in aqueous media. The results of applying the H-point standard additions method showed that the two drugs could be determined simultaneously with the concentration ratios of sulfamethoxazole to trimethoprim varying from 1:18 to 16:1 in the mixed samples. Also, the limits of detections were 0.58 and 0.37 μmol L -1 for sulfamethoxazole and trimethoprim, respectively. In addition the means of the calculated RSD (%) were 1.63 and 2.01 for SMX and TMP, respectively in synthetic mixtures. The proposed method has been successfully applied to the simultaneous determination of sulfamethoxazole and trimethoprim in some synthetic, pharmaceutical formulation and biological fluid samples.

  5. Application of Scion image software to the simultaneous determination of curcuminoids in turmeric (Curcuma longa).

    Science.gov (United States)

    Sotanaphun, Uthai; Phattanawasin, Panadda; Sriphong, Lawan

    2009-01-01

    Curcumin, desmethoxycurcumin and bisdesmethoxycurcumin are bioactive constituents of turmeric (Curcuma longa). Owing to their different potency, quality control of turmeric based on the content of each curcuminoid is more reliable than that based on total curcuminoids. However, to perform such an assay, high-cost instrument is needed. To develop a simple and low-cost method for the simultaneous quantification of three curcuminoids in turmeric using TLC and the public-domain software Scion Image. The image of a TLC chromatogram of turmeric extract was recorded using a digital scanner. The density of the TLC spot of each curcuminoid was analysed by the Scion Image software. The density value was transformed to concentration by comparison with the calibration curve of standard curcuminoids developed on the same TLC plate. The polynomial regression data for all curcuminoids showed good linear relationship with R(2) > 0.99 in the concentration range of 0.375-6 microg/spot. The limits of detection and quantitation were 43-73 and 143-242 ng/spot, respectively. The method gave adequate precision, accuracy and recovery. The contents of each curcuminoid determined using this method were not significantly different from those determined using the TLC densitometric method. TLC image analysis using Scion Image is shown to be a reliable method for the simultaneous analysis of the content of each curcuminoid in turmeric.

  6. [Simultaneous determination of seven residual solvents in bovis calculus artifactus by headspace gas chromatography].

    Science.gov (United States)

    Chi, Shuyao; Wu, Dike; Sun, Jinhong; Ye, Ruhan; Wang, Xiaoyan

    2014-05-01

    A headspace gas chromatography (HS-GC) method was developed for the simultaneous determination of seven residual solvents (petroleum ether (60-90 degrees C), acetone, ethyl acetate, methanol, methylene chloride, ethanol and butyl acetate) in bovis calculus artifactus. The DB-WAX capillary column and flame ionization detector (FID) were used for the separation and detection of the residual solvents, and the internal standard method was used for the quantification. The chromatographic conditions, such as equilibrium temperature and equilibrium time, were optimized. Under the optimized conditions, all of the seven residual solvents showed good linear relationships with good correlation coefficients (not less than 0.999 3) in the prescribed concentration range. At three spiked levels, the recoveries for the seven residual solvents were 94.7%-105.2% with the relative standard deviations (RSDs) less than 3.5%. The limits of detection (LODs) of the method were 0.43-5.23 mg/L, and the limits of quantification (LOQs) were 1.25-16.67 mg/L. The method is simple, rapid, sensitive and accurate, and is suitable for the simultaneous determination of the seven residual solvents in bovis calculus artifactus.

  7. Simultaneous Determination of Ciprofloxacin Hydrochloride and Dexamethasone Sodium Phosphate in Eye Drops by HPLC

    Directory of Open Access Journals (Sweden)

    Prakash Katakam

    2012-01-01

    Full Text Available A liquid chromatographic method was developed and validated for the simultaneous determination of ciprofloxacin hydrochloride and dexamethasone sodium phosphate in bulk and pharmaceutical formulations. Optimum separation was achieved in less than 5 min using a C18 column (250 mmx4.6 mm i.d, 5μ particle size by isocratic elution. The mobile phase consisting of a mixture of mixed phosphate buffer (pH 4 and acetonitrile (65:35, v/v was used. Column effluents were monitored at 254 nm at a flow rate of 1ml/min. Retention times of ciprofloxacin hydrochloride and dexamethasone sodium phosphate were 2.0 and 3.16 min respectively. The linearity of ciprofloxacin hydrochloride and dexamethasone sodium phosphate was in the range of 3-18 μg/ml and 1-6 μg/ml respectively. Developed method was economical in terms of the time taken and amount of solvent consumed for each analysis. The method was validated and successfully applied to the simultaneous determination of ciprofloxacin hydrochloride and dexamethasone sodium phosphate in bulk and pharmaceutical formulations.

  8. Simultaneous spectrophotometric determination of uranium and zirconium using cloud point extraction and multivariate methods

    International Nuclear Information System (INIS)

    Ghasemi, Jahan B.; Hashemi, Beshare; Shamsipur, Mojtaba

    2012-01-01

    A cloud point extraction (CPE) process using the nonionic surfactant Triton X-114 to simultaneous extraction and spectrophotometric determination of uranium and zirconium from aqueous solution using partial least squares (PLS) regression is investigated. The method is based on the complexation reaction of these cations with Alizarin Red S (ARS) and subsequent micelle-mediated extraction of products. The chemical parameters affecting the separation phase and detection process were studied and optimized. Under the optimum experimental conditions (i.e. pH 5.2, Triton X-114 = 0.20%, equilibrium time 10 min and cloud point 45 C), calibration graphs were linear in the range of 0.01-3 mg L -1 with detection limits of 2.0 and 0.80 μg L -1 for U and Zr, respectively. The experimental calibration set was composed of 16 sample solutions using an orthogonal design for two component mixtures. The root mean square error of predictions (RMSEPs) for U and Zr were 0.0907 and 0.1117, respectively. The interference effect of some anions and cations was also tested. The method was applied to the simultaneous determination of U and Zr in water samples.

  9. Study on performance of a simultaneous spectrometer of ICP emission source for the determination of the major elements in rocks

    International Nuclear Information System (INIS)

    Vieira, M.D.

    1987-01-01

    The optimization of operational parameters of a simultaneous spectrometer coupled to an ICP excitation source in order to establish an analytical method for the simultaneous determination of the major elements in rocks is studied. The mutual spectral interferences, calibration curves for the acid and saline matrix and the internal standard method with ytrium are analyzed. (M.J.C.) [pt

  10. New method for simultaneous determination of 55Fe and 59Fe in blood serum samples

    International Nuclear Information System (INIS)

    Saukkonen, H.; Uhlenius, R.

    1978-01-01

    Routine methods for the measurement of 55 Fe and 59 Fe activities in biological samples are frequently required in metabolic studies of iron. A new simple method for the simultaneous determination of 59 Fe and 55 Fe concentration in 5 cm 3 samples of blood is described and carefully evaluated. Before the measurement of the activity, organic matter was eliminated by HNO 3 -HClO 4 wet ashing and iron was electroplated onto a copper plate. The accuracy of results was studied by assessing samples, which contained known amounts of radioactivity and determining the counts per nanocurie in each case. The accuracy of the results of 59 Fe and 55 Fe determinations was found to be about 5%. The method has been routinely used to determine iron resorption in patients using the double isotope method. The determination proved to be satisfactory and not too laborious. When performing the yield determination there is a way of detecting and correcting mistakes or incompleteness in different stages of the measurement, thus leading to a high degree of reliability. (T.G.)

  11. Single-acquisition method for simultaneous determination of extrinsic gamma-camera sensitivity and spatial resolution

    Energy Technology Data Exchange (ETDEWEB)

    Santos, J.A.M. [Servico de Fisica Medica, Instituto Portugues de Oncologia Francisco Gentil do Porto, E.P.E., Rua Dr. Antonio Bernardino de Almeida, 4200-072 Porto (Portugal)], E-mail: a.miranda@portugalmail.pt; Sarmento, S. [Servico de Fisica Medica, Instituto Portugues de Oncologia Francisco Gentil do Porto, E.P.E., Rua Dr. Antonio Bernardino de Almeida, 4200-072 Porto (Portugal); Alves, P.; Torres, M.C. [Departamento de Fisica da Universidade do Porto, Rua do Campo Alegre 687, 4169-007 Porto (Portugal); Bastos, A.L. [Servico de Medicina Nuclear, Instituto Portugues de Oncologia Francisco Gentil do Porto, E.P.E., Rua Dr. Antonio Bernardino de Almeida, 4200-072 Porto (Portugal); Ponte, F. [Servico de Fisica Medica, Instituto Portugues de Oncologia Francisco Gentil do Porto, E.P.E., Rua Dr. Antonio Bernardino de Almeida, 4200-072 Porto (Portugal)

    2008-01-15

    A new method for measuring simultaneously both the extrinsic sensitivity and spatial resolution of a gamma-camera in a single planar acquisition was implemented. A dual-purpose phantom (SR phantom; sensitivity/resolution) was developed, tested and the results compared with other conventional methods used for separate determination of these two important image quality parameters. The SR phantom yielded reproducible and accurate results, allowing an immediate visual inspection of the spatial resolution as well as the quantitative determination of the contrast for six different spatial frequencies. It also proved to be useful in the estimation of the modulation transfer function (MTF) of the image formation collimator/detector system at six different frequencies and can be used to estimate the spatial resolution as function of the direction relative to the digital matrix of the detector.

  12. Single-acquisition method for simultaneous determination of extrinsic gamma-camera sensitivity and spatial resolution

    International Nuclear Information System (INIS)

    Santos, J.A.M.; Sarmento, S.; Alves, P.; Torres, M.C.; Bastos, A.L.; Ponte, F.

    2008-01-01

    A new method for measuring simultaneously both the extrinsic sensitivity and spatial resolution of a gamma-camera in a single planar acquisition was implemented. A dual-purpose phantom (SR phantom; sensitivity/resolution) was developed, tested and the results compared with other conventional methods used for separate determination of these two important image quality parameters. The SR phantom yielded reproducible and accurate results, allowing an immediate visual inspection of the spatial resolution as well as the quantitative determination of the contrast for six different spatial frequencies. It also proved to be useful in the estimation of the modulation transfer function (MTF) of the image formation collimator/detector system at six different frequencies and can be used to estimate the spatial resolution as function of the direction relative to the digital matrix of the detector

  13. Simultaneous determination of rutin and ascorbic acid in a sequential injection lab-at-valve system.

    Science.gov (United States)

    Al-Shwaiyat, Mohammed Khair E A; Miekh, Yuliia V; Denisenko, Tatyana A; Vishnikin, Andriy B; Andruch, Vasil; Bazel, Yaroslav R

    2018-02-05

    A green, simple, accurate and highly sensitive sequential injection lab-at-valve procedure has been developed for the simultaneous determination of ascorbic acid (Asc) and rutin using 18-molybdo-2-phosphate Wells-Dawson heteropoly anion (18-MPA). The method is based on the dependence of the reaction rate between 18-MPA and reducing agents on the solution pH. Only Asc is capable of interacting with 18-MPA at pH 4.7, while at pH 7.4 the reaction with both Asc and rutin proceeds simultaneously. In order to improve the precision and sensitivity of the analysis, to minimize reagent consumption and to remove the Schlieren effect, the manifold for the sequential injection analysis was supplemented with external reaction chamber, and the reaction mixture was segmented. By the reduction of 18-MPA with reducing agents one- and two-electron heteropoly blues are formed. The fraction of one-electron heteropoly blue increases at low concentrations of the reducer. Measurement of the absorbance at a wavelength corresponding to the isobestic point allows strictly linear calibration graphs to be obtained. The calibration curves were linear in the concentration ranges of 0.3-24mgL -1 and 0.2-14mgL -1 with detection limits of 0.13mgL -1 and 0.09mgL -1 for rutin and Asc, respectively. The determination of rutin was possible in the presence of up to a 20-fold molar excess of Asc. The method was applied to the determination of Asc and rutin in ascorutin tablets with acceptable accuracy and precision (1-2%). Copyright © 2017 Elsevier B.V. All rights reserved.

  14. Simultaneous determination of inorganic anions and cations in explosive residues by ion chromatography.

    Science.gov (United States)

    Meng, Hong-Bo; Wang, Tian-Ran; Guo, Bao-Yuan; Hashi, Yuki; Guo, Can-Xiong; Lin, Jin-Ming

    2008-07-15

    A non-suppressed ion chromatographic method by connecting anion-exchange and cation-exchange columns directly was developed for the separation and determination of five inorganic anions (sulfate, nitrate, chloride, nitrite, and chlorate) and three cations (sodium, ammonium, and potassium) simultaneously in explosive residues. The mobile phase was composed of 3.5mM phthalic acid with 2% acetonitrile and water at flow rate of 0.2 mL/min. Under the optimal conditions, the eight inorganic ions were completely separated and detected simultaneously within 16 min. The limits of detection (S/N=3) of the anions and cations were in the range of 50-100 microg/L and 150-320 microg/L, respectively, the linear correlation coefficients were 0.9941-0.9996, and the R.S.D. of retention time and peak area were 0.10-0.29% and 5.65-8.12%, respectively. The method was applied successfully to the analysis of the explosive samples with satisfactory results.

  15. Simultaneous determination of inorganic mercury and methylmercury compounds in natural waters

    Energy Technology Data Exchange (ETDEWEB)

    Logar, Martina; Horvat, Milena [Jozef Stefan Institute, Jamova 39, 1000 Ljubljana (Slovenia); Akagi, Hirokatsu [National Institute for Minamata Disease, 4058-18 Hama, Minamata, Kumamoto 867-0008 (Japan); Pihlar, Boris [Faculty of Chemistry and Chemical Technology, University of Ljubljana, Askerceva 5, 1000 Ljubljana (Slovenia)

    2002-11-01

    The purpose of the present work was to develop a simple, rapid, sensitive and accurate method for the simultaneous determination of inorganic mercury (Hg{sup 2+}) and monomethylmercury compounds (MeHg) in natural water samples at the pg L{sup -1} level. The method is based on the simultaneous extraction of MeHg and Hg{sup 2+}dithizonates into an organic solvent (toluene) after acidification of about 300 mL of a water sample, followed by back extraction into an aqueous solution of Na {sub 2}S, removal of H {sub 2}S by purging with N {sub 2}, subsequent ethylation with sodium tetraethylborate, room temperature precollection on Tenax, isothermal gas chromatographic separation (GC), pyrolysis and cold vapour atomic fluorescence spectrometric detection (CV AFS) of mercury. The limit of detection calculated on the basis of three times the standard deviation of the blank was about 0.006 ng L {sup -1} for MeHg and 0.06 ng L {sup -1} for Hg {sup 2+}when 300 mL of water was analysed. The repeatability of the results was about 5% for MeHg and 10% for Hg {sup 2+}. Recoveries were 90-110% for both species. (orig.)

  16. Simultaneous spectrophotometric determination of trimethoprim and sulphamethoxazole following charge-transfer complexation with chloranilic acid

    Directory of Open Access Journals (Sweden)

    Olajire A. Adegoke

    2017-05-01

    Full Text Available A simple, accurate and precise simultaneous spectrophotometric method has been developed for the analysis of trimethoprim–sulphamethoxazole combination in pure and tablet dosage forms. The method involves direct charge transfer complexation of trimethoprim (TMP with chloranilic acid (CAA in acetonitrile–dioxane solvent mixture and complexation of sulphamethoxazole (SMZ after its hydrolysis in dilute H2SO4. Optimization of temperature and time revealed the superiority of room temperature and 20 and 30 min respectively for TMP and SMZ. Optimal detector responses were obtained at 520 and 440 nm and were therefore selected as working wavelength maxima for SMZ and TMP respectively. TMP and hydrolysed SMZ were combined with CAA at mole ratios of 1:1 and 1:3 respectively. Accuracies were generally less than 4% (estimated as degree of inaccuracy or error with a precision of the order of less than 2% on a three-day assessment. Physicochemical factors responsible for complex stability were estimated and related to the observed data. The method was successfully applied to the determination of TMP and SMZ in tablet dosage forms with accuracies comparable to the official BP method. There were no interferences from common tablet excipients and TMP complex did not interfere with the assay of SMZ. The developed method could find application in routine quality control of TMP–SMZ combination. It is the first reported full simultaneous colorimetric assay of TMP and SMZ using the same analytical reagent.

  17. Simultaneous Determination of Hydroquinone, Catechol and Resorcinol at Graphene Doped Carbon Ionic Liquid Electrode

    Directory of Open Access Journals (Sweden)

    Li Ma

    2012-01-01

    Full Text Available A new composite electrode has been prepared with doping graphene into the paste consisting graphite and ionic liquid, n-octyl-pyridinum hexafluorophosphate (OPFP. This electrode shows an excellent electrochemical activity for the redox of hydroquinone (HQ, catechol (CC, and resorcinol (RS. In comparison with bare paste electrode, the redox peaks of three isomers of dihydroxybenzene can be obviously, simultaneously observed at graphene doping paste electrode. Under the optimized condition, the simultaneous determination of HQ, CC, and RS in their ternary mixture can be carried out with a differential pulse voltammetric technique. The peak currents are linear to the concentration of HQ, CC, and RS in the range form 1×10−5 to 4×10−4, 1×10−5 to 3×10−4, and 1×10−6 to 1.7×10−4 mol L−1, respectively. The limits of detection are 1.8×10−6 mol L−1 for HQ, 7.4×10−7 mol L−1 for CC, and 3.6×10−7 M for RS, respectively.

  18. Simultaneous determination of boron, carbon and nitrogen in silicon by deuteron activation analysis

    International Nuclear Information System (INIS)

    He, Shiyu; Wang, Yinsong; Jin, Baikang; Hua, Zhifen; Zhao, Kaihua

    1984-01-01

    The paper describes simultaneous determination of trace quantities of B, C and N in semiconductor silicon by nuclear reaction of 10 B(d, n) 11 C(T 1/2 = 20.3 min), 11 B(d, 2n) 11 C, 12 C(d, n) 13 N(T 1/2 = 9.96 min) and 14 N(d, n) 15 O(T 1/2 = 2.03 min) with deuterons from a 1.2 m cyclotron in our institute. An inert-gas fusion technique is adopted for rapid radiochemical separation after irradiation of the samples. 11 C, 13 N and 15 O are absorbed in ascarite 5A molecular sieve cooled in liquid nitrogen and Hopcalite reagent at a temperature of 650 deg C respectively. Positron Annihilation events of each produced nucleus are counted by a γ - γ coincidence measuring system. B, C and N contents of about several ten parts per billion in silicon are then calculated simultaneously by a relatively quantitative method. Relative standard deviation for C, B and N are less than +-50% respectively. This method is simple, rapid and sensitive for estimating light element content in silicon material. (author)

  19. A rapid simultaneous determination of methylxanthines and proanthocyanidins in Brazilian guaraná (Paullinia cupana Kunth.).

    Science.gov (United States)

    Machado, Kamilla Nunes; Freitas, Aline Alves de; Cunha, Luzia Helena; Faraco, André Augusto Gomes; Pádua, Rodrigo Maia de; Braga, Fernão Castro; Vianna-Soares, Cristina Duarte; Castilho, Rachel Oliveira

    2018-01-15

    Paullinia cupana is a plant native to Brazil that is widely used in traditional medicine as a physical and mental stimulant. It is also used worldwide to produce soft drinks. A method for the simultaneous quantitation of seven markers in guaraná by HPLC-PDA was developed, and extraction methods for the determination of methylxanthines and tannins were investigated. Quantified substances were theobromine, theophylline, caffeine, catechin, epicatechin, procyanidins A2 and B2. Results confirmed the satisfactory selectivity and linearity (r 2 ≥0.99) within the mass ranges. Repeatability (RSD≤2.80%), intermediate precision (RSD≤4.47%), accuracy (recoveries from 90.59%-104.67%), and robustness were demonstrated. Extract 1 presented the contents: 0.0177% (±1.02%) for theobromine, 0.0131% (±1.14%) for theophylline, 2.9429% (±1.27%) for caffeine, 0.4563% (±1.02%) for catechin, 0.5515% (±1.05%) for epicatechin, 0.0607% (±2.80%) for A2 and 0.1035% (±1.39%) for B2. The method for simultaneous quantitation of seven chemical markers in guaraná proved to be reliable using a simple and convenient HPLC setup. Copyright © 2017 Elsevier Ltd. All rights reserved.

  20. Targeted and untargeted-metabolite profiling to track the compositional integrity of ginger during processing using digitally-enhanced HPTLC pattern recognition analysis.

    Science.gov (United States)

    Ibrahim, Reham S; Fathy, Hoda

    2018-03-30

    Tracking the impact of commonly applied post-harvesting and industrial processing practices on the compositional integrity of ginger rhizome was implemented in this work. Untargeted metabolite profiling was performed using digitally-enhanced HPTLC method where the chromatographic fingerprints were extracted using ImageJ software then analysed with multivariate Principal Component Analysis (PCA) for pattern recognition. A targeted approach was applied using a new, validated, simple and fast HPTLC image analysis method for simultaneous quantification of the officially recognized markers 6-, 8-, 10-gingerol and 6-shogaol in conjunction with chemometric Hierarchical Clustering Analysis (HCA). The results of both targeted and untargeted metabolite profiling revealed that peeling, drying in addition to storage employed during processing have a great influence on ginger chemo-profile, the different forms of processed ginger shouldn't be used interchangeably. Moreover, it deemed necessary to consider the holistic metabolic profile for comprehensive evaluation of ginger during processing. Copyright © 2018. Published by Elsevier B.V.

  1. Simultaneous Determination of Four Anthraquinones in Polygoni Multiflori Radix with Single Reference Standard by High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Hua Yang

    2015-07-01

    Full Text Available Objective: To establish a rapid, accurate and reliable analytical method for the simultaneous determination of four major anthraquinones in Polygoni Multiflori Radix (PMR using single reference standard.

  2. Simultaneous Determination of Four Preservatives in Foodstuffs by High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Mohammad Faraji

    2016-04-01

    Full Text Available Background and objectives:  High concentration of preservatives in food may result in gastrointestinal disturbances whereby some patients suffering from asthma, rhinitis, or urticaria. The aim of this study is the introduction and optimization a new method for simultaneous determination of four preservatives (SB, PS, MP, PP in foodstuff by high performance liquid chromatography. Materials and methods: Important factors in extraction, separation and determination process were optimized using the one variable at a time method.  Figures of merit of the proposed method were evaluated. The amount of SB, PS, MP, PP in some food samples were determined using the proposed method. Result: The results showed that the obtained chromatogram of extract was free of significant interferences. The preservatives recoveries ranged from 88% to 110 %. Concentration of SB, PS, MP and PP in the 20studied samples ranges between N.D-639.9, N.D -214.5, N.D -579.8 and N.D -30.5 mg kg-1, respectively  Conclusion: The performance and reliability of proposed method as a simple, efficient and fast method for determination of SB, PS, MP, PP in the food samples was demonstrated.

  3. The application of the inductively coupled plasma system to the simultaneous determination of precious metals

    International Nuclear Information System (INIS)

    Watson, A.E.; Russell, G.M.; Middleton, H.R.; Davenport, F.F.

    1983-01-01

    This report describes the development of a spectrochemical technique using excitation by an inducticely coupled plasma (ICP) source for the simultaneous determination of the precious metals (defined here as gold, silver, and all the platinum-group metals except osmium) in a wide variety of samples from a plant for the extraction and refining of platinum metal. The limits of detection for the analytes were determined in various acid and salt media and, under the conditions used, ranged from 20 to 100ng/l. The analytes were determined in the presence of a thousandfold excess of each of the other precious metals used as a matrix element. Some severe interferences were noted but were ascribed to spectral-line overlap or to contamination of the matrix material. Various dissolution techniques, based upon standard procedures applied in the precious-metals industry, were used, depending on the particular type of material treated. The spectrometer was calibrated by the use of solutions containing the analytes, sodium chloride, and acid, with scandium as the internal standard. The accuracy and precision of the technique, established by the analysis of many samples of each type, were found to be satisfactory when close attention was paid to detail in the preparation of the analytical solution. The relative standard deviation of the method ranges from 0,005 to 0,05, depending on the element being determined

  4. Sequential injection approach for simultaneous determination of ultratrace plutonium and neptunium in urine with accelerator mass spectrometry

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Roos, Per

    2013-01-01

    An analytical method was developed for simultaneous determination of ultratrace level plutonium (Pu) and neptunium (Np) using iron hydroxide coprecipitation in combination with automated sequential injection extraction chromatography separation and accelerator mass spectrometry (AMS) measurement...... show that preboiling and aging are important for obtaining high chemical yields for both Pu and Np, which is possibly related to the aggregation and adsorption behavior of organic substances contained in urine. Although the optimal condition for Np and Pu simultaneous determination requires 5-day aging...

  5. Spectrophotometric Methods for Simultaneous Determination of Oxytetracycline HCl and Flunixin Meglumine in Their Veterinary Pharmaceutical Formulation

    Directory of Open Access Journals (Sweden)

    Hanan A. Merey

    2017-01-01

    Full Text Available Four precise, accurate, selective, and sensitive UV-spectrophotometric methods were developed and validated for the simultaneous determination of a binary mixture of Oxytetracycline HCl (OXY and Flunixin Meglumine (FLU. The first method, dual wavelength (DW, depends on measuring the difference in absorbance (ΔA 273.4–327 nm for the determination of OXY where FLU is zero while FLU is determined at ΔA 251.7–275.7 nm. The second method, first-derivative spectrophotometric method (1D, depends on measuring the peak amplitude of the first derivative selectively at 377 and 266.7 nm for the determination of OXY and FLU, respectively. The third method, ratio difference method, depends on the difference in amplitudes of the ratio spectra at ΔP 286.5–324.8 nm and ΔP 249.6–286.3 nm for the determination of OXY and FLU, respectively. The fourth method, first derivative of ratio spectra method (1DD, depends on measuring the amplitude peak to peak of the first derivative of ratio spectra at 296.7 to 369 nm and 259.1 to 304.7 nm for the determination of OXY and FLU, respectively. Different factors affecting the applied spectrophotometric methods were studied. The proposed methods were validated according to ICH guidelines. Satisfactory results were obtained for determination of both drugs in laboratory prepared mixture and pharmaceutical dosage form. The developed methods are compared favourably with the official ones.

  6. Simultaneous determination of free amino acids in Pu-erh tea and their changes during fermentation.

    Science.gov (United States)

    Zhu, Yuchen; Luo, Yinghua; Wang, Pengpu; Zhao, Mengyao; Li, Lei; Hu, Xiaosong; Chen, Fang

    2016-03-01

    Pu-erh ripened tea is produced through a unique microbial fermentation process from the sun-dried leaves of large-leaf tea species (Camellia sinensis (Linn.) var. assamica (Masters) Kitamura) in Yunnan province of China. In this study, the changes of amino acid profiles during fermentation of Pu-erh tea were investigated, based on the improved HPLC-UV method with PITC pre-column derivatization for the simultaneous determination of twenty free amino acids. Results showed that aspartic acid, glutamic acid, arginine, alanine, theanine and tyrosine were the major amino acids in tea samples. Fermentation significantly influenced on the amino acid profiles. The total free amino acid contents significantly decreased during fermentation (pfermentation and then decreased gradually. The results provided the useful information for the manipulation of fermentation process according to the changes of amino acids and acrylamide contents in Pu-erh ripened tea. Copyright © 2015 Elsevier Ltd. All rights reserved.

  7. Dual-mode gradient HPLC procedure for the simultaneous determination of chloroquine and proguanil.

    Science.gov (United States)

    Paci, A; Caire-Maurisier, A-M; Rieutord, A; Brion, F; Clair, P

    2002-01-01

    In order to assay the antipaludic capsule of the Service de Santé des Armées (SSA), that contains two antimalarial drugs, i.e. chloroquine sulfate (CQS, cp1) and proguanil hydrochloride (PGH, cp5), a HPLC procedure was developed. A reversed-phase ion-pair high-performance liquid chromatography (HPLC) method with an ultraviolet detection at 254 nm was set up and validated. Elution system includes programming of both organic concentration and flow-rate known as 'dual-mode gradient'. This method allows the simultaneous determination of both active compounds and separation of four process related substances. The method is simple, rapid, selective and accurate, and the precision is good with an inter- and intra-assay of <2%. The sensitivity is particularly suitable for pharmaceutical quality control.

  8. Rapid HPLC-MS method for the simultaneous determination of tea catechins and folates.

    Science.gov (United States)

    Araya-Farias, Monica; Gaudreau, Alain; Rozoy, Elodie; Bazinet, Laurent

    2014-05-14

    An effective and rapid HPLC-MS method for the simultaneous separation of the eight most abundant tea catechins, gallic acid, and caffeine was developed. These compounds were rapidly separated within 9 min by a linear gradient elution using a Zorbax SB-C18 packed with sub 2 μm particles. This methodology did not require preparative and semipreparative HPLC steps. In fact, diluted tea samples can be easily analyzed using HPLC-MS as described in this study. The use of mass spectrometry detection for quantification of catechins ensured a higher specificity of the method. The percent relative standard deviation was generally lower than 4 and 7% for most of the compounds tested in tea drinks and tea extracts, respectively. Furthermore, the method provided excellent resolution for folate determination alone or in combination with catechins. To date, no HPLC method able to discriminate catechins and folates in a quick analysis has been reported in the literature.

  9. Simultaneous Determination of Alkoxyalcohols in Wet Wipes Using Static Headspace Gas Chromatography and Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Lee, So Jin; Pyo, Hee Soo; Chung, Bong Chul; Lee, Jeon Gae [KIST, Seoul (Korea, Republic of); Kim, Hai Dong [Kyung Hee University, Seoul (Korea, Republic of)

    2014-09-15

    Alkoxyalcohols are used as solvents or preservatives in various consumer products such as wet wipes. The metabolites of alkoxyalcohols are known to be chronically toxic and carcinogenic to animals. Thus, an analytical method is needed to monitor alkoxyalcohols in wet wipes. The aim of this study was to develop a simultaneous analytical method for 14 alkoxyalcohols using headspace gas chromatography coupled with mass spectrometry to analyze the wet wipes. This method was developed by comparing with various headspace extraction parameters. The linear calibration curves were obtained for the method (r2 > 0.995). The limit of detection of alkoxyalcohols ranged from 2 to 200 ng mL-1. The precision of the determinative method was less than 18.20% coefficient of variation both intra and inter days. The accuracy of the method ranged from 82.86% to 119.83%. (2-Methoxymethylethoxy)propanol, 2-phenoxyethanol, and 1-phenoxy-2-propanol were mainly detected in wet wipes.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1999-07-01

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

  11. Development of the kits for RIA simultaneous determination of polypeptide hormones

    International Nuclear Information System (INIS)

    Szybinski, Z.

    1982-12-01

    A simple and universal modification of chloramine T technique has been developed for the radioactive iodination of several polypeptide hormones such as insulin, human growth hormone (HGH), human TSH, synthetic human gastrin and beta-endorphine. The prepared products proved to have good immunoreactivity suitable for RIA purposes. The technique is inexpensive and quick. A new procedure has also been worked out utilizing horse myeloperoxidase in solid state as catalyser. The hormones iodinated with this technique show better parameters (e.g. longer stability, better binding to antibody, more favourable adsorption on dextran-coated charcoal); however the specific activities achieved were lower. The possibilities of simultaneous measurement of insulin and HGH have been studied. In this connection, a comparatively simple method for the determination of the endogenous anti-insulin antibodies was developed and used for the control of patients with diabetes and for the checking of new insulin preparations. However, the technique requires relatively sophisticated equipment and computerized calculations

  12. Simultaneous determination of a binary mixture of pantoprazole sodium and itopride hydrochloride by four spectrophotometric methods

    Science.gov (United States)

    Ramadan, Nesrin K.; El-Ragehy, Nariman A.; Ragab, Mona T.; El-Zeany, Badr A.

    2015-02-01

    Four simple, sensitive, accurate and precise spectrophotometric methods were developed for the simultaneous determination of a binary mixture containing Pantoprazole Sodium Sesquihydrate (PAN) and Itopride Hydrochloride (ITH). Method (A) is the derivative ratio method (1DD), method (B) is the mean centering of ratio spectra method (MCR), method (C) is the ratio difference method (RD) and method (D) is the isoabsorptive point coupled with third derivative method (3D). Linear correlation was obtained in range 8-44 μg/mL for PAN by the four proposed methods, 8-40 μg/mL for ITH by methods A, B and C and 10-40 μg/mL for ITH by method D. The suggested methods were validated according to ICH guidelines. The obtained results were statistically compared with those obtained by the official and a reported method for PAN and ITH, respectively, showing no significant difference with respect to accuracy and precision.

  13. Simultaneous bulk density and soil moisture determination by attenuation of 137 Cs and 241 Am

    International Nuclear Information System (INIS)

    Barros Ferraz, E.S. de.

    1974-01-01

    The method of simultaneous bulk density and soil moisture determination by attenuation of 241 Am and 137 Cs gamma-radiation is introduced and studied with detail. Theoretical considerations are made about the attenuation process in the absorbers, the form of solving the problem of two unknowns, the sensitivity of the method the influences of the resolution time of the electronic counting equipment, and of the Compton scattering in the sample. From the methodological point of view studies are made about the influence of the geometry, adjustment of counting system, choice of radiation sources, attenuation coefficient and the manner of obtaining reliable measurements. Data obtained are analysed, discussed and compared with those found in the literature. Finally the author presents some applications of the method, its use in soil-water movement studies, in soil profile compaction studies, and specially in swelling soils. (author)

  14. Simultaneous determination of devolatilization and char burnout times during fluidized bed combustion of coal

    International Nuclear Information System (INIS)

    Christofiedes, N.; Brown, R.C.

    1992-01-01

    In this paper, the authors investigate a method for simultaneous determination of devolatilization and char burnout times based on the analysis of CO 2 emissions from a fluidized bed combustor. The technique is non-intrusive and can be performed under realistic combustion conditions. The authors' method involves batching single-size coal samples in a fluidized bed combustor that is heated with propane gas or other fuel. Carbon dioxide profiles versus time for the batch tests are analyzed with a linear model to obtain characteristic time constants for coal devolatilization and char combustion which can be related to total devolatilization time and burnout time for a coal sample. The authors' approach does not require special sample preparation, can be performed in actual combustion equipment and employs standard boiler instrumentation

  15. Simultaneous determination of some common food dyes in commercial products by digital image analysis

    Directory of Open Access Journals (Sweden)

    Mohammad-Hossein Sorouraddin

    2015-09-01

    Full Text Available A simple and relatively fast image-analysis method using digital images, obtained with a flatbed scanner, has been described. The method was used for the simultaneous determination of four common food dyes, namely, carmoisine, brilliant blue, sunset yellow, and quinoline yellow, in binary mixtures in commercial products without a need for any prior separation steps. The results obtained were validated against a standard high-performance liquid chromatography method and a good agreement was obtained. The parameters affecting the experimental results were optimized. Under the optimal conditions, the method provided acceptable linear ranges (20–250 mg/L with correlation coefficients higher than 0.998, suitable precision (relative standard deviation ≤ 4.5%, and limits of detection between 4.82 and 8.05 mg/L.

  16. Simultaneous kinetic spectrometric determination of three flavonoid antioxidants in fruit with the aid of chemometrics

    Science.gov (United States)

    Sun, Ruiling; Wang, Yong; Ni, Yongnian; Kokot, Serge

    2014-03-01

    A simple, inexpensive and sensitive kinetic spectrophotometric method was developed for the simultaneous determination of three anti-carcinogenic flavonoids: catechin, quercetin and naringenin, in fruit samples. A yellow chelate product was produced in the presence neocuproine and Cu(I) - a reduction product of the reaction between the flavonoids with Cu(II), and this enabled the quantitative measurements with UV-vis spectrophotometry. The overlapping spectra obtained, were resolved with chemometrics calibration models, and the best performing method was the fast independent component analysis (fast-ICA/PCR (Principal component regression)); the limits of detection were 0.075, 0.057 and 0.063 mg L-1 for catechin, quercetin and naringenin, respectively. The novel method was found to outperform significantly the common HPLC procedure.

  17. [Simultaneous determination of eleven components in Ginkgo biloba leaves by high performance liquid chromatography method].

    Science.gov (United States)

    Lv, Jin-Li; Yang, Biao; Li, Meng-Xuan; Meng, Zhao-Qing; Ma, Shi-Ping; Wang, Zhen-Zhong; Ding, Gang; Huang, Wen-Zhe; Xiao, Wei

    2017-03-01

    To study Ginkgo biloba leaves in different producing area, we establish an HPLC method for the simultaneously determination of seven flavonoids glycosides and four biflavonoids in G. biloba leaves. The analysis was performed on an Agilent ZORBAX SB-C₁₈ column(4.6 mm×250 mm, 5 μm) wich acetonitrile, and 0.4% phosphoric acid as mobile phase at flow rate of 1 mL•min⁻¹ in a gradient edution, and the detection was carried out at 254 nm.The calibration curves of the seven flavonoids glycosides and four biflavonoids had a good linearitiy with good recoveries. The established HPLC method is simple, rapid, accurate, reliable, and sensitive, and can be applied to the identification and quality control of G. biloba leaves. Copyright© by the Chinese Pharmaceutical Association.

  18. Resonant tunneling: A method for simultaneous determination of resonance energy and energy eigenvalue

    Energy Technology Data Exchange (ETDEWEB)

    Maiz, F., E-mail: Fethi_maiz@yahoo.fr [King Khalid University, Faculty of Science, Physics Department, P.O. Box 9004, Abha (Saudi Arabia); University of Cartage, Nabeul Engineering Preparatory Institute, Merazka, 8000 Nabeul (Tunisia); Eissa, S.A. [King Khalid University, Faculty of Science, Physics Department, P.O. Box 9004, Abha (Saudi Arabia); AL-AZHAR University, Faculty of Science, Physics Department, Nasr City, Cairo (Egypt); AlFaify, S. [King Khalid University, Faculty of Science, Physics Department, P.O. Box 9004, Abha (Saudi Arabia)

    2013-09-15

    Assuming an effective mass approximation and using Bastard's boundary conditions, a simple method for simultaneous determination of the energy levels forming the sub-band structure and the transmissions coefficient of non-symmetrical, non-periodical potential semiconducting heterostructure is being proposed. The method can be applied on a multilayer system with varying thickness and effective mass of the layers, and with potential that is neither periodical nor symmetrical. To illustrate the feasibility of the proposed method, cases of symmetrical rectangular triple-barrier structure with constant effective mass, multi-barrier semiconductor heterostructure (nine barriers–eight-wells), and monomer height barrier superlattices (300 barriers) systems have been examined. Findings show very good agreements with previously published results obtained by different methods on similar systems. The proposed method was found to be useful for any number of semiconducting layers arranged in any random way making it more realistic, simple, and applicable to superlattice analysis and for devices design.

  19. [Simultaneous determination of eight kinds of conjunct bile acids in human bile by R-HPLC].

    Science.gov (United States)

    Dai, Z; Tan, G; Qian, K; Chen, X

    1997-01-01

    A method for the simultaneous determination of eight kinds of conjunct bile acids in human bile was developed by HPLC. They were separated on a YWG-C18 (3 microns) column at 30 degrees C, with methanol/water (65/35, V/V, pH3.0) as mobile phase, and detection wavelength at UV 210 nm. The linear ranges were 50-1,000 microns.ml-1, the recoveries were 91.2%-108.6%. The biles of 30 cases with cholelithiasis cholecystolithiasis and 20 cases without gallstone were detected by HPLC. The results showed that the constitution of bile acids was different between patients with cholelithiasis cholecystolithiasis and patients without gallstone.

  20. Two different spectrofluorimetric methods for simultaneous determination of gemfibrozil and rosiglitazone in human plasma.

    Science.gov (United States)

    El-Din, Mohie M K Sharaf; Attia, Khalid A M; Nassar, Mohamed W I; Kaddah, Mohamed M Y

    2010-10-15

    Two accurate, reliable, and highly sensitive spectrofluorimetric methods were developed for simultaneous determination of binary mixture gemfibrozil and rosiglitazone in human plasma without prior separation steps. The first method is based on synchronous fluorescence spectrometry using double scans. At Δλ=27nm, gemfibrozil yields detectable signal that is independent of the presence of rosiglitazone. Similarly, at Δλ=120nm the signal of rosiglitazone is not influenced by the presence of gemfibrozil. Signals at two wavelengths, 301 (Δλ=27nm) and 368nm (Δλ=120nm) vary linearly with gemfibrozil and rosiglitazone concentrations over the range 100-700ngmL(-1) (for gemfibrozil) and 20-140ngmL(-1) (for rosiglitazone), respectively. The limits of detection (LOD) were 2.3 and 2.72ngmL(-1) for gemfibrozil and rosiglitazone, respectively. The second method is based on the technique of simultaneous equations (Vierodt's method), in which 258nm was selected as the excitation wavelength. Two equations are constructed based on the fact that at ( λ(EM)₂=302 nm of gemfibrozil) and (λ(EM)₂=369 nm of rosiglitazone) the fluorescence of the mixture is the sum of the individual fluorescence of gemfibrozil and rosiglitazone. The limits of detection (LOD) were 28.1 and 23.63ngmL(-1) for gemfibrozil and rosiglitazone, respectively. The proposed methods were successfully applied for the determination of the two compounds in synthetic mixtures and in human plasma with a good recovery. Copyright © 2010 Elsevier B.V. All rights reserved.

  1. Simultaneous determination of caffeine, theobromine, and theophylline by high-performance liquid chromatography.

    Science.gov (United States)

    Bispo, Marcia S; Veloso, Márcia Cristina C; Pinheiro, Heloísa Lúcia C; De Oliveira, Rodolfo F S; Reis, José Oscar N; De Andrade, Jailson B

    2002-01-01

    This work relates the development of an analytical methodology to simultaneously determine three methylxanthines (caffeine, theobromine, and theophylline) in beverages and urine samples based on reversed-phase high-performance liquid chromatography. Separation is made with a Bondesil C18 column using methanol-water-acetic acid or ethanol-water-acetic acid (20:75:5, v/v/v) as the mobile phase at 0.7 mL/min. Identification is made by absorbance detection at 273 nm. Under optimized conditions, the detection limit of the HPLC method is 0.1 pg/mL for all three methylxanthines. This method is applied to urine and to 25 different beverage samples, which included coffee, tea, chocolate, and coconut water. The concentration ranges determined in the beverages and urine are: < 0.1 pg/mL to 350 microg/mL and 3.21 microg/mL to 71.2 microg/mL for caffeine; < 0.1 pg/mL to 32 microg mL and < 0.1 pg/mL to 13.2 microg/mL for theobromine; < 0.1 pg/mL to 47 microg/mL and < 0.1 pg/mL to 66.3 microg/mL for theophylline. The method proposed in this study is rapid and suitable for the simultaneous quantitation of methylxanthines in beverages and human urine samples and requires no extraction step or derivatization.

  2. [Simultaneous determination of seven alkaloids and three flavonoids in Sophorae Tonkinensis Radix et Rhizoma by HPLC].

    Science.gov (United States)

    Han, Fu-Man; Wang, Li-Xin; Chen, Ying; Chen, Liang-Mian; Feng, Wei-Hong; Wang, Jin-Yu; Liu, De-Wen; You, Yun; Tong, Yan

    2016-12-01

    In this study, an HPLC method was developed for simultaneous determination of seven alkaloids (cytosine, oxymatrine, N-oxysophocarpine, N-methylcytisine, sophoranol, matrine, and sophocarpine) and three flavonoids (trifolirhizin, fermononetin, and maackiain) from different samples of Sophorae Tonkinensis Radix et Rhizoma. Samples were analyzed on a Welch XtimateTM C₁₈ column (4. 6 mm× 250 mm, 5 μm) eluted with the mobile phase of acetonitrile (A) and 0.01 mol•L⁻¹ ammonium acetate solution (pH 8.0) (B) in a linear gradient mode as follows: 0-20 min,4%-14% A;20-30 min,14%-25% A;30-45 min,25%-40% A;45-65 min,40%-55% A;65-75 min,55% A. The flow rate of the mobile phase, the column temperature, and the PDA detector wavelength were set at 1.0 mL•min⁻¹, 30 ℃, and 225 nm, respectively. For the method validation, these ten compounds showed good separation and satisfactory linearity (r≥0.999 7) within the concentration ranges tested. The mean recoveries were in the range of 98.60% to 102.6% with the RSD (n=6) between 0.60% and 3.7%. This method was proved to be simple, accurate and repeatable. The quantitative results showed that there were significant differences in the contents of seven alkaloids and three flavonoids among the different samples. This result revealed that the quality of Sophorae Tonkinensis Radix et Rhizoma varied widely. This method could be used for the simultaneous determination of the multi-ingredients from Sophorae Tonkinensis Radix et Rhizoma, which might provide scientific evidences to evaluate/control the quality of Sophorae Tonkinensis Radix et Rhizoma, comprehensively. Copyright© by the Chinese Pharmaceutical Association.

  3. Simultaneous Determination of Florfenicol and Diclazuril in Compound Powder by RP-HPLC-UV Method

    Directory of Open Access Journals (Sweden)

    Leilei Guo

    2014-01-01

    Full Text Available A RP-HPLC-UV method was developed and validated for simultaneous determination of florfenicol and diclazuril in compound powder. The separation involved using a SinoChoom ODS-BP C18 (5 μm, 4.6 mm × 250 mm analytical column. The mobile phase was a mixture of acetonitrile-0.2% phosphoric acid (pH was adjusted to 3.0 with triethylamine. The ratio of acetonitrile and 0.2% phosphoric acid in the mobile phase was 60 : 40 (v/v from 0 minutes to 6 minutes and 70 : 30 (v/v from 6.1 minutes to 15 minutes. The flow rate was 1 mL/min. The temperature of the analytical column was maintained at 30°C. The detection was monitored at 225 nm and 277 nm for florfenicol and diclazuril, respectively. The excipients in the compound powder did not interfere with the drug peaks. The calibration curves of florfenicol and diclazuril were fairly linear over the concentration ranges between 50.0–500.0 μg/mL (r=0.9995 and 10.0–100.0 μg/mL (r=0.9992, respectively. The RSD of both the intraday and interday variations was below 2.1% for florfenicol and diclazuril. The method was successfully validated according to International Conference on Harmonisation and proved to be suitable for the simultaneous determination of florfenicol and diclazuril in compound powder.

  4. Differentiating Puerariae Lobatae Radix and Puerariae Thomsonii Radix using HPTLC coupled with multivariate classification analyses.

    Science.gov (United States)

    Wong, Ka H; Razmovski-Naumovski, Valentina; Li, Kong M; Li, George Q; Chan, Kelvin

    2014-07-01

    Puerariae Lobatae Radix (PLR), the root of Pueraria lobata, is a traditional Chinese medicine for treating diabetes and cardiovascular diseases. Puerariae Thomsonii Radix (PTR), the root of Pueraria thomsonii, is a closely related species to PLR and has been used as a PLR substitute in clinical practice. The aim of this study was to compare the classification accuracy of high performance thin-layer chromatography (HPTLC) with that of ultra-performance liquid chromatography (UPLC) in differentiating PLR from PTR. The Matlab functions were used to facilitate the digitalisation and pre-processing of the HPTLC plates. Seven multivariate classification methods were evaluated for the two chromatographic methods. The results demonstrated that the HPTLC classification models were comparable to the UPLC classification models. In particular, k-nearest neighbours, partial least square-discriminant analysis, principal component analysis-discriminant analysis and support vector machine-discriminant analysis showed the highest rate of correct species classification, whilst the lowest classification rate was obtained from soft independent modelling of class analogy. In conclusion, HPTLC combined with multivariate analysis is a promising technique for the quality control and differentiation of PLR and PTR. Copyright © 2014 Elsevier B.V. All rights reserved.

  5. Phytochemical studies on the terpenoids of medicinally important plant Aerva lanata L. using HPTLC

    Institute of Scientific and Technical Information of China (English)

    Yamunadevi M; Wesely EG; Johnson M

    2011-01-01

    Objective:To elucidate the terpenoids profile of Aerva lanata (A. lanata) using high performance thin layer chromatography (HPTLC). Methods: Preliminary phytochemical screening was done and HPTLC studies were carried out. The n-hexane:ethyl acetate (7.2: 2.8) was employed as mobile phase for terpenoids. Results: The desired aim was achieved using n-hexane-ethyl acetate (7.2: 2.8) as the mobile phase. The methanolic extract of stem, leaves, root, flower and seeds of A. lanata showed the presence of 27 different types of terpenoids with 27 different Rf values in the range of 0.06 to 0.97. The developed HPTLC method for terpenoid profile is simple, precise and accurate and can be used for the identification and commercial application. Conclusions:HPTLC profile of terpenoids has been chosen here to reveal the diversity existing at biochemical level in A. lanata. Such finger printing is useful in differentiating the species from the adulterant and act as a biochemical marker for this medicinally important plant in the pharmaceutical industry and plant systematic studies.

  6. Net Analyte Signal Standard Additions Method for Simultaneous Determination of Sulfamethoxazole and Trimethoprim in Pharmaceutical Formulations and Biological Fluids

    Directory of Open Access Journals (Sweden)

    M. H. Givianrad

    2012-01-01

    Full Text Available The applicability of a novel net analyte signal standard addition method (NASSAM to the resolving of overlapping spectra corresponding to the sulfamethoxazole and trimethoprim was verified by UV-visible spectrophotometry. The results confirmed that the net analyte signal standard additions method with simultaneous addition of both analytes is suitable for the simultaneous determination of sulfamethoxazole and trimethoprim in aqueous media. Moreover, applying the net analyte signal standard additions method revealed that the two drugs could be determined simultaneously with the concentration ratios of sulfamethoxazole to trimethoprim varying from 1:35 to 60:1 in the mixed samples. In addition, the limits of detections were 0.26 and 0.23 μmol L-1 for sulfamethoxazole and trimethoprim, respectively. The proposed method has been effectively applied to the simultaneous determination of sulfamethoxazole and trimethoprim in some synthetic, pharmaceutical formulation and biological fluid samples.

  7. Sequential Spectrophotometric Method for the Simultaneous Determination of Amlodipine, Valsartan, and Hydrochlorothiazide in Coformulated Tablets

    Directory of Open Access Journals (Sweden)

    Hany W. Darwish

    2013-01-01

    Full Text Available A new, simple and specific spectrophotometric method was developed and validated in accordance with ICH guidelines for the simultaneous estimation of Amlodipine (AML, Valsartan (VAL, and Hydrochlorothiazide (HCT in their ternary mixture. In this method three techniques were used, namely, direct spectrophotometry, ratio subtraction, and isoabsorptive point. Amlodipine (AML was first determined by direct spectrophotometry and then ratio subtraction was applied to remove the AML spectrum from the mixture spectrum. Hydrochlorothiazide (HCT could then be determined directly without interference from Valsartan (VAL which could be determined using the isoabsorptive point theory. The calibration curve is linear over the concentration ranges of 4–32, 4–44 and 6–20 μg/mL for AML, VAL, and HCT, respectively. This method was tested by analyzing synthetic mixtures of the above drugs and was successfully applied to commercial pharmaceutical preparation of the drugs, where the standard deviation is <2 in the assay of raw materials and tablets. The method was validated according to the ICH guidelines and accuracy, precision, repeatability, and robustness were found to be within the acceptable limits.

  8. Validated Spectrophotometric Methods for Simultaneous Determination of Food Colorants and Sweeteners

    Directory of Open Access Journals (Sweden)

    Fatma Turak

    2013-01-01

    Full Text Available Two simple spectrophotometric methods have been proposed for simultaneous determination of two colorants (Indigotin and Brilliant Blue and two sweeteners (Acesulfame-K and Aspartame in synthetic mixtures and chewing gums without any prior separation or purification. The first method, derivative spectrophotometry (ZCDS, is based on recording the first derivative curves (for Indigotin, Brillant Blue, and Acesulfame-K and third-derivative curve (for Aspartame and determining each component using the zero-crossing technique. The other method, ratio derivative spectrophotometry (RDS, depends on application ratio spectra of first- and third-derivative spectrophotometry to resolve the interference due to spectral overlapping. Both colorants and sweeteners showed good linearity, with regression coefficients of 0.9992–0.9999. The LOD and LOQ values ranged from 0.05 to 0.33 μgmL−1 and from 0.06 to 0.47 μgmL−1, respectively. The intraday and interday precision tests produced good RSD% values (<0.81%; recoveries ranged from 99.78% to 100.67% for all two methods. The accuracy and precision of the methods have been determined, and the methods have been validated by analyzing synthetic mixtures containing colorants and sweeteners. Two methods were applied for the above combination, and satisfactory results were obtained. The results obtained by applying the ZCDS method were statistically compared with those obtained by the RDS method.

  9. Improvement on simultaneous determination of chromium species in aqueous solution by ion chromatography and chemiluminescence detection

    DEFF Research Database (Denmark)

    Gammelgaard, Bente; Liao, Y.P.; Jons, O.

    1997-01-01

    A sensitive method for the simultaneous determination of chromium(III) and chromium(VI) was chromatography and chemiluminescence detection. Two Dionex ion-exchange guard columns in series, CG5 and AG7, were used to separate chromium(III) from chromium(VI). Chromium(VI) was reduced by potassium......, the stabilities of reductant and luminol solutions were studied. The linear range of the calibration curve for chromium(III) and chromium(VI) was 1-400 mu g l(-1). The detection limit was 0.12 mu g l(-1) for chromium(III) and 0.09 mu g l(-1) for chromium(VI), respectively. The precision at the 20 mu g l(-1) level...... was 1.4% for chromium(III) and 2.5% for chromium(VI), respectively. The accuracy of the chromium(III) determination was determined by analysis of the NIST standard reference material 1643c, Trace elements in water with the result 19.1 +/- 1.0 mu g Cr(III) l(-1) (certified value 19.0 +/- 0.6 mu g Cr...

  10. Simultaneous quantitative determination of paracetamol and tramadol in tablet formulation using UV spectrophotometry and chemometric methods

    Science.gov (United States)

    Glavanović, Siniša; Glavanović, Marija; Tomišić, Vladislav

    2016-03-01

    The UV spectrophotometric methods for simultaneous quantitative determination of paracetamol and tramadol in paracetamol-tramadol tablets were developed. The spectrophotometric data obtained were processed by means of partial least squares (PLS) and genetic algorithm coupled with PLS (GA-PLS) methods in order to determine the content of active substances in the tablets. The results gained by chemometric processing of the spectroscopic data were statistically compared with those obtained by means of validated ultra-high performance liquid chromatographic (UHPLC) method. The accuracy and precision of data obtained by the developed chemometric models were verified by analysing the synthetic mixture of drugs, and by calculating recovery as well as relative standard error (RSE). A statistically good agreement was found between the amounts of paracetamol determined using PLS and GA-PLS algorithms, and that obtained by UHPLC analysis, whereas for tramadol GA-PLS results were proven to be more reliable compared to those of PLS. The simplest and the most accurate and precise models were constructed by using the PLS method for paracetamol (mean recovery 99.5%, RSE 0.89%) and the GA-PLS method for tramadol (mean recovery 99.4%, RSE 1.69%).

  11. Rapidly Simultaneous Determination of Six Effective Components in Cistanche tubulosa by Near Infrared Spectroscopy

    Directory of Open Access Journals (Sweden)

    Xinhong Wang

    2017-05-01

    Full Text Available Quantitative determination of multiple effective components in a given plant usually requires a very large amount of authentic natural products. In this study, we proposed a rapid and non-destructive method for the simultaneous determination of echinacoside, verbascoside, mannitol, sucrose, glucose and fructose in Cistanche tubulosa by near infrared spectroscopy (NIRS. Near infrared diffuse reflectance spectroscopy (DRS and high performance liquid chromatography (HPLC were conducted on 116 batches of C. tubulosa samples. The DRS data were processed using standard normal variety (SNV and multiplicative scatter correction (MSC methods. Partial least squares regression (PLSR was utilized to build calibration models for components-of-interest in C. tubulosa. All models were then assessed by calculating the root mean square error of calibration (RMSEC, correlation coefficient of calibration (r. The r values of all six calibration models were determined to be greater than 0.94, suggesting each model is reliable. Therefore, the quantitative NIR models reported in this study can be qualified to accurately quantify the contents of six medicinal components in C. tubulosa.

  12. Simultaneous determination of eight water-soluble vitamins in supplemented foods by liquid chromatography.

    Science.gov (United States)

    Zafra-Gómez, Alberto; Garballo, Antonio; Morales, Juan C; García-Ayuso, Luis E

    2006-06-28

    A fast, simple, and reliable method for the isolation and determination of the vitamins thiamin, riboflavin, niacin, pantothenic acid, pyridoxine, folic acid, cyanocobalamin, and ascorbic acid in food samples is proposed. The most relevant advantages of the proposed method are the simultaneous determination of the eight more common vitamins in enriched food products and a reduction of the time required for quantitative extraction, because the method consists merely of the addition of a precipitation solution and centrifugation of the sample. Furthermore, this method saves a substantial amount of reagents as compared with official methods, and minimal sample manipulation is achieved due to the few steps required. The chromatographic separation is carried out on a reverse phase C18 column, and the vitamins are detected at different wavelengths by either fluorescence or UV-visible detection. The proposed method was applied to the determination of water-soluble vitamins in supplemented milk, infant nutrition products, and milk powder certified reference material (CRM 421, BCR) with recoveries ranging from 90 to 100%.

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

    Science.gov (United States)

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

    2008-02-01

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

  14. Simultaneous determination of Sunset yellow and Tartrazine in soft drinks using gold nanoparticles carbon paste electrode.

    Science.gov (United States)

    Ghoreishi, Sayed Mehdi; Behpour, Mohsen; Golestaneh, Mahshid

    2012-05-01

    The monitoring of synthetic dyes in foods is very important due to their potential harmfulness to human beings. Herein, a carbon-paste electrode (CPE) that is chemically modified with gold nanoparticles (nAu) was fabricated and used for the determination of Sunset yellow (SY) and Tartrazine (Tz). Cyclic and differential pulse voltammetry (CV and DPV) results revealed two well-resolved anodic peaks for SY and Tz with remarkably increase in oxidation signals of these colourants. Based on this, a novel electrochemical method was developed for the simultaneous determination of SY and Tz. High sensitivity and selectivity, sub-micromolar detection limit, high reproducibility and regeneration of the electrode surface by simple polishing make the nAu-CPE electrode very suitable for the determination of SY and Tz in commercially available soft drinks. The detection limits was 3.0×10(-8) and 2.0×10(-9)moll(-1) for SY and Tz, respectively, which are remarkably lower than those reported previously for SY and Tz using other modified electrodes. Copyright © 2011 Elsevier Ltd. All rights reserved.

  15. Using nonequilibrium capillary electrophoresis of equilibrium mixtures (NECEEM) for simultaneous determination of concentration and equilibrium constant.

    Science.gov (United States)

    Kanoatov, Mirzo; Galievsky, Victor A; Krylova, Svetlana M; Cherney, Leonid T; Jankowski, Hanna K; Krylov, Sergey N

    2015-03-03

    Nonequilibrium capillary electrophoresis of equilibrium mixtures (NECEEM) is a versatile tool for studying affinity binding. Here we describe a NECEEM-based approach for simultaneous determination of both the equilibrium constant, K(d), and the unknown concentration of a binder that we call a target, T. In essence, NECEEM is used to measure the unbound equilibrium fraction, R, for the binder with a known concentration that we call a ligand, L. The first set of experiments is performed at varying concentrations of T, prepared by serial dilution of the stock solution, but at a constant concentration of L, which is as low as its reliable quantitation allows. The value of R is plotted as a function of the dilution coefficient, and dilution corresponding to R = 0.5 is determined. This dilution of T is used in the second set of experiments in which the concentration of T is fixed but the concentration of L is varied. The experimental dependence of R on the concentration of L is fitted with a function describing their theoretical dependence. Both K(d) and the concentration of T are used as fitting parameters, and their sought values are determined as the ones that generate the best fit. We have fully validated this approach in silico by using computer-simulated NECEEM electropherograms and then applied it to experimental determination of the unknown concentration of MutS protein and K(d) of its interactions with a DNA aptamer. The general approach described here is applicable not only to NECEEM but also to any other method that can determine a fraction of unbound molecules at equilibrium.

  16. Simultaneous voltammetric determination of tramadol and acetaminophen using carbon nanoparticles modified glassy carbon electrode

    International Nuclear Information System (INIS)

    Ghorbani-Bidkorbeh, Fatemeh; Shahrokhian, Saeed; Mohammadi, Ali; Dinarvand, Rassoul

    2010-01-01

    A sensitive and selective electrochemical sensor was fabricated via the drop-casting of carbon nanoparticles (CNPs) suspension onto a glassy carbon electrode (GCE). The application of this sensor was investigated in simultaneous determination of acetaminophen (ACE) and tramadol (TRA) drugs in pharmaceutical dosage form and ACE determination in human plasma. In order to study the electrochemical behaviors of the drugs, cyclic and differential pulse voltammetric studies of ACE and TRA were carried out at the surfaces of the modified GCE (MGCE) and the bare GCE. The dependence of peak currents and potentials on pH, concentration and the potential scan rate were investigated for these compounds at the surface of MGCE. Atomic force microscopy (AFM) was used for the characterization of the film modifier and its morphology on the surface of GCE. The results of the electrochemical investigations showed that CNPs, via a thin layer model based on the diffusion within a porous layer, enhanced the electroactive surface area and caused a remarkable increase in the peak currents. The thin layer of the modifier showed a catalytic effect and accelerated the rate of the electron transfer process. Application of the MGCE resulted in a sensitivity enhancement and a considerable decrease in the anodic overpotential, leading to negative shifts in peak potentials. An optimum electrochemical response was obtained for the sensor in the buffered solution of pH 7.0 and using 2 μL CNPs suspension cast on the surface of GCE. Using differential pulse voltammetry, the prepared sensor showed good sensitivity and selectivity for the determination of ACE and TRA in wide linear ranges of 0.1-100 and 10-1000 μM, respectively. The resulted detection limits for ACE and TRA was 0.05 and 1 μM, respectively. The CNPs modified GCE was successfully applied for ACE and TRA determinations in pharmaceutical dosage forms and also for the determination of ACE in human plasma.

  17. A new innovative spectrophotometric method for the simultaneous determination of sofosbuvir and ledipasvir

    Science.gov (United States)

    Mansour, Fotouh R.

    2018-01-01

    A new innovative spectrophotometric method is developed to determine the concentration ratios in binary mixtures by determining the zero crossing point in the first derivative of the gross curve. This relationship can be applied if the part of the UV spectrum of substance Y, that intersects with the overlaid spectra of substance X is straight. By plotting the intersection wavelength against the concentration ratio (Cx/Cy), a straight line was obtained with a co-efficient of determination equals 0.9999. As an application, simultaneous determination of sofosbuvir and ledipasvir in their binary mixtures was performed using two methods; a direct UV spectrophotometric method for determination of ledipasvir at 333 nm, and the new "wavelength-intersection ratio" method for determination of sofosbuvir. In the wavelength-intersection ratio method, different mixtures of sofosbuvir and ledipasvir containing different concentration ratios were prepared; the zero crossing point of the first derivative curve in the range 285 to 295 nm were determined for each mixture. An absorbance shift in the intersection was obtained with the change in the concentration ratio (sofosbuvir/ledipasvir). When the concentration ratio was plotted against the intersection wavelength, a straight line was obtained with a coefficient of determination of 0.9992. The direct method was linear in the range 3 to 18 μg/mL while the wavelength-intersection ratio method was linear in the range 11-110 μg/mL. The limits of detection were determined and found to be 0.5 and 3 μg/mL for ledipasvir and sofosbuvir, respectively. The accuracy and repeatability of the two methods were tested. The mean %recovery was found to be 100.19% and 100.75% for ledipasvir and sofosbuvir, respectively. The relative standard deviation was 0.57 for ledipasvir and 1.79 for sofosbuvir. The intermediate precision was also checked, the coefficients of variation for sofosbuvir and ledipasvir measurements between days did not exceed 1.88%.

  18. Simultaneous determination of dopamine, uric acid and nitrite using carboxylated graphene oxide/lanthanum modified electrode

    International Nuclear Information System (INIS)

    Ye, Fengying; Feng, Chenqi; Jiang, Jibo; Han, Sheng

    2015-01-01

    Highlights: • The carboxylated graphene oxide/lanthanum-modified glassy carbon electrode (GO-COOLa/GCE) was successfully utilized for the simultaneous detection and quantification of DA, UA and NO 2 − . • Combining the benefits of carboxylated graphene oxide and lanthanum, the modified sensor displayed large peak separations, long linear ranges and low detection limits for simultaneously detecting DA, UA and NO 2 − . • The GO-COOLa/GCE electrode showed well stability, good repeatability, rapid response, and high catalytic performance toward the oxidations of DA, UA and NO 2 − . - Abstract: A bare glassy carbon electrode (GCE) was reformed by carboxylated graphene oxide/lanthanum, and the modified electrode, called GO-COOLa/GCE, was fabricated for simultaneously detecting dopamine (DA), uric acid (UA) and nitrite (NO 2 − ) by cyclic voltammetry (CV), differential pulse voltammetry (DPV) and amperometry. Several factors which affected the electrocatalytic activity of the GO-COOLa/GCE electrode, such as the effect of pH, scan rate and concentration were studied. Due to the combination of carboxylated graphene oxide and lanthanum ions, the GO-COOLa/GCE sensor showed rapid response, excellent selectivity and high catalytic performance toward the electrooxidation of DA, UA and NO 2 − . In optimized conditions, two linear response ranges for determining DA were obtained over ranges of 0.01-1.96×10 2 μM and 1.96×10 2 -1.23×10 3 μM with detection limit of 0.018 μM (S/N = 3). And the responses of the GO-COOLa/GCE electrode for UA and NO 2 − were linear in the region of 1-1.53×10 3 μM and 1-2.75×10 3 μM with detection limits of 0.058 μM and 0.070 μM, respectively. Furthermore, this reformed electrode was successfully used to the detection of DA, UA and NO 2 − in real urine and serum samples, showing its promising application in the electroanalysis of real samples.

  19. Quantitative analysis of rutin, quercetin, naringenin, and gallic acid by validated RP- and NP-HPTLC methods for quality control of anti-HBV active extract of Guiera senegalensis.

    Science.gov (United States)

    Alam, Perwez; Parvez, Mohammad K; Arbab, Ahmed H; Al-Dosari, Mohammed S

    2017-12-01

    Guiera senegalensis J.F. Gmel (Combretaceae) is a folk medicinal plant used in various metabolic and infectious diseases. In addition to its antiviral activities against herpes and fowlpox, the anti-HBV efficacy is very recently reported. To develop and validate simple, sensitive RP-/NP-HPTLC methods for quantitative determination of biomarkers rutin, quercetin, naringenin, and gallic acid in the anti-HBV active G. senegalensis leaves ethanol-extract. RP-HPTLC (rutin & quercetin; phase- acetonitrile:water, 4:6) and NP-HPTLC (naringenin & gallic acid; phase- toluene:ethyl acetate:formic acid, 6:4:0.8) were performed on glass-backed silica gel plates 60F 254 -RP18 and 60F 254 , respectively. The methods were validated according to the ICH guidelines. Well-separated and compact spots (R f ) of rutin (0.52 ± 0.006), quercetin (0.23 ± 0.005), naringenin (0.56 ± 0.009) and gallic acid (0.28 ± 0.006) were detected. The regression equations (Y) were 12.434x + 443.49, 10.08x + 216.85, 11.253x + 973.52 and 11.082x + 446.41 whereas the coefficient correlations (r 2 ) were 0.997 ± 0.0004, 0.9982 ± 0.0001, 0.9974 ± 0.0004 and 0.9981 ± 0.0001, respectively. The linearity ranges (ng/spot) were 200-1400 (RP-HPTLC) and 100-1200 (NP-HPTLC). The LOD/LOQ (ng/band) were 33.03/100.1 (rutin), 9.67/29.31 (quercetin), 35.574/107.8 (naringenin), and 12.32/37.35 (gallic acid). Gallic acid (7.01 μg/mg) was the most abundant biomarker compared to rutin (2.42 μg/mg), quercetin (1.53 μg/mg) and naringenin (0.14 μg/mg) in the extract. The validated NP-/RP-HPTLC methods were simple, accurate, and sensitive for separating and quantifying antiviral biomarkers in G. senegalensis, and endorsed its anti-HBV activity. The developed methods could be further employed in the standardization and quality-control of herbal formulations.

  20. Norepinephrine-modified glassy carbon electrode for the simultaneous determination of ascorbic acid and uric acid

    International Nuclear Information System (INIS)

    Zare, H.R.; Memarzadeh, F.; Ardakani, M. Mazloum; Namazian, M.; Golabi, S.M.

    2005-01-01

    The oxidation of norepinephrine (NE) on a preactivated glassy carbon electrode leads to the formation of a deposited layer of about 4.2 x 10 -10 mol cm -2 at the surface of the electrode. The electron transfer rate constant, k s , and charge transfer coefficient, α, for electron transfer between the electrode and immobilized NE film were calculated as 44 s -1 and 0.46, respectively. The NE-modified glassy carbon electrode exhibited good electrocatalytic properties towards ascorbic acid (AA) oxidation in phosphate buffer (pH 7.0) with an overpotential of about 475 mV lower than that of the bare electrode. The electrocatalytic response was evaluated by cyclic voltammetry, chronoamperometry, amperometry and rotating disk voltammetry. The overall number of electrons involved in the catalytic oxidation of AA and the number of electrons involved in the rate-determining step are 2 and 1, respectively. The rate constant for the catalytic oxidation of AA was evaluated by RDE voltammetry and an average value of k h was found to be 8.42 x 10 3 M -1 s -1 . Amperometric determination of AA in stirred solution exhibits a linear range of 2.0-1300.0 μM (correlation coefficient 0.9999) and a detection limit of 0.076 μM. The precision of amperometry was found to be 1.9% for replicate determination of a 49.0 μM solution of AA (n = 6). In differential pulse voltammetric measurements, the NE-modified glassy carbon electrode can separate the AA and uric acid (UA) signals. Ascorbic acid oxidizes at more negative potential than UA. Also, the simultaneous determination of UA and AA is achieved at the NE-modified electrode

  1. Simultaneous determination of ascorbic acid, dopamine and uric acid based on tryptophan functionalized graphene

    International Nuclear Information System (INIS)

    Lian, Qianwen; He, Zhifang; He, Qian; Luo, Ai; Yan, Kaiwang; Zhang, Dongxia; Lu, Xiaoquan; Zhou, Xibin

    2014-01-01

    Highlights: • Trp-GR was synthesized by utilizing a facile ultrasonic method. • The material as prepared had well dispersivity in water and better conductivity than pure GR. • Trp-GR/GCE showed excellent potential for the determination of AA, DA and UA. • The proposed method was applied for the analysis of AA, DA and UA in real samples. - Abstract: A new type of tryptophan-functionalized graphene nanocomposite (Trp-GR) was synthesized by utilizing a facile ultrasonic method via π–π conjugate action between graphene (GR) and tryptophan (Trp) molecule. The material as prepared had well dispersivity in water and better conductivity than pure GR. The surface morphology of Trp-GR was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Raman spectroscopy. The electrochemical behaviors of ascorbic acid (AA), dopamine (DA), and uric acid (UA) were investigated by cyclic voltammetry (CV) on the surface of Trp-GR. The separation of the oxidation peak potentials for AA–DA, DA–UA and UA–AA was about 182 mV, 125 mV and 307 mV, which allowed simultaneously determining AA, DA, and UA. Differential pulse voltammetery (DPV) was used for the determination of AA, DA, and UA in their mixture. Under optimum conditions, the linear response ranges for the determination of AA, DA, and UA were 0.2–12.9 mM, 0.5–110 μM, and 10–1000 μM, with the detection limits (S/N = 3) of 10.09 μM, 0.29 μM and 1.24 μM, respectively. Furthermore, the modified electrode was investigated for real sample analysis

  2. Simultaneous determination of ascorbic acid, dopamine and uric acid based on tryptophan functionalized graphene

    Energy Technology Data Exchange (ETDEWEB)

    Lian, Qianwen; He, Zhifang; He, Qian; Luo, Ai; Yan, Kaiwang; Zhang, Dongxia [Key Laboratory of Bioelectrochemistry and Environmental Analysis of Gansu Province, College of Geography and Environment Science, Northwest Normal University, Lanzhou, 730070 (China); Lu, Xiaoquan, E-mail: Luxq@nwnu.edu.cn [Key Laboratory of Bioelectrochemistry and Environmental Analysis of Gansu Province, College of Chemistry and Chemical Engineering, Northwest Normal University, Lanzhou, 730070 (China); Zhou, Xibin, E-mail: zhouxb@nwnu.edu.cn [Key Laboratory of Bioelectrochemistry and Environmental Analysis of Gansu Province, College of Geography and Environment Science, Northwest Normal University, Lanzhou, 730070 (China)

    2014-05-01

    Highlights: • Trp-GR was synthesized by utilizing a facile ultrasonic method. • The material as prepared had well dispersivity in water and better conductivity than pure GR. • Trp-GR/GCE showed excellent potential for the determination of AA, DA and UA. • The proposed method was applied for the analysis of AA, DA and UA in real samples. - Abstract: A new type of tryptophan-functionalized graphene nanocomposite (Trp-GR) was synthesized by utilizing a facile ultrasonic method via π–π conjugate action between graphene (GR) and tryptophan (Trp) molecule. The material as prepared had well dispersivity in water and better conductivity than pure GR. The surface morphology of Trp-GR was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Raman spectroscopy. The electrochemical behaviors of ascorbic acid (AA), dopamine (DA), and uric acid (UA) were investigated by cyclic voltammetry (CV) on the surface of Trp-GR. The separation of the oxidation peak potentials for AA–DA, DA–UA and UA–AA was about 182 mV, 125 mV and 307 mV, which allowed simultaneously determining AA, DA, and UA. Differential pulse voltammetery (DPV) was used for the determination of AA, DA, and UA in their mixture. Under optimum conditions, the linear response ranges for the determination of AA, DA, and UA were 0.2–12.9 mM, 0.5–110 μM, and 10–1000 μM, with the detection limits (S/N = 3) of 10.09 μM, 0.29 μM and 1.24 μM, respectively. Furthermore, the modified electrode was investigated for real sample analysis.

  3. Simultaneous determination of radionuclides separable into natural decay series by use of time-interval analysis

    International Nuclear Information System (INIS)

    Hashimoto, Tetsuo; Sanada, Yukihisa; Uezu, Yasuhiro

    2004-01-01

    A delayed coincidence method, time-interval analysis (TIA), has been applied to successive α-α decay events on the millisecond time-scale. Such decay events are part of the 220 Rn→ 216 Po (T 1/2 145 ms) (Th-series) and 219 Rn→ 215 Po (T 1/2 1.78 ms) (Ac-series). By using TIA in addition to measurement of 226 Ra (U-series) from α-spectrometry by liquid scintillation counting (LSC), two natural decay series could be identified and separated. The TIA detection efficiency was improved by using the pulse-shape discrimination technique (PSD) to reject β-pulses, by solvent extraction of Ra combined with simple chemical separation, and by purging the scintillation solution with dry N 2 gas. The U- and Th-series together with the Ac-series were determined, respectively, from alpha spectra and TIA carried out immediately after Ra-extraction. Using the 221 Fr→ 217 At (T 1/2 32.3 ms) decay process as a tracer, overall yields were estimated from application of TIA to the 225 Ra (Np-decay series) at the time of maximum growth. The present method has proven useful for simultaneous determination of three radioactive decay series in environmental samples. (orig.)

  4. An automatic optosensing device for the simultaneous determination of resveratrol and piceid in wines

    Energy Technology Data Exchange (ETDEWEB)

    Molina-Garcia, Lucia; Ruiz-Medina, Antonio [Department of Physical and Analytical Chemistry, University of Jaen, Campus Las Lagunillas s/n, 23071 Jaen (Spain); Fernandez-de Cordova, Maria Luisa, E-mail: mferna@ujaen.es [Department of Physical and Analytical Chemistry, University of Jaen, Campus Las Lagunillas s/n, 23071 Jaen (Spain)

    2011-03-18

    For the first time, a spectrofluorimetric method is reported for the simultaneous determination of resveratrol (RVT) and piceid (PCD), two stilbenes showing diverse interesting physiological and biochemical attributes, as well as a wide range of health benefits ranging from cardioprotection to chemoprevention. The method makes use of a multicommutated flow-through optosensor in which the resolution of RVT and PCD is accomplished by means the sequential arrival of their photoproducts, on-line generated by UV-irradiation, to the detection area. This is possible due to the different kinetic behaviour of these latter on a solid support (C{sub 18} silica gel) filling a minicolumn placed before the detector. The measurement in solid-phase of the photochemically induced fluorescence of the photoproducts ({lambda}{sub ex}: 257 nm/{lambda}{sub em}: 382 nm) is used as analytical signal for monitoring both compounds. The method has been applied to the analysis of RVT and PCD in wines and requires a previous solid-phase extraction (SPE) using Bakerbond C{sub 18} cartridges. This pretreatment and the use of a solid-support in both the minicolumn and the flow-cell of the detector allow the determination of RVT and PCD by external calibration. Detection limits (DLs) are 9.3 and 12.6 ng mL{sup -1} for RVT and PCD, respectively. Commercial red and white wine samples have been analysed and the results obtained have been satisfactorily validated by high-performance liquid chromatography (HPLC).

  5. Simultaneous Determination of Caffeine and Chlorogenic Acids in Green Coffee by UV/Vis Spectroscopy

    Directory of Open Access Journals (Sweden)

    G. Navarra

    2017-01-01

    Full Text Available A simple method for the simultaneous determination of caffeine and chlorogenic acids content in green coffee was reported. The method was based on the use of UV/Vis absorption. It is relevant that the quantification of both caffeine and chlorogenic acids was performed without their preliminary chemical separation despite their spectral overlap in the range 250–350 nm. Green coffee was extracted with 70% ethanol aqueous solution; then the solution was analyzed by spectroscopy. Quantitative determination was obtained analytically through deconvolution of the absorption spectrum and by applying the Lambert-Beer law. The bands used for the deconvolution were the absorption bands of both caffeine and chlorogenic acids standards. The molar extinction coefficients for caffeine and chlorogenic acid in ethanol solution at 70% were calculated by using the chemical standards; the estimated values were ε(272 nm=12159±97 M−1 cm−1 for caffeine and ε(330 nm=27025±190 M−1 cm−1 for chlorogenic acids molecules, respectively. The estimate of concentration values was in agreement with the one obtained by High Performance Liquid Chromatography quantification. The method is fast and simple and allows us to realize routine controls during the coffee production. In addition, it could be applied on roasted coffee and espresso coffee.

  6. Simultaneous determination of arsenic, copper, manganese, selenium, and zinc in biological materials by neutron activation analysis

    International Nuclear Information System (INIS)

    Damsgaard, E.; Heydorn, K.

    1976-08-01

    A method for the simultaneous determination of arsenic, copper, manganese, selenium, and zinc in biological material was developed by the incorporation of separation procedures for copper and zinc into an existing procedure. Investigation of the performance characteristics of the method was carried out with reference to copper and zinc. For certain materials characterized by a high Cu/Zn ratio, or a high zinc content, or both, such as liver, copper ihterferes in the determination of zinc thus requiring a small correction by an iterative procedure. Blank values for copper depend on the rinsing of the irradiation container, and a single rinsing with redistilled water was found superior to other rinsing procedures. Nuclear interference was negligible. The accuracy of the method was checked by analysis of Standard Reference Materials and the precision verified by analysis of Intercomparison Samples. Results are presented for 5 male foetuses of 3-5 months' gestational age. The distribution of arsenic, manganese and selenium is similar to that previously reported for adults. With the exception of liver, concentrations of copper in foetal organs were lower than values in the literature indicate. (author)

  7. Simultaneous determination of isoniazid and p-aminosalicylic acid by capillary electrophoresis using chemiluminescence detection.

    Science.gov (United States)

    Zhang, Xinfeng; Xuan, Yuelan; Sun, Aimin; Lv, Yi; Hou, Xiandeng

    2009-01-01

    It was found that isoniazid (ISO) or p-aminosalicylic acid (PAS) could enhance the chemiluminescence (CL) emission from Cu (II)-luminol-hydrogen peroxide system, and the increased chemiluminescence signals were proportional to their concentrations, respectively. Based on this phenomenon, a chemiluminescence method coupled to capillary electrophoresis (CE) was established for simultaneous determination of ISO and PAS. The CE conditions including running buffer and running voltage were investigated in detail. The effects of the pH of H(2)O(2) solution and the concentrations of luminol, H(2)O(2) and Cu (II) on the CL signal were also investigated carefully. Under the optimized conditions, the analysis could be accomplished within 10 min, with the limits of detection of 0.3 microg mL(-1) for ISO and 1.1 microg mL(-1) for PAS, corresponding to 7.2 and 26.4 pg per injection (24 nL), respectively. Finally, the method was validated by determining the two analytes in pharmaceutical preparation and spiked human serum samples. The results of pharmaceutical tablet analysis were in good agreement with the labeled amounts. The recoveries for ISO and PAS in human serum were in the range of 92-104% and 90-113%, respectively. Copyright 2008 John Wiley & Sons, Ltd.

  8. [Simultaneous determination of ten organotin compounds in polyvinyl chloride plastics using gas chromatography-mass spectrometry].

    Science.gov (United States)

    Li, Ying; Li, Bin; Liu, Li; Zhang, Chen; Wu, Jingwu; Liu, Zhihong; Li, Xintian

    2009-01-01

    A rapid and effective gas chromatography coupled with mass spectrometry method has been developed systematically and studied for the simultaneous determination of 10 organotin compounds, dibutyltin-dichloride (DBT), n-butyltin-trichloride (MBT), triethyltinchloride (TET), fentin-chloride (TPhT), chlorotributylstannane (TBT), tri-n-propyltinchloride (TPrT), diphenyltin-dichloride (DPhT), tetrabutyltin (TeBT), di-n-octyltin-dichloride (DOT), phenyltin trichloride (MPhT)), in polyvinyl chloride (PVC) plastics. The PVC sample was dissolved with tetrahydrofuran and the polymer in the sample was precipitated with methanol, and then the target compounds were derivatized with sodium tetraethylborate and extracted with hexane under ultrasonication. The qualitative and quantitative analysis were carried out by GC-MS and the total ion chromatogram and selected ion chromatogram were obtained. The derivatization and extraction conditions, such as the derivatization time, derivatization pH value, dosages of derivatization reagent and precipitation reagent were optimized. The good linearities, recoveries and precisions were obtained. The linearity ranges were 0.5 - 50 mg/L. The linearity correlation coefficients of 10 organotin compounds were between 0.997 8 and 0.999 7. The average recoveries were 84.23% - 109.1% with relative standard deviations of 4.24% - 10.75%. The established method has been successfully applied to the determination of organotin compounds in PVC plastics.

  9. Simultaneous in vivo determination of calcium and phosphate effective intestinal absorption in the rat

    International Nuclear Information System (INIS)

    Ladizesky, M.; Mautalen, C.A.; Cabrejas, M.; Degrossi, O.J.

    1978-01-01

    A description is given of a technique which allows a more precise assessment of the interrelation between calcium and phosphate transport systems. Rats were given an i.p. or oral dose of 47 Ca with 40 Ca as carrier and/or 32 P with 31 P as carrier. The animals were sacrificed and activities in body and excised gastrointestinal tract determined. The 1.28 MeV photopeak activity was measured for calcium 47, and phosphorus 32 activity was determined by measuring the Bremsstrahlung produced by this isotope in the rat's body in the 80 to 200 keV range. The rates of intestinal absorption of calcium and phosphate differed; there seemed to be no urinary excretion of the radioisotopes within 3 hours. The reciprocal influence of calcium and phosphate on the intestinal absorption was also studied. The technique is simple and allows the simultaneous in vivo measurement of the effective intestinal absorption of calcium and phosphate. (U.K.)

  10. Simultaneous determination of rifabutin and human serum albumin in pharmaceutical formulations by capillary electrophoresis.

    Science.gov (United States)

    Ermolenko, Yu; Anshakova, A; Osipova, N; Kamentsev, M; Maksimenko, O; Balabanyan, V; Gelperina, S

    Capillary zone electrophoresis (CZE) was used for determination of rifabutin (RFB), an anti-tuberculosis antibiotic drug, in various pharmaceutical formulations. Apart from that, simultaneous determination of RFB and human serum albumin (HSA) was performed. Electrophoretic behaviour of RFB was examined at various pH levels. CE conditions: a quartz capillary tube (internal diameter 75mm, effective length 50cm, total length 60cm), the capillary temperature was 25°С, the voltage applied to the capillary tube was +20kV, the UV detection wavelength was 214nm, hydrodynamic injection of the sample was performed at 30mbar for 5s, tetraborate buffer solution (0.01М, рН9.2). The obtained results are characterized by high efficiency (number of theoretical plates up to 260,000) and sufficient sensitivity (LOQ starting from 0.02μg/ml for RFB). The obtained data are in good accord with both HPLC results (for RFB) and spectrophotometry (for HSA). Copyright © 2017 Elsevier Inc. All rights reserved.

  11. Simultaneous RP-HPLC determination of sparfloxacin and dexamethasone in pharmaceutical formulations

    Directory of Open Access Journals (Sweden)

    Syed Naeem Razzaq

    2013-06-01

    Full Text Available The present study describes the development and subsequent validation of simple and accurate stability indicating RP-HPLC method for the determination of sparfloxacin and dexamethasone in pharmaceutical formulations in the presence of their stress-induced degradation products. Both the drugs and their stress-induced degradation products were separated within 10 minutes using C8 column and mixture of methanol and 0.02 M phosphate buffer pH 3.0 (60:40 v/v, respectively as mobile phase at 270 nm using diode array detector. Regression analysis showed linearity in the range of 15-105 µg/mL for sparfloxacin and 5-35 µg/mL for dexamethasone. All the analytes were adequately resolved with acceptable tailing. Peak purity of the two drugs was also greater than 0.9999, showing no co-elution peaks. The developed method was applied for simultaneous determination of sparfloxacin and dexamethasone in pharmaceutical formulations for stability studies.

  12. Microwave assisted direct saponification for the simultaneous determination of cholesterol and cholesterol oxides in shrimp.

    Science.gov (United States)

    Souza, Hugo A L; Mariutti, Lilian R B; Bragagnolo, Neura

    2017-05-01

    A novel microwave-assisted direct saponification method for the simultaneous determination of cholesterol and cholesterol oxides in shrimp was developed and validated. Optimal saponification conditions, determined by means of an experimental design, were achieved using 500mg of sample and 20mL of 1mol/L KOH ethanol solution for 16min at 45°C at maximum power at 200W and magnetic stirring at 120rpm. Higher extraction of cholesterol oxides in a reduced saponification time (∼75 times) was achieved in comparison with the direct cold saponification method. The new method showed low detection (≤0.57μg/mL) and quantification (≤1.73μg/mL) limits, good repeatability (≤10.50% intraday and ≤8.56% interday) and low artifact formation (evaluated by using a deuterated cholesterol-D6 standard). Raw, salted and dried-salted shrimps were successfully analyzed by the validated method. The content of cholesterol oxides increased after salting and decreased after drying. Copyright © 2016 Elsevier Ltd. All rights reserved.

  13. Simultaneous determination of Ra-226, Ra-228 and Pb-210 using a successive coprecipitations techniques

    International Nuclear Information System (INIS)

    Vilhena Schayer Sabino, C. de; Kastner, S.M.S.; Amaral, A.M.

    1990-01-01

    Several techniques for determination of Ra-226, Ra228 and Pb-210. were developed and used in routine at CDTN in the laboratories of radiochemistry. The matrixes were: water and industrial wastes. Some problems of these techniques were the time spent for analyses and chemical separations, interferents, among others. Now-a-days the method in routine developed here is the one of successive coprecipitations, followed α and β countings of the Ra-226 and Ra-228 daughters. This method is based on coprecipitation, purification of barium radium sulfate with EDTA in acetic solution. Lead is dissolved, radium remains precipitated and suffers a new purification and the time for growing of their daughters is waited to be performed the simultaneous α and β countings for Ra-226 and Ra-228 determination. Pb-210 is analyzed in the floating of the first purification with a carrier of bismuth, and the time for Bi-210 growing is waited. Then it is precipitated as hydroxid, purified as phosphate and the β counting of Bi-210 is done. (author) [pt

  14. Simultaneous determination of caffeine, theophylline and theobromine in food samples by a kinetic spectrophotometric method.

    Science.gov (United States)

    Xia, Zhenzhen; Ni, Yongnian; Kokot, Serge

    2013-12-15

    A novel kinetic spectrophotometric method was developed for the simultaneous determination of caffeine, theobromine and theophylline in food samples. This method was based on the different kinetic characteristics between the reactions of analytes with cerium sulphate in sulphuric acid and the associated change in absorbance at 320 nm. Experimental conditions, the effects of sulphuric acid, cerium sulphate and temperature, were optimised. Linear ranges (0.4-8.4 μg mL(-1)) for all three analytes were established, and the limits of detection were: 0.30 μg mL(-1) (caffeine), 0.33 μg mL(-1) (theobromine) and 0.16 μg mL(-1) (theophylline). The recorded data were processed by partial least squares and artificial neural network, and the developed mathematical models were then used for prediction. The proposed, novel method was applied to determine the analytes in commercial food samples, and there were no significant differences between the results from the proposed method and those obtained by high-performance liquid chromatography. Copyright © 2013 Elsevier Ltd. All rights reserved.

  15. Simultaneous determination of eight flavonoids in the flowers of Matricaria chamomilla by high performance liquid chromatography.

    Science.gov (United States)

    Xie, Xiao-Yu; Chen, Fang-Fang; Shi, Yan-Ping

    2014-01-01

    An HPLC method was developed for simultaneous determination of five flavones (apigenin, three apigenin 7-O-glucoside acylated derivatives, and luteolin) and three methoxylated flavonols in Matricaria chamomilla. Full validation of the assay was carried out including linearity, LODs, LOQs, precision, repeatability, stability, and accuracy. The results demonstrated that the method developed was simple, accurate, and reliable. Five batches of M. chamomilla samples were determined using the developed method, and total contents of the eight flavonoids ranged from 1.843 to 2.134 mg/g. Among them, the content of apigenin was the highest with values of 0.538 to 0.618 mg/g. In addition, the extract solution from M. chamomilla exhibited a significant dose-dependent inhibition of 2,2-diphenyl-1-picrylhydrazyl (DPPH) activity, with a 50% inhibition (SC50) at a concentration of 3.06 +/- 0.09 mg/mL, and the flavonoids apigenin-7-O-(6"-acetyl)-glucoside, luteolin, apigenin, eupatolitin, and chrysosplenol D played an important role in the antioxidant activities of the extract solution from M. chamomilla.

  16. An automatic optosensing device for the simultaneous determination of resveratrol and piceid in wines

    International Nuclear Information System (INIS)

    Molina-Garcia, Lucia; Ruiz-Medina, Antonio; Fernandez-de Cordova, Maria Luisa

    2011-01-01

    For the first time, a spectrofluorimetric method is reported for the simultaneous determination of resveratrol (RVT) and piceid (PCD), two stilbenes showing diverse interesting physiological and biochemical attributes, as well as a wide range of health benefits ranging from cardioprotection to chemoprevention. The method makes use of a multicommutated flow-through optosensor in which the resolution of RVT and PCD is accomplished by means the sequential arrival of their photoproducts, on-line generated by UV-irradiation, to the detection area. This is possible due to the different kinetic behaviour of these latter on a solid support (C 18 silica gel) filling a minicolumn placed before the detector. The measurement in solid-phase of the photochemically induced fluorescence of the photoproducts (λ ex : 257 nm/λ em : 382 nm) is used as analytical signal for monitoring both compounds. The method has been applied to the analysis of RVT and PCD in wines and requires a previous solid-phase extraction (SPE) using Bakerbond C 18 cartridges. This pretreatment and the use of a solid-support in both the minicolumn and the flow-cell of the detector allow the determination of RVT and PCD by external calibration. Detection limits (DLs) are 9.3 and 12.6 ng mL -1 for RVT and PCD, respectively. Commercial red and white wine samples have been analysed and the results obtained have been satisfactorily validated by high-performance liquid chromatography (HPLC).

  17. Net Analyte Signal Standard Additions Method for Simultaneous Determination of Sulfamethoxazole and Trimethoprim in Pharmaceutical Formulations and Biological Fluids

    OpenAIRE

    Givianrad, M. H.; Mohagheghian, M.

    2012-01-01

    The applicability of a novel net analyte signal standard addition method (NASSAM) to the resolving of overlapping spectra corresponding to the sulfamethoxazole and trimethoprim was verified by UV-visible spectrophotometry. The results confirmed that the net analyte signal standard additions method with simultaneous addition of both analytes is suitable for the simultaneous determination of sulfamethoxazole and trimethoprim in aqueous media. Moreover, applying the net analyte signal standard a...

  18. Determination of kinetic coefficients for the simultaneous reduction of sulfate and uranium by Desulfovibrio desulfuricans bacteria

    International Nuclear Information System (INIS)

    Tucker, M.D.

    1995-05-01

    Uranium contamination of groundwaters and surface waters near abandoned mill tailings piles is a serious concern in many areas of the western United States. Uranium usually exists in either the U(IV) or the U(VI) oxidation state. U(VI) is soluble in water and, as a result, is very mobile in the environment. U(IV), however, is generally insoluble in water and, therefore, is not subject to aqueous transport. In recent years, researchers have discovered that certain anaerobic microorganisms, such as the sulfate-reducing bacteria Desulfovibrio desulfuricans, can mediate the reduction of U(VI) to U(IV). Although the ability of this microorganism to reduce U(VI) has been studied in some detail by previous researchers, the kinetics of the reactions have not been characterized. The purpose of this research was to perform kinetic studies on Desulfovibrio desulficans bacteria during simultaneous reduction of sulfate and uranium and to determine the phase in which uranium exists after it has been reduced and precipitated from solution. The studies were conducted in a laboratory-scale chemostat under substrate-limited growth conditions with pyruvate as the substrate. Kinetic coefficients for substrate utilization and cell growth were calculated using the Monod equation. The maximum rate of substrate utilization (k) was determined to be 4.70 days -1 while the half-velocity constant (K s ) was 140 mg/l COD. The yield coefficient (Y) was determined to be 0.17 mg cells/mg COD while the endogenous decay coefficient (k d ) was calculated as 0.072 days -1 . After reduction, U(IV) Precipitated from solution in the uraninite (UO 2 ) phase. Uranium removal efficiency as high as 90% was achieved in the chemostat

  19. 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…

  20. Fractionation of human serum lipoproteins and simultaneous enzymatic determination of cholesterol and triglycerides

    International Nuclear Information System (INIS)

    Qureshi, Rashid Nazir; Kok, Wim Th.; Schoenmakers, Peter J.

    2009-01-01

    A method based on Asymmetric Flow Field-Flow Fractionation (AF4) was developed to separate different types of lipoproteins from human serum. The emphasis in the method optimization was on the possibilities to characterize the largest lipoprotein fractions (LDL and VLDL), which is usually not possible with the size-exclusion chromatography methods applied in routine analysis. Different channel geometries and flow programs were tested and compared. The use of a short fractionation channel was shown to give less sample dilution at the same fractionation power compared to a conventional, long channel. Different size selectivities were obtained with an exponential decay and a linear cross flow program. The ratio of the UV absorption signal to the light scattering signal was used to validate the relation between retention time and size of the fractionated particles. An experimental setup was developed for the simultaneous determination of the cholesterol and triglycerides distribution over the lipoprotein fractions, based on enzymatic reactions followed by UV detection at 500 nm. Coiled and knitted PTFE tubing reactors were compared. An improved peak sharpness and sensitivity were observed with the knitted tubing reactor. After optimization of the experimental conditions a satisfactory linearity and precision (2-3% rsd for cholesterol and 5-6% rsd for triglycerides) were obtained. Finally, serum samples, a pooled sample from healthy volunteers and samples of sepsis patients, were analyzed with the method developed. Lipoprotein fractionation and cholesterol and triglyceride distributions could be correlated with the clinical background of the samples.

  1. Simultaneous chemometric determination of pyridoxine hydrochloride and isoniazid in tablets by multivariate regression methods.

    Science.gov (United States)

    Dinç, Erdal; Ustündağ, Ozgür; Baleanu, Dumitru

    2010-08-01

    The sole use of pyridoxine hydrochloride during treatment of tuberculosis gives rise to pyridoxine deficiency. Therefore, a combination of pyridoxine hydrochloride and isoniazid is used in pharmaceutical dosage form in tuberculosis treatment to reduce this side effect. In this study, two chemometric methods, partial least squares (PLS) and principal component regression (PCR), were applied to the simultaneous determination of pyridoxine (PYR) and isoniazid (ISO) in their tablets. A concentration training set comprising binary mixtures of PYR and ISO consisting of 20 different combinations were randomly prepared in 0.1 M HCl. Both multivariate calibration models were constructed using the relationships between the concentration data set (concentration data matrix) and absorbance data matrix in the spectral region 200-330 nm. The accuracy and the precision of the proposed chemometric methods were validated by analyzing synthetic mixtures containing the investigated drugs. The recovery results obtained by applying PCR and PLS calibrations to the artificial mixtures were found between 100.0 and 100.7%. Satisfactory results obtained by applying the PLS and PCR methods to both artificial and commercial samples were obtained. The results obtained in this manuscript strongly encourage us to use them for the quality control and the routine analysis of the marketing tablets containing PYR and ISO drugs. Copyright © 2010 John Wiley & Sons, Ltd.

  2. Simultaneous determination of metformin and vildagliptin in human plasma by a HILIC-MS/MS method.

    Science.gov (United States)

    Pontarolo, Roberto; Gimenez, Ana Carolina; de Francisco, Thais Martins Guimarães; Ribeiro, Rômulo Pereira; Pontes, Flávia Lada Degaut; Gasparetto, João Cleverson

    2014-08-15

    The objective of this work was to develop and validate a HILIC-MS/MS method for the simultaneous determination of metformin and vildagliptin in human plasma. Chromatographic separation was achieved using an Atlantis HILIC Silica 150-mm × 2.1-mm, 3-μm particle size column maintained at 40°C. The isocratic mobile phase consisted of 20% water and 80% acetonitrile/water solution 95:5 (v/v), containing both 0.1% formic acid and 3mM ammonium formate. The flow rate was maintained at 400 μL min(-1). Data from validation studies demonstrated that the new method is highly selective, sensitive (limits of detection vildagliptin in plasma volunteers who orally received a single dose of metformin (850 mg), vildagliptin (50mg) or drug association (metformin 850 mg+vildagliptin 50mg). The new method can thus also be used as a tool for the clinical monitoring of metformin and vildagliptin. Copyright © 2014 Elsevier B.V. All rights reserved.

  3. Simultaneous determination of atorvastatin calcium, ezetimibe, and fenofibrate in a tablet formulation by HPLC.

    Science.gov (United States)

    Patel, Archita; Macwana, Chhaya; Parmar, Vishal; Patel, Samir

    2012-01-01

    An accurate, simple, reproducible, and sensitive HPLC method was developed and validated for the simultaneous determination of atorvastatin calcium, ezetimibe, and fenofibrate in a tablet formulation. The analyses were performed on an RP C18 column, 150 x 4.60 mm id, 5 pm particle size. The mobile phase methanol-acetonitrile-water (76 + 13 + 11, v/v/v), was pumped at a constant flow rate of 1 mL/min. UV detection was performed at 253 nm. Retention times of atorvastatin calcium, ezetimibe, and fenofibrate were found to be 2.25, 3.68, and 6.41 min, respectively. The method was validated in terms of linearity, precision, accuracy, LOD, LOQ, and robustness. The response was linear in the range 2-10 microg/mL (r2 = 0.998) for atorvastatin calcium, 2-10 microg/mL (r2 = 0.998) for ezetimibe, and 40-120 microg/mL (r2 = 0.998) for fenofibrate. The developed method can be used for routine quality analysis of the drugs in the tablet formulation.

  4. Simultaneous determination of ethinyl estradiol and drospirenone in oral contraceptive by high performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Viviane Benevenuti Silva

    2013-09-01

    Full Text Available A simple, rapid, economical and reliable high performance liquid chromatographic method has been developed and successfully applied in simultaneous determination of ethinyl estradiol and drospirenone in coated tablets. The HPLC method was performed on a LiChroCART® 100RP column (125x4 mm i.d., 5 µm with acetonitrile:water 50:50 (v/v as mobile phase, pumped at a flow rate of 1.0 mL.min-1. The fluorescence detection for ethinyl estradiol was made at λex= 280 nm and λem= 310 nm and a UV detection for drospirenone was made at 200 nm. The elution time for ethinyl estradiol and drospirenone were 4.0 and 5.7 min, respectively. The method was validated in accordance to USP 34 guidelines. The proposed HPLC method presented advantages over reported methods and is suitable for quality control assays of ethinyl estradiol and drospirenone in coated tablets.

  5. 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.

  6. Stability indicating RP-HPLC method for simultaneous determination of piroxicam and ofloxacin in binary combination.

    Science.gov (United States)

    John, Peter; Azeem, Waqar; Ashfaq, Muhammad; Khan, Islam Ullah; Razzaq, Syed Naeem

    2015-09-01

    A simple and precise RP-HPLC method was developed for simultaneous determination of piroxicam and ofloxacin in pharmaceutical formulations and human serum. Optimum separations of piroxicam, ofloxacin and stress-induced degradation products were achieved by use of Hypersil BDS C8 column (250 x 4.6mm, 5 μm). The mobile phase was a mixture of acetonitrile: 0.012M K2HPO4: 0.008M sodium citrate (both buffers mixed and pH adjusted to 2.8) (50:25:25 v/v/v) delivered at flow rate of 1.5 mL min⁻¹ using DAD at 254 nm. Response was linear function of concentration over the ranges of 70-130 mg mL⁻¹ for piroxicam and ofloxacin (r² ≥ 0.999). The method efficiently separated the analytical peaks from degradation products with acceptable tailing and resolution. The developed method was successfully used for concurrent analysis of piroxicam and ofloxacin in pharmaceutical formulations, human serum and in vitro drug interaction studies.

  7. Fractionation of human serum lipoproteins and simultaneous enzymatic determination of cholesterol and triglycerides

    Energy Technology Data Exchange (ETDEWEB)

    Qureshi, Rashid Nazir [Polymer-Analysis Group, van' t Hoff Institute for Molecular Sciences, University of Amsterdam, Nieuwe Achtergracht 166, 1018WV Amsterdam (Netherlands); Kok, Wim Th., E-mail: W.Th.Kok@uva.nl [Polymer-Analysis Group, van' t Hoff Institute for Molecular Sciences, University of Amsterdam, Nieuwe Achtergracht 166, 1018WV Amsterdam (Netherlands); Schoenmakers, Peter J. [Polymer-Analysis Group, van' t Hoff Institute for Molecular Sciences, University of Amsterdam, Nieuwe Achtergracht 166, 1018WV Amsterdam (Netherlands)

    2009-11-03

    A method based on Asymmetric Flow Field-Flow Fractionation (AF4) was developed to separate different types of lipoproteins from human serum. The emphasis in the method optimization was on the possibilities to characterize the largest lipoprotein fractions (LDL and VLDL), which is usually not possible with the size-exclusion chromatography methods applied in routine analysis. Different channel geometries and flow programs were tested and compared. The use of a short fractionation channel was shown to give less sample dilution at the same fractionation power compared to a conventional, long channel. Different size selectivities were obtained with an exponential decay and a linear cross flow program. The ratio of the UV absorption signal to the light scattering signal was used to validate the relation between retention time and size of the fractionated particles. An experimental setup was developed for the simultaneous determination of the cholesterol and triglycerides distribution over the lipoprotein fractions, based on enzymatic reactions followed by UV detection at 500 nm. Coiled and knitted PTFE tubing reactors were compared. An improved peak sharpness and sensitivity were observed with the knitted tubing reactor. After optimization of the experimental conditions a satisfactory linearity and precision (2-3% rsd for cholesterol and 5-6% rsd for triglycerides) were obtained. Finally, serum samples, a pooled sample from healthy volunteers and samples of sepsis patients, were analyzed with the method developed. Lipoprotein fractionation and cholesterol and triglyceride distributions could be correlated with the clinical background of the samples.

  8. Simultaneous Liquid Chromatographic Determination of 10 Ultra-Violet Filters in Sunscreens.

    Science.gov (United States)

    Wharton, Mary; Geary, Michael; O'Connor, Niamh; Curtin, Laura; Ketcher, Krystal

    2015-09-01

    A rapid HPLC method was developed for the simultaneous determination of 10 UV filters found in sunscreen. The following UV filters were analyzed in this method; 2-phenylbenzimidazole-5-sulfonic acid, benzophenone-3, isoamyl p-methoxycinnamate, 4-methylbenzylidene camphor, octocrylene, ethylhexyl dimethyl 4-aminobenzoic acid, ethylhexyl methoxycinnamate, butyl methoxydibenzoylmethane, ethylhexyl salicylate and homosalate. The method was developed on two columns; a Thermo Hypersil C18 BDS, 3 µm column (4.6 × 100 mm) and a Chromolith RP-18e Monolithic column (4.6 × 100 mm). The same mobile phase of ethanol and 1% acetic acid (70:30, v/v) was employed for both columns. The separation of the 10 UV filters was carried out successfully on both columns; the optimal resolution was obtained on the Thermo Scientific Hypersil column in a time frame of 7 min. An isocratic elution utilizing ethanol and acetic acid (70:30, v/v) at a temperature of 35°C was employed. The method was applied to a number of commercial samples of sunscreen and lotions and was validated according to International Conference on Harmonisation guidelines for selectivity, linearity, accuracy, precision and robustness. A comparison of the performances of both columns was also carried out. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  9. Simultaneous Determination of Different Anions in Milk Samples Using Ion Chromatography with Conductivity Detection

    Directory of Open Access Journals (Sweden)

    Gülçin Gümüş Yılmaz

    2016-12-01

    Full Text Available The description of a simple method for simultaneous determination of chloride, nitrate, sulfate, iodide, phosphate, thiocyanate, perchlorate, and orotic acid in milk samples was outlined. The method involves the use of dialysis cassettes for matrix elimination, followed by ion chromatography on a high capacity anion exchange column with suppressed conductivity detection. The novelty of dialysis process was that it did not need any chemical and organic solvent for elimination of macromolecules such as fat, carbohydrates and proteins from milk samples. External standard calibration curves for these analytes were linear with great correlation coefficients. The relative standard deviations of analyte concentrations were acceptable both inter-day and intra-day evaluations. Under optimized conditions, the limit of detection (Signal-to-Noise ratio = 3 for chloride, phosphate, thiocyanate, perchlorate, iodide, nitrate, sulfate, and orotate was found to be 0.012, 0.112, 0.140, 0.280, 0.312, 0.516, 0.520, and 0.840 mg L−1, respectively. Significant results were obtained for various spiked milk samples with % recovery in the range of 93.88 - 109.75 %. The proposed method was successfully applied to milk samples collected from Istanbul markets. The advantages of the method described herein are reagent-free, simple, and reliable.

  10. Simultaneous determination of quinolones for veterinary use by high-performance liquid chromatography with electrochemical detection.

    Science.gov (United States)

    Rodríguez Cáceres, M I; Guiberteau Cabanillas, A; Galeano Díaz, T; Martínez Cañas, M A

    2010-02-01

    A selective method based on high-performance liquid chromatography with electrochemical detection (HPLC-ECD) has been developed to enable simultaneous determination of three fluoroquinolones (FQs), namely danofloxacin (DANO), difloxacin (DIFLO) and sarafloxacin (SARA). The fluoroquinolones are separated on a Novapack C-18 column and detected in a high sensitivity amperometric cell at a potential of +0.8 V. Solid-phase extraction was used for the extraction of the analytes in real samples. The range of concentration examined varied from 10 to 150 ng g(-1) for danofloxacin, from 25 to 100 ng g(-1) for sarafloxacin and from 50 to 315 ng g(-1) for difloxacin, respectively. The method presents detection limits under 10 ng g(-1) and recoveries around 90% for the three analytes have been obtained in the experiments with fortified samples. This HPLC-ECD approach can be useful in the routine analysis of antibacterial residues being less expensive and less complicated than other more powerful tools as hyphenated techniques. 2009 Elsevier B.V. All rights reserved.

  11. Simultaneous determination of telmisartan and amlodipine in dog plasma by LC-MS-MS.

    Science.gov (United States)

    Wang, Baolian; Sheng, Li; Li, Yan

    2015-01-01

    A simple, rapid and sensitive method was established for the simultaneous determination of telmisartan and amlodipine in dog plasma by a HPLC-MS-MS analysis. The plasma sample preparation was a simple deproteinization by the addition of three volumes of methanol/acetonitrile mixture followed by centrifugation. The analytes and internal standard diphenhydramine were separated on a Zorbax SB-C18 column with a mobile phase of acetonitrile : water (45 : 55, v/v) at a flow rate of 0.2 mL/min with an operating temperature of 25°C. Detection was carried out by electrospray ionization in positive-ion multiple reaction monitoring mode. The calibration plots in dog plasma were linear over the ranges of 0.5-2,000 ng/mL for telmisartan and 0.5-500 ng/mL for amlodipine. The lower limit of quantification was 0.5 ng/mL for two analytes. The intra- and interday precisions (RSD%) were within 9.0%. The average recoveries of analytes were >85.0%. The method was successfully applied to the pharmacokinetic study of the two compounds after oral administration of telmisartan-amlodipine combination preparation to dogs. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  12. Chromatographic methods for the simultaneous determination of binary mixture of Saxagliptin HCl and Metformin HCl

    Directory of Open Access Journals (Sweden)

    Hanan A. Merey

    2017-12-01

    Full Text Available Two chromatographic methods were suggested for the simultaneous determination of a binary mixture containing Saxagliptin HCl (SAG and Metformin HCl (MET. First method was RP-HPLC method. Chromatographic separation was done on Kinetex™ column–C18 (4.6 × 150 mm, 2.6 µm using mobile phase consisted of acetonitrile:phosphate buffer pH = 4.5 ± 0.1 adjusted with orthophosphoric acid (13:87, v/v. Isocratic elution at a flow rate 1.5 mL/min and UV detection at 220.0 nm was performed. Second method was spectro-densitometric method. Chromatographic separation was done on precoated silica gel aluminium plates 60 F254 as a stationary phase and developing system consisting of chloroform:methanol:formic acid (80:20:0.3, by volume. The density of the separated bands was measured by UV detector at 210.0 nm. The proposed methods were validated as per the ICH guidelines parameters like Linearity, precision, accuracy, selectivity, limit of detection and limit of quantitation. Statistical comparison was done between the obtained results and those obtained by the reported methods, showing no significant difference with respect to accuracy and precision. Keywords: Saxagliptin HCl, Metformin HCl, RP-HPLC, TLC

  13. A Validated HPLC-DAD Method for Simultaneous Determination of Etodolac and Pantoprazole in Rat Plasma

    Directory of Open Access Journals (Sweden)

    Ali S. Abdelhameed

    2014-01-01

    Full Text Available A simple, sensitive, and accurate HPLC-DAD method has been developed and validated for the simultaneous determination of pantoprazole and etodolac in rat plasma as a tool for therapeutic drug monitoring. Optimal chromatographic separation of the analytes was achieved on a Waters Symmetry C18 column using a mobile phase that consisted of phosphate buffer pH~4.0 as eluent A and acetonitrile as eluent B in a ratio of A : B, 55 : 45 v/v for 6 min, pumped isocratically at a flow rate of 0.8 mL min−1. The eluted analytes were monitored using photodiode array detector set to quantify samples at 254 nm. The method was linear with r2=0.9999 for PTZ and r2=0.9995 for ETD at a concentration range of 0.1–15 and 5–50 μgmL−1 for PTZ and ETD, respectively. The limits of detection were found to be 0.033 and 0.918 μgmL−1 for PTZ and ETD, respectively. The method was statistically validated for linearity, accuracy, precision, and selectivity following the International Conference for Harmonization (ICH guidelines. The reproducibility of the method was reliable with the intra- and interday precision (% RSD <7.76% for PTZ and <7.58 % for ETD.

  14. [Simultaneous determination of four common nonprotein nitrogen substances in urine by high performance liquid chromatography].

    Science.gov (United States)

    Ma, Yuhua; Huang, Dongqun; Zhang, Rui; Xu, Shiru; Feng, Shun

    2013-11-01

    A high performance liquid chromatographic (HPLC) method was proposed to simultaneously determine four common nonprotein nitrogen substances, including creatine (Cr), creatinine (Cn), uric acid (Ua) and pseudouridine (Pu) in urine. After proteins being removed by acetone precipitation method, freeze drying and redissolving, the urine samples were analyzed by HPLC. Chromatographic separation was performed on a Waters RP18 Column (150 mm x 4.60 mm, 3.5 microm) in gradient elution mode using 10.0 mmol/L KH2PO4 solution (pH 4.78) and acetonitrile as mobile phases at a flow rate of 0.8 mL/min. The samples were detected at 220 nm. Rapid separation was achieved within 7 min. Under the optimized conditions, good linearities of four common nonprotein nitrogen substances were obtained in the range of 0.1-250 mg/L. The detection limits were 9.31 (Cr), 26.19 (Cn), 4.70 (Ua), an 6.30 (Pu) microg/L and the recoveries were in the range of 81%-111% with the relative standar deviations of 0.23%-2.78% (n = 3). The results demonstrate that this method is simple, rapid and accurate with good reproducibility, and can provide early diagnosis and preliminary judgment for type 2 diabetes mellitus (T2DM) patients with renal damage.

  15. [Simultaneous determination of five main index components and specific chromatograms analysis in Xiaochaihu granules].

    Science.gov (United States)

    Zhuang, Yan-Shuang; Cai, Hao; Liu, Xiao; Cai, Bao-Chang

    2012-01-01

    Reversed phase high performance liquid chromatography with diode array detector was employed for simultaneous determination of five main index components and specific chromatograms analysis in Xiaochaihu granules with a linear gradient elution of acetonitrile-water (containing 0.1% phosphoric acid) as mobile phase. The results showed that five main index components (baicalin, baicalein, wogonoside, wogonin, enoxolone) were separated well under the analytical condition. The linear ranges of five components were 0.518 - 16.576, 0.069 - 2.197, 0.167 - 5.333, 0.009 - 0.297 and 0.006 - 0.270 mg x g(-1), respectively. The correlation coefficients were 0.999 9, and the average recoveries ranged from 95% to 105%. Twelve common peaks were selected as the specific chromatograms of Xiaochaihu granules with baicalin as the reference peak. There were good similarities between the reference and the ten batches of samples. The similarity coefficients were no less than 0.9. The analytical method established is highly sensitive with strong specificity and it can be used efficiently in the quality control of Xiaochaihu granules.

  16. Simultaneous determination of flavonoids in chrysanthemum by capillary zone electrophoresis with running buffer modifiers.

    Science.gov (United States)

    Zhang, Shan; Dong, Shuqing; Chi, Langzhu; He, Pingang; Wang, Qingjiang; Fang, Yuzhi

    2008-08-15

    Despite the separation efficiency of capillary electrophoresis (CE) is much higher than other chromatographic methods, it is sometimes difficult to perfectly separate the complex ingredients in biological samples. One possible and simple way to develop the separation effect in CE is to add some modifiers in the running buffer. In this paper, the suitable running buffer modifiers were explored to simultaneously separate and detect six typical flavonoids (apigenin, luteolin, kaempferol, quercetin, (+)-catechin and (-)-epicatechin) which are the main active ingredients in chrysanthemum by capillary zone electrophoresis with amperometric detection (CZE-AD). It was found that when beta-cyclodextrin (beta-CD) and the mixture of methanol and ethanol were used as running buffer modifiers, a baseline separation of the six analytes could be accomplished in less than 20 min and the detection limits were as low as 10(-7) or 10(-8)gm l(-1). Other factors affecting the CZE separation, such as working potential, pH value and ionic strength of running buffer, separation voltage and sample injection time were extensively investigated. Under the optimum conditions, a successful practical application on the determination of chrysanthemum samples confirmed the validity and practicability of this method.

  17. [Simultaneous Determination of Three Kinds of Effective Constituents in Cannabis Plants by Reversed-phase HPLC].

    Science.gov (United States)

    Fu, Q; Shu, Z; Deng, K; Luo, X; Zeng, C G

    2016-08-01

    To establish a high performance liquid chromatographic (HPLC) method for simultaneous determination of three effective constituents, including tetrahydrocannabinol (THC), cannabidiol (CBD) and cannabinol (CBN) in Cannabis plants. A C₁₈ column was used in this study, and acetonitrile-phosphate buffer (0.015 mol/L KH₂PO₄) was used as mobile phase at a flow rate of 1.0 mL/min. At a detection wavelength of 220 mm, UV absorption spectra were collected at the wavelength range of 190-400 nm, and the spectra and retention time were counted as qualitative evidence. THC, CBD and CBN could be well separated by this method. Three components had good linear relationship in the range of 0.4-40 μg/mL ( R ²≥0.999 3). The recoveries were over 87%. The limits of detection were 1.8 ng, 2.0 ng and 1.3 ng, respectively. The relative standard deviation (RSD) were less than 5% for both inter-day and intra-day precisions. Reversed-phase HPLC method is simple, rapid and accurate, and it is suitable for the qualitative and quantitative detection of THC, CBD and CBN in Cannabis plants. Copyright© by the Editorial Department of Journal of Forensic Medicine

  18. Different Chromatographic Methods for Simultaneous Determination of Mefenamic Acid and Two of Its Toxic Impurities.

    Science.gov (United States)

    Morcoss, Martha M; Abdelwahab, Nada S; Ali, Nouruddin W; Elsaady, Mohammed T

    2017-08-01

    Two sensitive, accurate and precise chromatographic methods mentioned as TLC-densitometric method and RP-HPLC-DAD method, were developed and validated for the simultaneous determination of mefenamic acid (MEF) and its two toxic impurities, benzoic acid (BA) and 2,3-dimethylaniline (DMA). In the proposed TLC-densitometric method a developing system consisting of chloroform:acetone:acetic acid:ammonia solution(70:30:2:2, v/v/v/v) was used, TLC aluminum plates 60 F254 was used as a stationary phase and the separated bands were UV-scanned at 225 nm. While the proposed RP-HPLC-DAD method depended on chromatographic separation on C18 column using 0.05 M KH2PO4 buffer: acetonitrile (40:60, v/v) as a mobile phase at constant flow rate of 1 mL/min with UV detection at 225 nm. Linear relationships were obtained in the ranges of 0.3-2, 0.3-2 and 0.3-1.8 μg/band (for TLC-densitometric method) and in the ranges of 7-50, 10-50 and 7-50 μg/mL (for HPLC-DAD method) for MEF, BA and DMA, respectively. Factors affecting the developed methods have been studied and optimized. Moreover ,the proposed methods were successfully applied for determination of the studied drug in its pharmaceutical dosage form. The methods showed no significance difference when compared with the reported method using F-test and Student's-t test. The low of detection and quantization limits of the proposed methods get them suitable for quality control and stability studies of MEF in pharmaceutical formulation. The developed methods have advantages of being more selective and sensitive than the published methods. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  19. Simultaneous determination of the lipoxygenase and hydroperxide lyase specificity in olive fruit pulp

    Directory of Open Access Journals (Sweden)

    Salas, Joaquín J.

    2000-06-01

    Full Text Available Olive pulp lipoxygenase regiospecificity and hydroperoxide lyase substrate specificity are important parameters in order to justify the volatile composition of olive oil. A new radiolabelling method to determine simultaneously these properties using only thin layer chromatography steps is described in the present work. The method involves incubation of an enzyme preparation from olive pulp with radiolabelled linoleate, followed by the fractionation of the resulting lipid products, previously treated with 2,4-dinitrophenyl hydrazine, on thin layer chromatography plates coated with polyethylenglycol 400. The results obtained are in agreement with previous studies carried out by other methods.La regioespecificidad de la lipoxigenasa y la especificidad del sustrato hidroperóxido liasa de pulpa de aceituna son parámetros importantes en la justificación de la composición en volátiles del aceite de oliva. En este trabajo se describe un nuevo método de marcaje radioactivo para determinar simultáneamente estas propiedades, usando solo etapas de cromatografía en capa fina. El método implica la incubación de una preparación enzimática de pulpa de aceituna con linoleato marcado, seguido del fraccionamiento de los productos lipídicos resultantes, previamente tratados con 2,4-dinitrofenil hidrazina, sobre placas de cromatografía en capa fina soportadas con polietilenglicol 400. Los resultados obtenidos están de acuerdo con estudios previos llevados a cabo con otros métodos.

  20. Simultaneous determination of three surfactants and water in shampoo and liquid soap by ATR-FTIR.

    Science.gov (United States)

    Carolei, Luciano; Gutz, Ivano G R

    2005-03-31

    It is demonstrated for the first time that the principal constituents of a shampoo as well as of a liquid soap -three surfactants and water- can be determined directly, simultaneously and quickly in undiluted samples by attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy in the middle infrared region, despite the broad absorption bands of the solvent. Two of the surfactants, sodium lauryl ether sulfate (SLES) and cocoamidopropyl betaine (CAPB), are common to both formulations; alkylpolyglucoside (APG) is the third surfactant of the liquid soap and cocodiethanolamide (CDEA), the corresponding ingredient of the shampoo. Absorbance data of the undiluted samples and of the calibration standards was collected in the middle infrared region of the spectrum (800-1600 and 1900-3000cm(-1)). Two methods of multivariate quantification were compared: classical least squares (CLS), where absorbance data measured at 200 wavenumbers was processed, and inverse least squares (ILS), where data at 10 selected wavenumbers was analyzed. A spectra normalization procedure, based on a dominating water band, was examined. Twenty-seven standard mixtures were used for each application, consisting of all combinations at three concentration levels of each surfactant, respectively the lower limit, the expected value and the upper limit accepted in quality control. By favoring wavenumbers where absorption bands of the minor components (APG in the liquid soap and CDEA in the shampoo) are more intense, good results were obtained for 18 simulated samples of shampoo and 18 samples of liquid soap, no matter if calculations were made by CLS or ILS. The relative errors for water (major component, 84-88%) and SLES (7-10%) were always below 2%; for CAPB (2-4%), APG (<2%) and CDEA (<2%), they occasionally reached 5% of the component, an uncertainty of less than 0.07% in terms of the sample weight.

  1. Simultaneous Determination of Eight Bioactive Compounds in Dianthus superbus by High-performance Liquid Chromatography.

    Science.gov (United States)

    Yun, Bo-Ra; Yang, Hye Jin; Weon, Jin Bae; Lee, Jiwoo; Eom, Min Rye; Ma, Choong Je

    2016-05-01

    Dianthus superbus, one of traditional herbal medicine, is widely used to treat urethritis, carbuncles and carcinoma. A simultaneous determination method was established for controlling the quality of D. superbus using the eight compounds, (E)-methyl-4-hydroxy-4-(8a-methyl-3-oxodecahydronaphthalen-4a-yl) (1), diosmetin-7-O(2'',6''-di-O-α-L-rhamnopyranosyl)-β-D-glucopyranoside (2), vanillic acid (3), 4-hydroxyphenyl acetic acid (4), 4-methoxyphenyl acetic acid (5), (E)-4-methoxycinnamic acid (6), 3-methoxy-4-hydroxyphenylethanol (7), and methyl hydroferulate (8) isolated from D. superbus. This analysis method was developed using high performance liquid chromatography coupled with diode array detector with a Shishedo C18 column at a column temperature of 3°C. The mobile phase was composed of 0.1% trifluoroacetic acid in water and acetonitrile. The flow rate was 1 ml/min and detection wavelength was set at 205 nm and 280 nm. Validation was performed in order to demonstrate selectivity, accuracy and precision of the method. The calibration curves showed good linearity (R (2) > 0.99). The limits of detection and limits of quantification were within the ranges 0.0159-0.6205 μg/ml and 0.3210-1.8802 μg/ml, respectively. Moreover, the relative standard deviations of intra- and inter-day precision were both Dianthus superbus was established by high performance liquid chromatography-diode array detectorDeveloped analysis method is validated with linearity, precious and accuracyThe newly established method was successfully evaluated contents of eight compounds in 12 D. superbus samples (D.1.D.12) from various regions and compared. Abbreviations used: HPLC: High performance liquid chromatography, LOD: Limits of detection, LOQ: Limits of quantification, RSD: Relative standard deviation.

  2. Simultaneous determination of psychotropic drugs in human urine by capillary electrophoresis with electrochemiluminescence detection

    Energy Technology Data Exchange (ETDEWEB)

    Li Jianguo [Key Laboratory of Analytical Chemistry for Life Science (Education Ministry of China), School of Chemistry and Chemical Engineering, Nanjing University, Nanjing 210093 (China); School of Chemistry and Chemical Engineering, Suzhou University, Suzhou 215006 (China); Zhao Fengjuan [Key Laboratory of Analytical Chemistry for Life Science (Education Ministry of China), School of Chemistry and Chemical Engineering, Nanjing University, Nanjing 210093 (China); Ju Huangxian [Key Laboratory of Analytical Chemistry for Life Science (Education Ministry of China), School of Chemistry and Chemical Engineering, Nanjing University, Nanjing 210093 (China)]. E-mail: hxju@nju.edu.cn

    2006-08-04

    Amitriptyline, doxepin and chlorpromazine are often used as psychotropic drugs in treatment of the various mental diseases, and are also partly excreted by kidney. This work developed a simple, selective and sensitive method for their simultaneous monitoring in human urine using capillary electrophoresis coupled with electrochemiluminescence (ECL) detection based on end-column ECL reaction of tris-(2,2'-bipyridyl)ruthenium(II) with aliphatic tertiary amino moieties. Acetone was used as an additive to the running buffer to obtain their absolute separation. Under optimized conditions the proposed method displayed a linear range from 5.0 to 800 ng mL{sup -1} for the three drugs with the correlation coefficients more than 0.995 (n = 8). Their limits of detection were 0.8 ng mL{sup -1} (3.6 fg), 1.0 ng mL{sup -1} (4.5 fg) and 1.5 ng mL{sup -1} (6.8 fg) at a signal to noise ratio of 3, respectively. The relative standard deviations for five determinations of 20 ng mL{sup -1} amitriptyline, doxepin and chlorpromazine were 1.7%, 4.2% and 3.6%, respectively. For practical application an extract step with 90:10 heptane/ethyl acetate (v/v) was performed to eliminate the influence of ionic strength in sample. The recoveries of amitriptyline, doxepin and chlorpromazine at different levels in human urine were between 83% and 93%, which showed that the method was valuable in clinical and biochemical laboratories for monitoring amitriptyline, doxepin and chlorpromazine.

  3. Simultaneous separation and determination of fructose, sorbitol, glucose and sucrose in fruits by HPLC-ELSD.

    Science.gov (United States)

    Ma, Chunmei; Sun, Zhen; Chen, Changbao; Zhang, Lili; Zhu, Shuhua

    2014-02-15

    A high-performance liquid chromatography (HPLC) method with evaporative light scattering detection (ELSD) was optimised for simultaneous determination of fructose, sorbitol, glucose and sucrose in fruits. The analysis was carried out on a Phenomenex Luna 5u NH₂ 100A column (250 mm × 4.60mm, 5 micron) with isocratic elution of acetonitrile:water (82.5:17.5, v/v). Drift tube temperature of the ELSD system was set to 82 °C and nitrogen flow rate was 2.0 L min⁻¹. The regression equation revealed good linear relationship (R = 0.9967-0.9989) within test ranges. The limits of detection (LOD) and quantification (LOQ) for four analytes (peach, apple, watermelon, and cherry fruits) were in the range of 0.07-0.27 and 0.22-0.91 mg L⁻¹, respectively. The proposed HPLC-ELSD method was validated for quantification of sugars in peach, apple, watermelon, and cherry fruits, and the results were satisfactory. The results showed that the contents of the four sugars varied among fruits. While fructose (5.79-104.01 mg g⁻¹) and glucose (9.25-99.62 mg g⁻¹) emerged as common sugars in the four fruits, sorbitol (8.70-19.13 mg g⁻¹) were only found in peach, apple and cherry fruits, and sucrose (15.82-106.39 mg g⁻¹) were in peach, apple and watermelon. There was not detectable sorbitol in watermelon and sucrose in cherry fruits, respectively. Copyright © 2013 Elsevier Ltd. All rights reserved.

  4. Genetic and metabolic diversity in Stevia rebaudiana using RAPD and HPTLC analysis.

    Science.gov (United States)

    Chester, Karishma; Tamboli, Ennus Tajuddin; Parveen, Rabea; Ahmad, Sayeed

    2013-06-01

    Stevia rebaudiana Bertoni (Asteraceae) is an important medicinal plant and is much used due to its zero calories sweetening property. Stevia leaves as well as its extracts and pure compounds are currently used in the preparation of several medicines, food products and neutraceuticals. To study the genetic and metabolic variability in S. rebaudiana among accessions of different geographical regions of India using random amplified polymorphic DNA (RAPD) markers and high-performance thin layer chromatography (HPTLC) analysis. The RAPD analysis of Stevia rebaudiana (11 accessions) was carried out using 20 random operon primers. Dendrogram was constructed for cluster analysis based on the unweighted pair group method with arithmetic means (UPGMA) using Winboot. The HPTLC analysis of all samples was carried out on silica using acetone:ethyl acetate:water (5:4:1, v/v/v) for fingerprinting and quantification of stevioside and rebaudioside A at 360 nm after spraying with anisaldehyde sulphuric acid. Ten out of 20 primers screened were found most informative; amplification products of the genotypes yielded a total of 87 scorable bands (67 polymorphic), whereas genetic similarity (GS) coefficient (0.01-0.08) and polymorphism (67.24-92.40%) showed huge variability. Similarly, HPTLC analysis showed large variation among different samples with respect to their presence or absence of metabolite and their concentration. Out of the 11 Stevia accessions, Delhi and Mohali varieties showed much relatedness with each other and were concluded to be the superior genotype in context to RAPD and HPTLC analysis. The information obtained here could be valuable for devising strategies for cultivating this medicinal plant.

  5. Simultaneous determination of paracetamol and penicillin V by square-wave voltammetry at a bare boron-doped diamond electrode

    International Nuclear Information System (INIS)

    Švorc, Ľubomír; Sochr, Jozef; Tomčík, Peter; Rievaj, Miroslav; Bustin, Dušan

    2012-01-01

    Highlights: ► Unmodified BDD electrode = sensitive electrochemical sensor for drugs determination. ► No special pretreatment of samples except simple dilution. ► Selective method, common compounds present in urine do not interfere in high excess. ► Simultaneous determination of PAR and PEN has yet not been published in literature. - Abstract: A simple, sensitive and selective square-wave voltammetry method for simultaneous determination of paracetamol and penicillin V on a bare (unmodified) boron-doped diamond electrode has been developed. The good potential separation of about 0.35 V between the oxidation peak potentials of both drugs present in mixture was found. It was found by cyclic voltammetry that paracetamol gave quasireversible wave and penicillin V provided irreversible oxidation peak. The effect of supporting electrolyte, pH and scan rate on voltammetric response of both drugs was studied to select the optimum experimental conditions. The optimal conditions for quantitative simultaneous determination were obtained in acetate buffer solution at pH 5.0. The oxidation peak of paracetamol and penicillin V showed a systematic increase in peak currents with increase of their concentration. The calibration curves for the simultaneous determination of paracetamol and penicillin V exhibited the good linear responses within the concentration range from 0.4 to 100 μM for both drugs. The detection limit was established to 0.21 and 0.32 μM for paracetamol and penicillin V, respectively. The method proved the good sensitivity, repeatability (RSD of 1.5 and 2.1% for mixture solution of 10 μM PCM and PEN) and selectivity when influence of interferents commonly existing in human urine was negligible. The practical analytical utility of proposed method was demonstrated by simultaneous determination of paracetamol and penicillin V in human urine samples, with results similar to those obtained using a high-performance liquid chromatography method as an

  6. Simultaneous determination of chromium(III) and chromium(VI) in aqueous solutions by ion chromatography and chemiluminescence detection

    DEFF Research Database (Denmark)

    Gammelgaard, Bente; Jøns, O; Nielsen, B

    1992-01-01

    A method for the simultaneous determination of chromium(iii) and chromium(vi) in a flow system based on chemiluminescence was developed. A Dionex cation-exchange guard column was used to separate chromium(iii) from chromium(vi), and chromium(vi) was reduced by potassium sulfite, whereupon both...

  7. 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 ...

  8. A method to simultaneously determining the reduction in PAH dissolved concentrations and bioaccessibility in carbon amended soils

    DEFF Research Database (Denmark)

    Marchal, Geoffrey; Smith, Kilian E. C.; Rein, Arno

    In order to investigate the potential of different soil amendments (activated charcoal (AC), charcoal (biochar), compost) to sorb PAHs and their effect on bioaccessibility and biodegradation of PAHs in soil, a method was developed that can determine simultaneously the changes in PAH dissolved...

  9. Separation and Simultaneous Determination of 14 Fungicides with the Combination of Multi-Analyte Methods and HPLC Detection

    Energy Technology Data Exchange (ETDEWEB)

    Canping, Pan [Department of Applied Chemistry, China Agricultural University, Beijing (China)

    2009-07-15

    The separation and simultaneous HPLC-MS determination for a series of fungicide products is reported. Multi-analyte methods were applied on a Chromolith RP-18e monolithic column having low resistance and enabling high flow rates and short analysis time at very good separation power. Details and analytical conditions are described with chromatograms illustrating the results and work done. (author)

  10. Sequential Injection Method for Rapid and Simultaneous Determination of 236U, 237Np, and Pu Isotopes in Seawater

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Steier, Peter

    2013-01-01

    An automated analytical method implemented in a novel dual-column tandem sequential injection (SI) system was developed for simultaneous determination of 236U, 237Np, 239Pu, and 240Pu in seawater samples. A combination of TEVA and UTEVA extraction chromatography was exploited to separate and purify...... target analytes, whereupon plutonium and neptunium were simultaneously isolated and purified on TEVA, while uranium was collected on UTEVA. The separation behavior of U, Np, and Pu on TEVA–UTEVA columns was investigated in detail in order to achieve high chemical yields and complete purification...

  11. A method for simultaneous determination of wear-resistance of structurally identical machine parts with mutual friction

    International Nuclear Information System (INIS)

    Valigura, V.; Volyn'ski, A.

    1979-01-01

    There are mechanisms in the technique, boundary state of separate parts of which is determined by the process of wear of three elements of the mechanism, made of the same material (for example antifriction bearings). The main concept of wear determination in the case of such a mechanism is to conduct measurements by means of simultaneous application of three different methods, for example: the method of roentgen-fluorescence; the tracer technique with application of activation by means of irradiation by different elementary particles, practically by means of neutrons and protons; the method of artifical bases application. In the paper the method is presented having been developed in the Institute of Working Machines of the Poznan Polytechnic. This method of simultaneous investigation in the wear process of bearing rings, inner and outer, and rolling elements of roller bearings. All these elements of bearings are made of LX-15 steel. The method developed, permits to determine the wear sufficient for practical purposes sensitivity [ru

  12. Simultaneous determination of macronutrients, micronutrients and trace elements in mineral fertilizers by inductively coupled plasma optical emission spectrometry

    International Nuclear Information System (INIS)

    Oliveira Souza, Sidnei de; Silvério Lopes da Costa, Silvânio; Santos, Dayane Melo; Santos Pinto, Jéssica dos; Garcia, Carlos Alexandre Borges

    2014-01-01

    An analytical method for simultaneous determination of macronutrients (Ca, Mg, Na and P), micronutrients (Cu, Fe, Mn and Zn) and trace elements (Al, As, Cd, Pb and V) in mineral fertilizers was optimized. Two-level full factorial design was applied to evaluate the optimal proportions of reagents used in the sample digestion on hot plate. A Doehlert design for two variables was used to evaluate the operating conditions of the inductively coupled plasma optical emission spectrometer in order to accomplish the simultaneous determination of the analyte concentrations. The limits of quantification (LOQs) ranged from 2.0 mg kg −1 for Mn to 77.3 mg kg −1 for P. The accuracy and precision of the proposed method were evaluated by analysis of standard reference materials (SRMs) of Western phosphate rock (NIST 694), Florida phosphate rock (NIST 120C) and Trace elements in multi-nutrient fertilizer (NIST 695), considered to be adequate for simultaneous determination. Twenty-one samples of mineral fertilizers collected in Sergipe State, Brazil, were analyzed. For all samples, the As, Ca, Cd and Pb concentrations were below the LOQ values of the analytical method. For As, Cd and Pb the obtained LOQ values were below the maximum limit allowed by the Brazilian Ministry of Agriculture, Livestock and Food Supply (Ministério da Agricultura, Pecuária e Abastecimento — MAPA). The optimized method presented good accuracy and was effectively applied to quantitative simultaneous determination of the analytes in mineral fertilizers by inductively coupled plasma optical emission spectrometry (ICP OES). - Highlights: • Determination of inorganic constituents in mineral fertilizers was proposed. • Experimental design methodology was used to optimize analytical method. • The sample preparation procedure using diluted reagents (HNO 3 and H 2 O 2 ) was employed. • The analytical method was satisfactorily to the determination of thirteen elements. • The ICP OES technique can be

  13. Simultaneous UV Spectrophotometric Determination of Cetrizine and Dextromethorphan in Tablet Dosage Form

    Directory of Open Access Journals (Sweden)

    R. Vijayalakshmi

    2010-01-01

    Full Text Available Two accurate, precise, sensitve and economical procedures for simultaneous estimation of cetrizine and dextromethorphan in tablet dosage forms have been developed. First method employs formation and solving of simultaneous equations using 230 nm and 280 nm as two analytical wavelengths for both drugs in methanol. The second method is Q-analysis based on measurement of absorptivity at 224 nm (as isobestic point and 280 nm (λmax of CTZ. Cetrizine and dextromethorphan at their respective λmax 280 nm and 230 nm and at 224 nm (isobestic point shows linearity in a concentration range of 10-30 mcg/mL for both the drugs. The recovery studies confirmed accuracy of the proposed methods and low values of standard deviation confirmed precision of the methods. The methods were validated as per ICH guidelines.

  14. Atom localization and center-of-mass wave-function determination via multiple simultaneous quadrature measurements

    International Nuclear Information System (INIS)

    Evers, Joerg; Qamar, Shahid; Zubairy, M. Suhail

    2007-01-01

    We discuss localization and center-of-mass wave-function measurement of a quantum particle using multiple simultaneous dispersive interactions of the particle with different standing-wave fields. In particular, we consider objects with an internal structure consisting of a single ground state and several excited states. The transitions between ground and the corresponding excited states are coupled to the light fields in the dispersive limit, thus giving rise to a phase shift of the light field during the interaction. We show that multiple simultaneous measurements allow both an increase in the measurement or localization precision in a single direction and the performance of multidimensional measurements or localization. Further, we show that multiple measurements may relax the experimental requirements for each individual measurement

  15. Simultaneous determination of rabeprazole sodium and itopride hydrochloride in capsule dosage form by spectrophotometry.

    Science.gov (United States)

    Sabnis, Shweta S; Gandhi, Santosh V; Madgulkar, A R; Bothara, K G

    Three methods viz. Absorbance Ratio Method (I), Dual Wavelength Method (II) and First Order Derivative Spectroscopic Method (III) for simultaneous estimation of Rabeprazole sodium and Itopride hydrochloride have been developed. The drugs obey Beer's law in the concentration range 2-20 microg/ml for RAB and 5-75 microg/ml for ITO. The results of analysis of drugs have been validated statistically and by recovery studies.

  16. Simultaneous Voltammetric/Amperometric Determination of Sulfide and Nitrite in Water at BDD Electrode

    Directory of Open Access Journals (Sweden)

    Anamaria Baciu

    2015-06-01

    Full Text Available This work reported new voltammetric/amperometric-based protocols using a commercial boron-doped diamond (BDD electrode for simple and fast simultaneous detection of sulfide and nitrite from water. Square-wave voltammetry operated under the optimized working conditions of 0.01 V step potential, 0.5 V modulation amplitude and 10 Hz frequency allowed achieving the best electroanalytical parameters for the simultaneous detection of nitrite and sulfide. For practical in-field detection applications, the multiple-pulsed amperometry technique was operated under optimized conditions, i.e., −0.5 V/SCE for a duration of 0.3 s as conditioning step, +0.85 V/SCE for a duration of 3 s that assure the sulfide oxidation and +1.25 V/SCE for a duration of 0.3 s, where the nitrite oxidation occurred, which allowed the simultaneously detection of sulfide and nitrite without interference between them. Good accuracy was found for this protocol in comparison with standardized methods for each anion. Also, no interference effect was found for the cation and anion species, which are common in the water matrix.

  17. Simultaneous determination of ethamsylate, tramadol and lidocaine in human urine by capillary electrophoresis with electrochemiluminescence detection.

    Science.gov (United States)

    Li, Jianguo; Ju, Huangxian

    2006-09-01

    Ethamsylate, tramadol and lidocaine, partly excreted by the kidney, are generally used as hemostatic, analgesic and local anesthetic in surgery. We developed a simple and sensitive method for their simultaneous monitoring in human urine based on CE coupled with electrochemiluminescence detection by end-column mode. Under optimized conditions the proposed method yielded linear ranges from 5.0 x 10(-8) to 5.0 x 10(-5), 1.0 x 10(-7) to 1.0 x 10(-4) and 1.0 x 10(-7) to 1.0 x 10(-4) M with LODs of 8.0 x 10(-9) M (36 amol), 1.6 x 10(-8) M (72 amol) and 1.0 x 10(-8) M (45 amol) (S/N = 3) for ethamsylate, tramadol and lidocaine, respectively. The RSD for their simultaneous detection at 1.0 x 10(-6) M was 2.1, 2.8 and 3.2% (n = 7), respectively. For practical application an extraction step with ethyl acetate at pH 11 was performed to eliminate the influence of the sample ionic strength. The recoveries of ethamsylate, tramadol and lidocaine at different levels in human urine were between 87 and 95%. This method was used for simultaneous detection of ethamsylate, tramadol and lidocaine in clinic urine samples from two medicated patients. It was valuable in clinical and biochemical laboratories for monitoring these drugs for various purposes.

  18. Different Spectrophotometric Methods for Simultaneous Determination of Trelagliptin and Its Acid Degradation Product

    Science.gov (United States)

    Hassan, Mostafa A.; Zaghary, Wafaa A.

    2018-01-01

    New spectrophotometric and chemometric methods were carried out for the simultaneous assay of trelagliptin (TRG) and its acid degradation product (TAD) and applied successfully as a stability indicating assay to recently approved Zafatek® tablets. TAD was monitored using TLC to ensure complete degradation. Furthermore, HPLC was used to confirm dealing with one major acid degradation product. The proposed methods were developed by manipulating zero-order, first-derivative, and ratio spectra of TRG and TAD using simultaneous equation, first-derivative, and mean-centering methods, respectively. Using Spectra Manager II and Minitab v.14 software, the absorbance at 274 nm–260.4 nm, amplitudes at 260.4 nm–274.0 nm, and mean-centered values at 287.6 nm–257.2 nm were measured against methanol as a blank for TRG and TAD, respectively. Linearity and the other validation parameters were acceptable at concentration ranges of 5–50 μg/mL and 2.5–25 μg/mL for TRG and TAD, respectively. Using one-way analysis of variance (ANOVA), the optimized methods were compared and proved to be accurate for the simultaneous assay of TRG and TAD. PMID:29629213

  19. Simultaneous determination of arsenic and antimony by hydride generation atomic fluorescence spectrometry with dielectric barrier discharge atomizer

    Energy Technology Data Exchange (ETDEWEB)

    Xing Zhi [Department of Chemistry, Key Laboratory for Atomic and Molecular Nanosciences of the Education Ministry, Tsinghua University, Beijing 100084 (China); Kuermaiti, Biekesailike [Department of Chemistry, Key Laboratory for Atomic and Molecular Nanosciences of the Education Ministry, Tsinghua University, Beijing 100084 (China); Products Quality Inspection Institute, Yili, Xinjiang 835000 (China); Wang Juan; Han Guojun; Zhang Sichun [Department of Chemistry, Key Laboratory for Atomic and Molecular Nanosciences of the Education Ministry, Tsinghua University, Beijing 100084 (China); Zhang Xinrong, E-mail: xrzhang@mail.tsinghua.edu.cn [Department of Chemistry, Key Laboratory for Atomic and Molecular Nanosciences of the Education Ministry, Tsinghua University, Beijing 100084 (China)

    2010-12-15

    Simultaneous determination of As and Sb by hydride generation atomic fluorescence spectrometry was developed with the dielectric barrier discharge plasma as the hydride atomizer. The low-temperature and atmospheric-pressure micro-plasma was generated in a quartz cylindrical configuration device, which was constructed by an axial internal electrode and an outer electrode surrounding outside of the tube. The optimization of the atomizer construction and parameters for hydride generation and fluorescence detection systems were carried out. Under the optimized conditions, the detection limits for As and Sb were 0.04 and 0.05 {mu}g L{sup -1}, respectively. In addition, the applicability of the present method was confirmed by the detection of As and Sb in reference materials of quartz sandstone (GBW07106) and argillaceous limestone (GBW07108). The present work provided a new approach to exploit the miniaturized hydride generation dielectric barrier discharge atomic fluorescence spectrometry system for simultaneous multi-element determination.

  20. Simultaneous Determination of Eosin-Yellow and Ponceau-S Using H-Point Standard Addition Method in Micellar Media

    Directory of Open Access Journals (Sweden)

    Amandeep Kaur

    2012-01-01

    Full Text Available H-point standard addition method (HPSAM is developed for simultaneous determination of eosin-Y and ponceau-s in micellar media. Nickel chloride (NiCl2 is used as chromogenic reagent for complexes formation of eosin-Y and ponceau-S food colorants. The measurements were carried out using sodium lauryl sulphate as a surfactant, in buffered solution at pH 6.0. The concentration range of 0.115-2.53 μg/mL of eosin-Y and 0.159-3.80 μg/mL of ponceau-S. The proposed procedures have been applied successfully for the simultaneous determination of eosin-Y and ponceau-S in synthetic binary mixtures and real samples.

  1. Simultaneous determination of arsenic and antimony by hydride generation atomic fluorescence spectrometry with dielectric barrier discharge atomizer

    International Nuclear Information System (INIS)

    Xing Zhi; Kuermaiti, Biekesailike; Wang Juan; Han Guojun; Zhang Sichun; Zhang Xinrong

    2010-01-01

    Simultaneous determination of As and Sb by hydride generation atomic fluorescence spectrometry was developed with the dielectric barrier discharge plasma as the hydride atomizer. The low-temperature and atmospheric-pressure micro-plasma was generated in a quartz cylindrical configuration device, which was constructed by an axial internal electrode and an outer electrode surrounding outside of the tube. The optimization of the atomizer construction and parameters for hydride generation and fluorescence detection systems were carried out. Under the optimized conditions, the detection limits for As and Sb were 0.04 and 0.05 μg L -1 , respectively. In addition, the applicability of the present method was confirmed by the detection of As and Sb in reference materials of quartz sandstone (GBW07106) and argillaceous limestone (GBW07108). The present work provided a new approach to exploit the miniaturized hydride generation dielectric barrier discharge atomic fluorescence spectrometry system for simultaneous multi-element determination.

  2. Simultaneous determination of anthraquinones, their 8-beta-D-glucosides, and sennosides of Rhei Rhizoma by capillary electrophoresis.

    Science.gov (United States)

    Koyama, Junko; Morita, Izumi; Fujiyoshi, Hirotaka; Kobayashi, Norihiro

    2005-05-01

    The simultaneous separation and determination of major anthraquinones (emodin, chrysophanol, rhein and their glucosides, aloe-emodin, sennoside A, and sennoside B) of Rhei Rhizoma were achieved by cyclodextrin modified capillary zone electrophoresis. The running electrolyte used in this method was 0.005 M alpha-cyclodextrin in 0.03 M borate buffer (pH 10.0) containing 20% acetonitrile, with an applied voltage of 20 kV.

  3. Simultaneous determination of macronutrients, micronutrients and trace elements in mineral fertilizers by inductively coupled plasma optical emission spectrometry

    Science.gov (United States)

    de Oliveira Souza, Sidnei; da Costa, Silvânio Silvério Lopes; Santos, Dayane Melo; dos Santos Pinto, Jéssica; Garcia, Carlos Alexandre Borges; Alves, José do Patrocínio Hora; Araujo, Rennan Geovanny Oliveira

    2014-06-01

    An analytical method for simultaneous determination of macronutrients (Ca, Mg, Na and P), micronutrients (Cu, Fe, Mn and Zn) and trace elements (Al, As, Cd, Pb and V) in mineral fertilizers was optimized. Two-level full factorial design was applied to evaluate the optimal proportions of reagents used in the sample digestion on hot plate. A Doehlert design for two variables was used to evaluate the operating conditions of the inductively coupled plasma optical emission spectrometer in order to accomplish the simultaneous determination of the analyte concentrations. The limits of quantification (LOQs) ranged from 2.0 mg kg- 1 for Mn to 77.3 mg kg- 1 for P. The accuracy and precision of the proposed method were evaluated by analysis of standard reference materials (SRMs) of Western phosphate rock (NIST 694), Florida phosphate rock (NIST 120C) and Trace elements in multi-nutrient fertilizer (NIST 695), considered to be adequate for simultaneous determination. Twenty-one samples of mineral fertilizers collected in Sergipe State, Brazil, were analyzed. For all samples, the As, Ca, Cd and Pb concentrations were below the LOQ values of the analytical method. For As, Cd and Pb the obtained LOQ values were below the maximum limit allowed by the Brazilian Ministry of Agriculture, Livestock and Food Supply (Ministério da Agricultura, Pecuária e Abastecimento - MAPA). The optimized method presented good accuracy and was effectively applied to quantitative simultaneous determination of the analytes in mineral fertilizers by inductively coupled plasma optical emission spectrometry (ICP OES).

  4. A stochastic mathematical model for determination of transition time in the non-simultaneous case of surface and underground mining

    OpenAIRE

    Bakhtavar, E.; Abdollahisharif, J.; Aminzadeh, A.

    2017-01-01

    This research introduces a stochastic mathematical model that uses open pit long-term production planning on an integrated open pit and underground block model to determine the optimal time for transition from open pit to underground mining. In the model, ore grade is considered a random parameter in objective function and ore grade blending constraints. The objective function is modelled as the maximization of net present value in the mode of non-simultaneous combined open pit and undergroun...

  5. Simultaneous determination of cytosine arabinoside, daunorubicin and etoposide in human plasma

    DEFF Research Database (Denmark)

    Krogh-Madsen, Mikkel; Hansen, Steen Honoré; Honoré, Per Hartvig

    2010-01-01

    A method for simultaneous bioanalysis of the three cytotoxic drugs cytosine arabinoside, daunorubicin and etoposide in human plasma was developed and validated. A HPLC method with ultra-violet and fluorescence detection, preceded by mixed-mode cation-exchange solid phase extraction sample....... The overall precision (% relative standard deviation) was within 0.2-13.5% and the recovery ranged between 86.1% and 110.1% for the three drugs at all concentrations tested. Plasma samples were stable for at least two months when stored at -20 degrees C. The method was successfully applied to quantification...

  6. Simultaneous determination of reference free-stream temperature and convective heat transfer coefficients

    International Nuclear Information System (INIS)

    Jeong, Gi Ho; Song, Ki Bum; Kim, Kui Soon

    2001-01-01

    This paper deals with the development of a new method that can obtain heat transfer coefficient and reference free stream temperature simultaneously. The method is based on transient heat transfer experiments using two narrow-band TLCs. The method is validated through error analysis in terms of the random uncertainties in the measured temperatures. It is shown how the uncertainties in heat transfer coefficient and free stream temperature can be reduced. The general method described in this paper is applicable to many heat transfer models with unknown free stream temperature

  7. Determination of sulfonamides and trimethoprim using high temperature HPLC with simultaneous temperature and solvent gradient.

    Science.gov (United States)

    Giegold, Sascha; Teutenberg, Thorsten; Tuerk, Jochen; Kiffmeyer, Thekla; Wenclawiak, Bernd

    2008-10-01

    A fast HPLC method for the analysis of eight selected sulfonamides (SA) and trimethoprim has been developed with the use of high temperature HPLC. The separation could be achieved in less than 1.5 min on a 50 mm sub 2 microm column with simultaneous solvent and temperature gradient programming. Due to the lower viscosity of the mobile phase and the increased mass transfer at higher temperatures, the separation could be performed on a conventional HPLC system obtaining peak widths at half height between 0.6 and 1.3 s.

  8. HPLC DETERMINATION OF FENBENDAZOLE AND IVERMECTIN SIMULTANEOUSLY IN BULK AND PHARMACEUTICAL DOSAGE FORMS

    OpenAIRE

    Battula Sreenivasa Rao, Mandapati Varaprasad Reddy*, Bhatraju Sreenivasa Rao

    2017-01-01

    In the present study, a simple, precise and accurate high performance liquid chromatography with photodiode array detector was developed for the simultaneous estimation of ivermectin & fenbendazole in bulk and tablet dosage forms. A Zorbax C8 column (250 cm × 4.6 mm × 5 μm) with mobile phase consisting of 0.1 M potassium dihydrogen orthophosphate and methanol (60:40 v/v) having pH 4.5 (adjusted with orthophosphoric acid) was used. The flow rate was 1.2 ml/min and the effluents were detected a...

  9. A novel electro analytical nanosensor based on graphene oxide/silver nanoparticles for simultaneous determination of quercetin and morin

    International Nuclear Information System (INIS)

    Yola, Mehmet Lütfi; Gupta, Vinod Kumar; Eren, Tanju; Şen, Arif Emre; Atar, Necip

    2014-01-01

    Graphical abstract: - Abstract: In this report, silver nanoparticles (AgNPs) with the mean diameters of 10-30 nm were self-assembled onto the surfaces of 2-aminoethanethiol (2-AET) functionalized graphene oxide (AETGO) sheets. The graphene oxide (GO) and AgNPs-AETGO nanocomposites were characterized by a transmission electron microscope (TEM), x-ray photoelectron spectroscopy (XPS), reflection–absorption infrared spectroscopy (RAIRS) and the x-ray diffraction (XRD). The simultaneous determination of quercetin (QR) and morin (MR) has been performed on glassy carbon electrode (GCE) modified with AgNPs-AETGO (AgNPs-AETGO/GCE). QR presented an oxidation step at Ea of 200 mV and reduction step at Ec of 150 mV and RT presented an oxidation step at Ea of 600 mV at AgNPs-AETGO/GCE by cyclic voltammetry (CV). The linearity ranges and the detection limits of QR and MR were 1.0 × 10-8 - 5.0 × 10-6 M and 3.3 × 10-9 M, respectively. The AgNPs-AETGO/GCE was also applied to real samples for the simultaneous determination of QR and MR. Thus the developed method can be adopted as an alternative to the published chromatographic, spectrophotometric and electroanalytical methods for simultaneous determination of QR and MR

  10. Simultaneous determination of sulphoraphane and sulphoraphane nitrile in Brassica vegetables using ultra-performance liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Alvarez-Jubete, Laura; Smyth, Thomas J; Valverde, Juan; Rai, Dilip K; Barry-Ryan, Catherine

    2014-01-01

    Several analytical methods exist for the determination of sulphoraphane or sulphoraphane nitrile from biological matrices and plant extracts. However, no UPLC-MS/MS method exists for the simultaneous detection of both. To develop and validate an UPLC-MS/MS method for the simultaneous analysis of sulphoraphane and sulphoraphane nitrile from Brassica oleracea L. ssp. italica This method was developed utilising an Acquity BEH C8 column with gradient elution combined with tandem mass spectrometry, using positive electrospray ionisation in multiple reaction monitoring mode. The retention times for sulphoraphane and sulphoraphane nitrile were 0.4 and 0.6 min respectively, and total run time was 3 min. The method was validated for linearity, sensitivity, precision, accuracy, matrix effects and recovery. The method was employed to determine glucoraphanin hydrolysis products in broccoli and the predominant product was found to vary depending on the variety tested. It was also applied to the accurate determination of sulphoraphane and sulphoraphane nitrile in broccoli samples hydrolysed under different conditions. It was observed that the formation of sulphoraphane and sulphoraphane nitrile was influenced by the temperature of the reaction. The validated UPLC-MS/MS method for simultaneous detection of sulphoraphane and sulphoraphane nitrile was shown to be applicable to broccoli plants and is expected to be applicable to other cruciferous sources. Copyright © 2013 John Wiley & Sons, Ltd.

  11. Simultaneous electrochemical determination of L-cysteine and L-cysteine disulfide at carbon ionic liquid electrode.

    Science.gov (United States)

    Safavi, Afsaneh; Ahmadi, Raheleh; Mahyari, Farzaneh Aghakhani

    2014-04-01

    A linear sweep voltammetric method is used for direct simultaneous determination of L-cysteine and L-cysteine disulfide (cystine) based on carbon ionic liquid electrode. With carbon ionic liquid electrode as a high performance electrode, two oxidation peaks for L-cysteine (0.62 V) and L-cysteine disulfide (1.3 V) were observed with a significant separation of about 680 mV (vs. Ag/AgCl) in phosphate buffer solution (pH 6.0). The linear ranges were obtained as 1.0-450 and 5.0-700 μM and detection limits were estimated to be 0.298 and 4.258 μM for L-cysteine and L-cysteine disulfide, respectively. This composite electrode was applied for simultaneous determination of L-cysteine and L-cysteine disulfide in two real samples, artificial urine and nutrient broth. Satisfactory results were obtained which clearly indicate the applicability of the proposed electrode for simultaneous determination of these compounds in complex matrices.

  12. Simultaneous determination of hydroquinone and catechol based on glassy carbon electrode modified with gold-graphene nanocomposite

    International Nuclear Information System (INIS)

    Ma, X.; Liu, Z.; Qiu, C.; Chen, T.; Ma, H.

    2013-01-01

    We have synthesized a virtually monodisperse gold-graphene (Au-G) nanocomposite by a single-step chemical reduction method in aqueous dimethylformamide solution. The nanoparticles are homogenously distributed over graphene nanosheets. A glassy carbon electrode was modified with this nanocomposite and displayed high electrocatalytic activity and extraordinary electronic transport properties due to its large surface area. It enabled the simultaneous determination of hydroquinone (HQ) and catechol (CC) in acetate buffer solution of pH 4.5. Two pairs of well-defined, quasi-reversible redox peaks are obtained, one for HQ and its oxidized form, with a 43 mV separation of peak potentials (ΔEp), the other for CC and its oxidized form, with a ΔEp of 39 mV. Due to the large separation of oxidation peak potentials (102 mV), the concentrations of HQ and CC can be easily determined simultaneously. The oxidation peak currents for both HQ and CC increase linearly with the respective concentrations in the 1.0 μM to 0.1 mM concentration range, with the detection limits of 0.2 and 0. 15 μM (S/N = 3), respectively. The modified electrode was successfully applied to the simultaneous determination of HQ and CC in spiked tap water, demonstrating that the Au-G nanocomposite may act as a high-performance sensing material in the selective detection of some environmental pollutants. (author)

  13. Simultaneous Determination of Hydroquinone and Catechol by Poly (L-methionine Coated Hydroxyl Multiwalled Carbon Nanotube Film

    Directory of Open Access Journals (Sweden)

    Ying Zhang

    2014-07-01

    Full Text Available A simply and high selectively electrochemical method has been developed for the simultaneous determination of hydroquinone and catechol at a glassy carbon electrode modified with the poly L-methionine/multiwall carbon nanotubes, which significantly increased the reversible electrochemical reaction. The electrochemical behavior of catechol and hydroquinone at the modified electrode was studied by cyclic voltammetry and differential pulse voltammetry. The presence of hydroxyl MWCNTs in the composite film enhances the surface coverage concentration of poly L- methionine/multiwall carbon nanotubes. The results suggest that pH=6 is the optimum acidity condition for the selective and simultaneous determination of catechol and hydroquinone. Under the optimized condition, the response peak currents of the modified electrodes were linear over ranges of 8.0´10-7~2.0´10-4 mol/L (R2=0.997 for hydroquinone and 8.0´10-7~2.0´10-4, R2=0.997 for catechol. The sensor also exhibited good sensitivity with the detection limit of 8.0´10-8 mol/L and 1.0´10- 7 mol/L for hydroquinone and catechol, respectively. This study provides a new kind of composite modified electrode for electrochemical sensors with good selectivity and strong anti- interference. It has been applied to simultaneous determination of hydroquinone and catechol in water sample with simplicity and high selectivity.

  14. Simultaneous determination of naphthol isomers at poly(3-methylthiophene)-nano-Au modified electrode with the enhancement of surfactant

    Energy Technology Data Exchange (ETDEWEB)

    Li, Linlin [School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100 (China); Shandong Institute for Product Quality Inspection, Jinan 250100 (China); Liu, Enli; Wang, Xiaolin; Chen, Jia [School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100 (China); Zhang, Xiaoli, E-mail: zhangxl@sdu.edu.cn [School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100 (China)

    2015-08-01

    A polymer film incorporated gold nanoparticle modified electrode was fabricated. The fabricated process involved eletrodeposition of gold nanoparticles and electropolymerization of the 3-methylthiophene (abbreviated 3MT) onto the glassy carbon electrode (GCE). The resulting electrode (P3MT-nano-Au/GCE) was characterized by scanning electron microscopy (SEM), and a simultaneous determination of naphthol isomers at P3MT-nano-Au/GCE was studied using semi-derivative voltammetry. Because of the synergistic effect of gold nanoparticles and poly(3MT), the sensitivity and distinguishability in the simultaneous determination of naphthol isomers were greatly increased. Besides, a further increase in the detecting sensitivity of naphthol isomers could be obtained in the presence of surfactant, cetyl trimethyl ammonium bromide (CTAB). Also, the role of different kinds of surfactants was texted and the action mechanism was discussed in detail. Under the optimal conditions, the linear calibration ranges of the determination of naphthols were 7.0 × 10{sup −7} to 1.5 × 10{sup −4} mol/L for 1-naphthol and 1.0 × 10{sup −6} to 1.5 × 10{sup −4} mol/L for 2-naphthol with detection limits of 1.0 × 10{sup −7} and 3.0 × 10{sup −7} mol/L (S/N = 3), respectively. - Highlights: • Nano-Au-polymer film was fabricated by eletrodeposition and electropolymerization. • Naphthol isomers were detected simultaneously. • Surfactant improved the sensitivity and selectivity.

  15. Compositional Determination of Shale with Simultaneous Neutron and X-ray Tomography

    Science.gov (United States)

    LaManna, J.; Hussey, D. S.; Baltic, E.; Jacobson, D. L.

    2017-12-01

    Understanding the distribution of organic material, mineral inclusions, and porosity are critical to properly model the flow of fluids through rock formations in applications ranging from hydraulic fracturing and gas extraction, CO2 sequestration, geothermal power, and aquifer management. Typically, this information is obtained on the pore scale using destructive techniques such as focused ion beam scanning electron microscopy. Neutrons and X-rays provide non-destructive, complementary probes to gain three-dimensional distributions of porosity, minerals, and organic content along with fluid interactions in fractures and pore networks on the core scale. By capturing both neutron and X-ray tomography simultaneously it is possible to capture slowly dynamic or stochastic processes with both imaging modes. To facilitate this, NIST offers a system for simultaneous neutron and X-ray tomography at the Center for Neutron Research. This instrument provides neutron and X-ray beams capable of penetrating through pressure vessels to image the specimen inside at relevant geological conditions at resolutions ranging from 15 micrometers to 100 micrometers. This talk will discuss current efforts at identifying mineral and organic content and fracture and wettability in shales relevant to gas extraction.

  16. Sample preparation combined with electroanalysis to improve simultaneous determination of antibiotics in animal derived food samples.

    Science.gov (United States)

    da Silva, Wesley Pereira; de Oliveira, Luiz Henrique; Santos, André Luiz Dos; Ferreira, Valdir Souza; Trindade, Magno Aparecido Gonçalves

    2018-06-01

    A procedure based on liquid-liquid extraction (LLE) and phase separation using magnetically stirred salt-induced high-temperature liquid-liquid extraction (PS-MSSI-HT-LLE) was developed to extract and pre-concentrate ciprofloxacin (CIPRO) and enrofloxacin (ENRO) from animal food samples before electroanalysis. Firstly, simple LLE was used to extract the fluoroquinolones (FQs) from animal food samples, in which dilution was performed to reduce interference effects to below a tolerable threshold. Then, adapted PS-MSSI-HT-LLE protocols allowed re-extraction and further pre-concentration of target analytes in the diluted acid samples for simultaneous electrochemical quantification at low concentration levels. To improve the peak separation, in simultaneous detection, a baseline-corrected second-order derivative approach was processed. These approaches allowed quantification of target FQs from animal food samples spiked at levels of 0.80 to 2.00 µmol L -1 in chicken meat, with recovery values always higher than 80.5%, as well as in milk samples spiked at 4.00 µmol L -1 , with recovery values close to 70.0%. Copyright © 2018 Elsevier Ltd. All rights reserved.

  17. Simultaneous determination of triacetin, acetic ether, butyl acetate and amorolfine hydrochloride in amorolfine liniment by HPLC.

    Science.gov (United States)

    Gao, Yuan; Li, Li; Zhang, Jianjun; Shu, Wenjuan; Gao, Liqiong

    2012-04-01

    A simple, rapid, specific and precise reversed-phase high-performance liquid chromatographic method was developed for simultaneous estimation of triacetin, acetic ether, butyl acetate and amorolfine in marketed pharmaceutical liniment. Chromatographic separation was performed on a Shimadzu VP-ODS C(18) column using the mixture of citric acid-hydrochloric acid-sodium hydrate buffer (pH 3.0), acetonitrile and methanol (32:30:38) as the mobile phase at a flow rate of 1.0 mL/min with UV-detection at 215 nm. The method separated the four components simultaneously in less than 10 min. The validation of the method was performed with respect to specificity, linearity, accuracy, and precision. The calibration curves were linear in the range of 35.1-81.9 μ/mL for triacetin, 431.1-1005.9 μ/mL for acetic ether, 167.0-389.7 μ/mL for butyl acetate and 151.0-352.3 μ/mL for amorolfine. The mean 100% spiked recovery for triacetin, acetic ether, butyl acetate and amorolfine is 99.43 ± 0.42, 101.5 ± 1.09, 101.4 ± 1.02 and 100.8 ± 0.69, respectively. The intra-day and inter-day relative standard deviation values were liniment.

  18. [Simultaneous determination of 6 neonicotinoid residues in soil using DLLME-HPLC and UV].

    Science.gov (United States)

    Sun, Bao-li; Shan, Hong; Li, Yan-hua; Zeng, Ya-ling; Shen, Xiu-li; Tong, Cheng-feng

    2013-09-01

    A simple, cheap and rugged method was developed for simultaneous deter mination of 6 neonicotinoid residues in soil, including imidacloprid, acetamiprid, thiamethoxam, thiacloprid, clothianidin and nitenpyram. The soil sample was produced by dispersive liquid-liquid micro-extraction (DLLME) after extracted by the mixed solution of acetonitrile and CH2Cl2 (2:1, phi). The analytes were separated by HPLC with Alltima C18 column (4.6 mm x 250 mm, 5 microm) and detected by PDA at 260 nm. External standard method was used for quantification. The results showed that good linearity was obtained with correlation coefficients between 0.9982 and 0.9999 in the range of 0.5-200 microg x L(-1). The limits of detection (LODs) were in the range between 0.0005 and 0.003 microg x mL(-1) (S/N = 3). The method was validated with five soil samples spiked at three fortification levels (0.05, 0.1, 1.0 mg x kg(-1)) and recoveries were in the range of 55.3%-95.6% with RSD of 1.4%-7.0%. The effect of clean-up was evaluated by UV spectra and demonstrated that the method established is effective. In conclusion, this method is competent for the simultaneous analysis of 6 neonicotinoid residues in soil.

  19. A validated HPTLC method for estimation of moxifloxacin hydrochloride in tablets.

    Science.gov (United States)

    Dhillon, Vandana; Chaudhary, Alok Kumar

    2010-10-01

    A simple HPTLC method having high accuracy, precision and reproducibility was developed for the routine estimation of moxifloxacin hydrochloride in the tablets available in market and was validated for various parameters according to ICH guidelines. moxifloxacin hydrochloride was estimated at 292 nm by densitometry using Silica gel 60 F254 as stationary phase and a premix of methylene chloride: methanol: strong ammonia solution and acetonitrile (10:10:5:10) as mobile phase. Method was found linear in a range of 9-54 nanograms with a correlation coefficient >0.99. The regression equation was: AUC = 65.57 × (Amount in nanograms) + 163 (r(2) = 0.9908).

  20. Stability Indicating RP-HPLC Method for Simultaneous Determination of Aspirin and Clopidrogel in Dosage Form

    International Nuclear Information System (INIS)

    Mohd Gousuddin; Sengupta, P.; Tripathi, V.D.; Das, A.

    2016-01-01

    Stability-indicating High Performance Liquid Chromatographic (HPLC) method was developed for simultaneous Aspirin and Clopidogrel, A Phenomenex Gemini C-18, 5 μm column having 250 mm x 4.6 mm i.d. in isocratic mode, with mobile phase containing buffer solution 0.3 % orthophosphoric acid : acetonitrile (65:35, v/v). The flow rate was 1 ml/ min and effluents were monitored at 266 nm. For linearity seven points calibration curve were obtained in a concentration range from 0.030-0.120 mg/ ml for aspirin and 0.015-0.060 mg/ ml for clopidogrel with correlation coefficient 0.9999. In the present study stability indicating HPLC method for the combination was tested by degrading the drugs together under various stress conditions like acid hydrolysis, base hydrolysis, oxidation, thermal and photolytic stress which is recommended by ICH guideline. (author)

  1. Simultaneous determination of carbohydrates and simmondsins in jojoba seed meal (Simmondsia chinensis) by gas chromatography.

    Science.gov (United States)

    Lein, Sabine; Van Boven, Maurits; Holser, Ron; Decuypere, Eddy; Flo, Gerda; Lievens, Sylvia; Cokelaere, Marnix

    2002-11-22

    Separate methods for the analyses of soluble carbohydrates in different plants and simmondsins in jojoba seed meal are described. A reliable gas chromatographic procedure for the simultaneous quantification of D-pinitol, myo-inositoL sucrose, 5-alpha-D-galactopyranosyl-D-pinitol. 2-alpha-D-galactopyranosyl-D-pinitol, simmondsin, 4-demethylsimmondsin, 5-demethylsimmondsin and 4,5-didemethylsimmondsin as trimethylsilyl derivatives in jojoba seed meal has been developed. The study of different extraction mixtures allowed for the quantitative recovery of the 9 analytes by a mixture of methanol-water (80:20, v/v) in the concentration range between 0.1 and 4%. Comparison of the separation parameters on three different capillary stationary phases with MS detection allowed for the choice of the optimal gas chromatographic conditions for baseline separation of the analytes.

  2. Simultaneous determination of five tetracycline and macrolide antibiotics in feeds using HPCE.

    Science.gov (United States)

    Tong, Jing; Rao, Qinxiong; Zhu, Kui; Jiang, Zhigang; Ding, Shuangyang

    2009-12-01

    This work demonstrates the potential of HPCE in the analysis of antibiotics in a complex matrix such as feedstuffs. Using 20 mM citric acid-40 mM Na(2)HPO(4) buffer (pH 2.65), the five antibiotics, tetracycline, oxytetracycline, doxycycline, tilmicosin, and tylosin were successfully separated at 30 kV in a 64.5 cm x 75 microm id capillary. Good repeatability, stability, and reliability of the method were supported by 70%, and the limit of detection of the five analytes was 0.5-1 mg/kg. It was for the first time that a capillary electrophoretic method was employed to simultaneously detect five tetracycline and macrolide antibiotics in animal feeds.

  3. Chemometric simultaneous determination of Sofosbuvir and Ledipasvir in pharmaceutical dosage form

    Science.gov (United States)

    Khalili, Mahsa; Sohrabi, Mahmoud Reza; Mirzabeygi, Vahid; Torabi Ziaratgahi, Nahid

    2018-04-01

    Partial least squares (PLS), different families of continuous wavelet transform (CWT), and first derivative spectrophotometry (DS) techniques were studied for quantification of Sofosbuvir (SFB) and Ledipasvir (LDV) simultaneously without separation step. The components were dissolved in Acetonitrile and the spectral behaviors were evaluated in the range of 200 to 400 nm. The ultraviolet (UV) absorbance of LDV exhibits no interferences between 300 and 400 nm and it was decided to predict the LDV amount through the classic spectrophotometry (CS) method in this spectral region as well. Data matrix of concentrations and calibrated models were developed, and then by applying a validation set the accuracy and precision of each model were studied. Actual concentrations versus predicted concentrations plotted and good correlation coefficients by each method resulted. Pharmaceutical dosage form was quantified by developed methods and the results were compared with the High Performance Liquid Chromatography (HPLC) reference method. Analysis Of Variance (ANOVA) in 95% confidence level showed no significant differences among methods.

  4. Direct determination of free thyroxine in two simultaneous radioimmunoassays with different test principles

    International Nuclear Information System (INIS)

    Lohkamp, F.; Schmidt, M.

    1982-01-01

    Serum FT 4 was measured simultaneously by the commercial FT 4 kits of Amersham-Buchler and Corning Medical in 4 groups with defined thyroid function as follows: 57 euthroid subjects with and without goitre, 27 patients on T 4 supplementation. 12 subjects on oral contraceptives and 26 subclinically hyperthyroid patients. All patients underwent physical examination, thyroid scintigraphy and additional in-vitro tests (total thyroxine T 4 , total triiodothyronine T 3 and TRH/TSH assay). Both assays generally correlated well with the definded thyroid functional status except for the patients on oral contraceptives. Contrary to the FT 4 -test (Amersham-Buchler) in this group the FT 4 -test (Corning Medical) produced a significantly increased mean for FT 4 as compared to the euthyroid group thus indicating a probably insufficient compensation for high but not necessarily abnormal levels of TBG concentration. Using the FT 4 -assay (Amersham-Buchler) the normal range of FT 4 values of euthyroid subjects from the area of Bamberg with marked iodine deficiency agrees well with recently published results of a multicentre trial thus confirming the assumption of serum FT 4 not being strongly dependent on iodine intake. The results of the FT 4 -test (Corning) showed a wider scatter of normal ranges of FT 4 values for all groups and concomitantly reduced discrimination compared to the corresponding simultaneously obtained FT 4 -test (Amersham-Buchler) results. Though cost and time saving, the commercial radioimmunoassays will require further critical evaluation of normal range validity on larger populations of defined abnormalities will require further critical evaluation of normal range validity on larger populations of defined abnormalities of thyroid function to elucidate inherent deficiencies of the new FT 4 methods and of their diagnostic efficiency. (orig./MG) [de

  5. Multivariate optimization of headspace trap for furan and furfural simultaneous determination in sponge cake.

    Science.gov (United States)

    Cepeda-Vázquez, Mayela; Blumenthal, David; Camel, Valérie; Rega, Barbara

    2017-03-01

    Furan, a possibly carcinogenic compound to humans, and furfural, a naturally occurring volatile contributing to aroma, can be both found in thermally treated foods. These process-induced compounds, formed by close reaction pathways, play an important role as markers of food safety and quality. A method capable of simultaneously quantifying both molecules is thus highly relevant for developing mitigation strategies and preserving the sensory properties of food at the same time. We have developed a unique reliable and sensitive headspace trap (HS trap) extraction method coupled to GC-MS for the simultaneous quantification of furan and furfural in a solid processed food (sponge cake). HS Trap extraction has been optimized using an optimal design of experiments (O-DOE) approach, considering four instrumental and two sample preparation variables, as well as a blocking factor identified during preliminary assays. Multicriteria and multiple response optimization was performed based on a desirability function, yielding the following conditions: thermostatting temperature, 65°C; thermostatting time, 15min; number of pressurization cycles, 4; dry purge time, 0.9min; water / sample amount ratio (dry basis), 16; and total amount (water + sample amount, dry basis), 10g. The performances of the optimized method were also assessed: repeatability (RSD: ≤3.3% for furan and ≤2.6% for furfural), intermediate precision (RSD: 4.0% for furan and 4.3% for furfural), linearity (R 2 : 0.9957 for furan and 0.9996 for furfural), LOD (0.50ng furan g sample dry basis -1 and 10.2ng furfural g sample dry basis -1 ), LOQ (0.99ng furan g sample dry basis -1 and 41.1ng furfural g sample dry basis -1 ). Matrix effect was observed mainly for furan. Finally, the optimized method was applied to other sponge cakes with different matrix characteristics and levels of analytes. Copyright © 2016. Published by Elsevier B.V.

  6. Simultaneous determination of uranium and plutonium in dissolver solution of irradiated fuel, using ID-TIMS. IRP-11

    International Nuclear Information System (INIS)

    Shah, Raju; Sasi Bhushan, K.; Govindan, R.; Alamelu, D.; Khodade, P.S.; Aggarwal, S.K.

    2007-01-01

    A simple sample preparation and simultaneous analysis method to determine uranium and plutonium from dissolver solution, employing the technique of Isotope Dilution Mass spectrometry has been demonstrated. The method used, co-elusion of Uranium and Plutonium from anion exchanger column after initial elution of major part of uranium in 1:5 HNO 3 in order to reduce the initial U/Pu ratio from 1000 to about 100-200 in the co-eluted fraction. Due to the availability of variable multi-collector system, different Faraday cups were adjusted to collect the different ion intensities corresponding to the different masses, during the simultaneous analysis of Uranium and Plutonium, loaded on Re double filament assembly. 233 U and PR grade Plutonium were used as spikes to determine Uranium and Plutonium from dissolver solution of irradiated fuel from research reactor. The possibility of getting the isotopic composition of uranium from the simultaneous analysis of co-eluted purified fraction of U and Pu from spiked aliquots is also explained. (author)

  7. 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.

  8. Simultaneous determination of macronutrients, micronutrients and trace elements in mineral fertilizers by inductively coupled plasma optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira Souza, Sidnei de [Laboratório de Química Analítica Ambiental (LQA), Departamento de Química, Centro de Ciências Exatas e Tecnologia, Universidade Federal de Sergipe (UFS), 49100-000, São Cristovão, SE (Brazil); Silvério Lopes da Costa, Silvânio [Laboratório de Química Analítica Ambiental (LQA), Departamento de Química, Centro de Ciências Exatas e Tecnologia, Universidade Federal de Sergipe (UFS), 49100-000, São Cristovão, SE (Brazil); Coordenação de Química, Universidade Federal de Alagoas (UFAL), Campus Arapiraca, 57309-005, Arapiraca, AL (Brazil); Santos, Dayane Melo; Santos Pinto, Jéssica dos; Garcia, Carlos Alexandre Borges [Laboratório de Química Analítica Ambiental (LQA), Departamento de Química, Centro de Ciências Exatas e Tecnologia, Universidade Federal de Sergipe (UFS), 49100-000, São Cristovão, SE (Brazil); and others

    2014-06-01

    An analytical method for simultaneous determination of macronutrients (Ca, Mg, Na and P), micronutrients (Cu, Fe, Mn and Zn) and trace elements (Al, As, Cd, Pb and V) in mineral fertilizers was optimized. Two-level full factorial design was applied to evaluate the optimal proportions of reagents used in the sample digestion on hot plate. A Doehlert design for two variables was used to evaluate the operating conditions of the inductively coupled plasma optical emission spectrometer in order to accomplish the simultaneous determination of the analyte concentrations. The limits of quantification (LOQs) ranged from 2.0 mg kg{sup −1} for Mn to 77.3 mg kg{sup −1} for P. The accuracy and precision of the proposed method were evaluated by analysis of standard reference materials (SRMs) of Western phosphate rock (NIST 694), Florida phosphate rock (NIST 120C) and Trace elements in multi-nutrient fertilizer (NIST 695), considered to be adequate for simultaneous determination. Twenty-one samples of mineral fertilizers collected in Sergipe State, Brazil, were analyzed. For all samples, the As, Ca, Cd and Pb concentrations were below the LOQ values of the analytical method. For As, Cd and Pb the obtained LOQ values were below the maximum limit allowed by the Brazilian Ministry of Agriculture, Livestock and Food Supply (Ministério da Agricultura, Pecuária e Abastecimento — MAPA). The optimized method presented good accuracy and was effectively applied to quantitative simultaneous determination of the analytes in mineral fertilizers by inductively coupled plasma optical emission spectrometry (ICP OES). - Highlights: • Determination of inorganic constituents in mineral fertilizers was proposed. • Experimental design methodology was used to optimize analytical method. • The sample preparation procedure using diluted reagents (HNO{sub 3} and H{sub 2}O{sub 2}) was employed. • The analytical method was satisfactorily to the determination of thirteen elements. • The

  9. A METHOD OF AUTOMATIC DETERMINATION OF THE NUMBER OF THE ELECTRICAL MOTORS SIMULTANEOUSLY WORKING IN GROUP

    Directory of Open Access Journals (Sweden)

    A. V. Voloshko

    2016-11-01

    Full Text Available Purpose. Propose a method of automatic determination of the number of operating high voltage electric motors in the group of the same type based on the determination and analysis of the account data of power consumption, obtained from of electric power meters installed at the connection of motors. Results. The algorithm of the automatic determination program for the number of working in the same group of electric motors, which is based on the determination of the motor power minimum value at which it is considered on, was developed. Originality. For the first time a method of automatic determination of the number of working of the same type high-voltage motors group was proposed. Practical value. Obtained results may be used for the introduction of an automated accounting run of each motor, calculating the parameters of the equivalent induction motor or a synchronous motor.

  10. Analysis of odorous gases with simultaneous GC-MS and sensory determination

    Energy Technology Data Exchange (ETDEWEB)

    Orko, I.; Lehtomaeki, J.; Sandell, E.; Arnold, M. [VTT Chemical Technology, Espoo (Finland). Environmental Technology

    1995-12-31

    Industrial odorous off-gases can consist of hundreds of different compounds giving cause to odour annoyance in the vicinity of the odour-emitting plant. For the identification of the odorous components in the gas, traditional analytical methods are not always sufficient since the odour threshold values cannot often be found in literature. This report describes the development of a GC-MS sniffing port method for identifying odorous compounds in off-gases. In the method the sample is injected into a gas chromatograph and divided into two flows. The compounds in these sample flows are separated in two identical columns and detected simultaneously in a mass spectrometer and by sensory means. The olfactory detections are marked in the iongram and the odorous compounds are identified. Tenax TA adsorbent is generally used for collecting the odorous sample for analysis. The compounds are released from the adsorbent for analysis by thermal desorption. The report also describes a case study where the GC-MS sniffing port method was applied to a gaseous emission from a food factory. Over ten odorous compounds could be identified. (author)

  11. Ultrasound-assisted extraction method for the simultaneous determination of emerging contaminants in freshwater sediments.

    Science.gov (United States)

    de Sousa, Diana Nara Ribeiro; Grosseli, Guilherme Martins; Mozeto, Antonio Aparecido; Carneiro, Renato Lajarim; Fadini, Pedro Sergio

    2015-10-01

    Sediments are the fate of several emerging organic contaminants, such as pharmaceuticals, personal care products and hormones, and therefore an important subject in environmental monitoring studies. In the present work, a simple and sensitive method was developed, validated and applied for the simultaneous extraction of atenolol, caffeine, carbamazepine, diclofenac, ibuprofen, naproxen, propranolol, triclosan, estrone, 17-β-estradiol and 17-α-ethinylestradiol using ultrasound-assisted extraction from freshwater sediment samples followed by solid-phase extraction clean-up and liquid chromatography with tandem mass spectrometry detection. The solvent type and extraction pH were evaluated to obtain the highest recoveries of the compounds. The best method shows absolute recoveries between 54.0 and 94.4% at 50 ng/g concentration. The method exhibits good precision with relative standard deviation ranging from 1.0-16%. The detection and quantification limits ranged from 0.006-0.067 and 0.016-0.336 ng/g, respectively. The developed method was successfully applied to freshwater sediment samples collected from different sites in Jundiaí River basin of São Paulo State, Brazil. The compounds atenolol, caffeine, propranolol and triclosan were detected in all the sampling sites with concentrations of 13.8, 41.0, 28.5 and 176 ng/g, respectively. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Aptamer-functionalized magnetic nanoparticles for simultaneous fluorometric determination of oxytetracycline and kanamycin

    International Nuclear Information System (INIS)

    Liu, Changbin; Lu, Chunxia; Tang, Zonggui; Chen, Xia; Wang, Guohong; Sun, Fengxia

    2015-01-01

    This work describes a method for the simultaneous detection of oxytetracycline (OTC) and kanamycin (KMY) using aptamers acting as both recognition and separation elements, and complementary oligonucleotides labeled with a green emitting fluorophore (carboxyfluorescein, FAM) and a yellow emitting fluorophore (carboxy-X-rhodamine, ROX), respectively, as signal labels. An OTC aptamer and a KMY aptamer were immobilized on the surface of magnetic nanoparticles (MNPs) via avidin-biotin chemistry. The aptamers preferentially bind their respective targets and thereby cause the upconcentration of analytes. However, in their absence they bind fluorescently-tagged complementary oligonucleotide later added to the reaction system. This cause the NPs to become fluorescent, with emission peaks located at 520 and 608 nm, respectively. The effects of the concentration of avidin, aptamer, complementary oligonucleotide, incubation temperature and incubation time were optimized. Under the optimal conditions, linear relationships were obtained in the range of 1–50 ng∙mL −1 for OTC and KMY, with limits of detection of 0.85 ng∙mL −1 and 0.92 ng∙mL −1 , respectively. The method was applied to the analysis of pork, milk, and honey samples spiked with OTC and MKY. Recoveries ranged from 76.5 to 94.7 % and 77.8 to 93.1 %, respectively, and the relative standard deviation was <10.0 %. (author)

  13. Determination of temperature dependant viscosity values of lubricants via simultaneous measurements of refractive index

    International Nuclear Information System (INIS)

    Yaltkaya, S.

    2005-01-01

    Viscosity is one of the most important parameter in rheological and tribological properties of fluids. The objective of this study is to obtain the viscosity values from the simultaneous refractive-index measurements of lubricants, simply by dipping the fiber-optic probe into the oil to be measured. Due to the fact that these parameters are temperature dependent, within the interval under consideration, oil heated up steadily while measuring the viscosity and refractive index at the same time. The refractive index sensor, the digital viscometer and the thermometer were connected to a PC via an analog to digital converter and the values were acquired at the same time. The fiber optic refractive index sensor has been designed in our laboratory. By utilising Fresnel's fundamental reflection law, the intensity of reflected light from boundary surface (optic fiber core-motor oil) was measured at 660 nm wavelength and then refractive index of the oil was calculated. The derived refractive index values were converted viscosity values that acquired by using the calibration equation. The viscometer, used during the study, was the rotational Brookfield type

  14. Simultaneous determination of dynamic cardiac metabolism and function using PET/MRI.

    Science.gov (United States)

    Barton, Gregory P; Vildberg, Lauren; Goss, Kara; Aggarwal, Niti; Eldridge, Marlowe; McMillan, Alan B

    2018-05-01

    Cardiac metabolic changes in heart disease precede overt contractile dysfunction. However, metabolism and function are not typically assessed together in clinical practice. The purpose of this study was to develop a cardiac positron emission tomography/magnetic resonance (PET/MR) stress test to assess the dynamic relationship between contractile function and metabolism in a preclinical model. Following an overnight fast, healthy pigs (45-50 kg) were anesthetized and mechanically ventilated. 18 F-fluorodeoxyglucose ( 18 F-FDG) solution was administered intravenously at a constant rate of 0.01 mL/s for 60 minutes. A cardiac PET/MR stress test was performed using normoxic gas (F I O 2  = .209) and hypoxic gas (F I O 2  = .12). Simultaneous cardiac imaging was performed on an integrated 3T PET/MR scanner. Hypoxic stress induced a significant increase in heart rate, cardiac output, left ventricular (LV) ejection fraction (EF), and peak torsion. There was a significant decline in arterial SpO 2 , LV end-diastolic and end-systolic volumes in hypoxia. Increased LV systolic function was coupled with an increase in myocardial FDG uptake (Ki) during hypoxic stress. PET/MR with continuous FDG infusion captures dynamic changes in both cardiac metabolism and contractile function. This technique warrants evaluation in human cardiac disease for assessment of subtle functional and metabolic abnormalities.

  15. Automated determination of fibrillar structures by simultaneous model building and fiber diffraction refinement.

    Science.gov (United States)

    Potrzebowski, Wojciech; André, Ingemar

    2015-07-01

    For highly oriented fibrillar molecules, three-dimensional structures can often be determined from X-ray fiber diffraction data. However, because of limited information content, structure determination and validation can be challenging. We demonstrate that automated structure determination of protein fibers can be achieved by guiding the building of macromolecular models with fiber diffraction data. We illustrate the power of our approach by determining the structures of six bacteriophage viruses de novo using fiber diffraction data alone and together with solid-state NMR data. Furthermore, we demonstrate the feasibility of molecular replacement from monomeric and fibrillar templates by solving the structure of a plant virus using homology modeling and protein-protein docking. The generated models explain the experimental data to the same degree as deposited reference structures but with improved structural quality. We also developed a cross-validation method for model selection. The results highlight the power of fiber diffraction data as structural constraints.

  16. Screening of Chemical Dyes in Traditional Chinese Medicine by HPTLC-MS.

    Science.gov (United States)

    He, Fengyan; He, Yi; Zheng, Xiaowei; Wang, Ruizhong; Lu, Jing; Dai, Zhong; Ma, Shuangcheng

    2018-05-01

    It has been uncovered that chemical dyes are illegally used in traditional Chinese medicines to brighten color and cover up inferiority, which threaten the safety of patients. In the present study, an HPTLC-MS method was developed for the effective screening of 11 chemical dyes (Sudan I, II, III, and IV; 808 Scarlet; Sudan Red 7B; malachite green; Basic Orange 2; auramine; Orange II; and erythrosine) in traditional Chinese medicine (TCM) raw materials and Chinese patent medicines. Firstly, unwashed HPTLC plates were chosen by comparing the background signals of the TLC plates used directly and prewashed with analytical grade and HPLC grade solvents. Twice developments were conducted to isolate chemical dyes of different polarity. Possible adulterants were preliminarily identified by comparing Rf values and in situ UV-Vis spectra with those of the references. Further confirmation was conducted by tandem MS analysis via an elution head-based TLC-MS interface. Sudan I and IV, 808 Scarlet, and Orange II were successfully detected in eight batches of TCM. The proposed method could be applied as a reliable technology for the screening of chemical dyes in TCM.

  17. SIMULTANEOUS ULTRAVIOLET AND OPTICAL EMISSION-LINE PROFILES OF QUASARS: IMPLICATIONS FOR BLACK HOLE MASS DETERMINATION

    International Nuclear Information System (INIS)

    Ho, Luis C.; Dong Xiaobo; Goldoni, Paolo; Ponti, Gabriele; Greene, Jenny E.

    2012-01-01

    The X-shooter instrument on the Very Large Telescope was used to obtain spectra of seven moderate-redshift quasars simultaneously covering the spectral range ∼3000 Å to 2.5 μm. At z ≈ 1.5, most of the prominent broad emission lines in the ultraviolet to optical region are captured in their rest frame. We use this unique data set, which mitigates complications from source variability, to intercompare the line profiles of C IV λ1549, C III] λ1909, Mg II λ2800, and Hα and evaluate their implications for black hole (BH) mass estimation. We confirm that Mg II and the Balmer lines share similar kinematics and that they deliver mutually consistent BH mass estimates with minimal internal scatter (∼<0.1 dex) using the latest virial mass estimators. Although no virial mass formalism has yet been calibrated for C III], this line does not appear promising for such an application because of the large spread of its velocity width compared to lines of both higher and lower ionization; part of the discrepancy may be due to the difficulty of deblending C III] from its neighboring lines. The situation for C IV is complex and, because of the limited statistics of our small sample, inconclusive. On the one hand, slightly more than half of our sample (4/7) have C IV line widths that correlate reasonably well with Hα line widths, and their respective BH mass estimates agree to within ∼0.15 dex. The rest, on the other hand, exhibit exceptionally broad C IV profiles that overestimate virial masses by factors of 2-5 compared to Hα. As C IV is widely used to study BH demographics at high redshifts, we urgently need to revisit our analysis with a larger sample.

  18. Simultaneous determination of inorganic anions and cations by supercritical fluid chromatography using evaporative light scattering detection.

    Science.gov (United States)

    Foulon, Catherine; Di Giulio, Pauline; Lecoeur, Marie

    2018-01-26

    Supercritical fluid chromatography (SFC) is commonly used for the analysis of non-polar compounds, but remains poorly explored for the separation of polar and ionized molecules. In this paper, SFC has been investigated for the separation of 14 inorganic ions sampled in aqueous solutions. Four polar stationary phases were first screened using CO 2 -methanol-based mobile phases containing water or different acidic or basic additives, in order to select the most efficient conditions for the simultaneous retention of inorganic cations and anions and to favor their detection using evaporative light scattering detector (ELSD). Orthogonal selectivity was obtained depending on the stationary phase used: whereas anions are less retained on HILIC stationary phase, 2-ethylpyridine (2-EP) stationary phase exhibits strong interaction for anions. Best results were obtained under gradient elution mode using a 2-EP stationary phase and by adding 0.2% triethylamine in the CO 2 -methanol-based mobile phase. The composition of the injection solvent was also investigated. The results showed that a methanolic sample containing a percentage of water not exceeding 20% does not affect the analytical performances obtained on 2-EP. Moreover, the presence of triethylamine in the injection solvent contributes to eliminate peaks shoulders. Among the 14 inorganic ions tested, three cations (Li + , Ca 2+ and Mg 2+ ) and five anions (Cl - , Br - , NO 3 - , I - , SCN - ) were totally resolved in 15 min. NO 3 - and NO 2 - still coeluted in the final optimized conditions. The other investigated ions were either strongly retained on the stationary phase or not detected by the ELSD. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Application of adsorptive stripping voltammetry to the simultaneous determination of bismuth and copper in the presence of nuclear fast red

    International Nuclear Information System (INIS)

    Gholivand, M.B.; Romiani, A.A.

    2006-01-01

    A sensitive and selective method for the simultaneous determination of copper and bismuth by adsorptive stripping was developed using nuclear fast red (2-anthracenesulfonic acid, 4-amino-9,10-dihydro-1,3-dihydroxy-9,10-dioxo-, monosodium salt) as selective complexing agent onto hanging mercury drop electrode. In a single scan both metals gave peaks that were distinctly separated by 85 mV allowing their determination in the presence of each other. Optimal analytical conditions were found to be: nuclear fast red concentration of 80 μM, pH of 2.8 and adsorptive potential of -300 mV versus Ag/AgCl. With accumulation time of 180 s the peaks currents are proportional to concentration of copper and bismuth over the 1-100 and 5-60 ng mL -1 range with detection limits of 0.2 and 1.2 ng mL -1 , respectively. The procedure was applied to simultaneous determination of copper and bismuth in some real samples

  20. Simultaneous determination of paracetamol, 4-Aminophenol, 4-Chloroacetanilid, Benzyl alcohol,Benzaldehyde and EDTA by HPLC methodin paracetamol injection ampoule

    Directory of Open Access Journals (Sweden)

    Ali Merrikhi Khosroshahi

    2016-06-01

    Full Text Available Paracetamol that is known as acetaminophen have the most consume as an analgesic and antipyretic drug in the world. That is formulated in single compound or mixture at many forms such as tablets, syrups, suspensions and drops. The last form is intravenous injections. Paracetamol derived from 4-minophenol which is synthesized by acylated the P-acetaminophenol and acetic anhydride. 4-aminophenol is the main impurity at manufacturing of paracetamol which could produce by hydrolysis during storage or synthesis under normal conditions (temperature, pH, etc.. Also, 4-chloroacetanilid may be observed as an impurity in the raw material of paracetamol synthesis. Benzyl alcohol is a preservative that used in Paracetamol for injection. It will be very important if there are analytical techniques to measuring paracetamol and its degradation products accurately and easily. Undoubtedly the most important and widely used, separation technique is chromatography. There are several reports about separation and quantitative determination of paracetamol lonely or simultaneous determination of paracetamol and 4-aminophenol. In this paper investigated simultaneous determination of paracetamol, 4-aminophenol, 4-chloroacetanilid, benzyl alcohol, benzaldehyde, and EDTA in paracetamol for injection ampoules by high performance liquid chromatography. By changing the ratio of mixing methanol and acetonitrile as mobile phase at the wavelength of 215 nm and pH=3 separation of all compounds were completely done.

  1. A Validated Stability-Indicating HPLC Method for Simultaneous Determination of Amoxicillin and Enrofloxacin Combination in an Injectable Suspension

    Directory of Open Access Journals (Sweden)

    Nidal Batrawi

    2017-02-01

    Full Text Available The combination of amoxicillin and enrofloxacin is a well-known mixture of veterinary drugs; it is used for the treatment of Gram-positive and Gram-negative bacteria. In the scientific literature, there is no high-performance liquid chromatography (HPLC-UV method for the simultaneous determination of this combination. The objective of this work is to develop and validate an HPLC method for the determination of this combination. In this regard, a new, simple and efficient reversed-phase HPLC method for simultaneous qualitative and quantitative determination of amoxicillin and enrofloxacin, in an injectable preparation with a mixture of inactive excipients, has been developed and validated. The HPLC separation method was performed using a reversed-phase (RP-C18e (250 mm × 4.0 mm, 5 μm column at room temperature, with a gradient mobile phase of acetonitrile and phosphate buffer containing methanol at pH 5.0, a flow rate of 0.8 mL/min and ultraviolet detection at 267 nm. This method was validated in accordance with the Food and Drug Administration (FDA and the International Conference on Harmonisation (ICH guidelines and showed excellent linearity, accuracy, precision, specificity, robustness, ruggedness, and system suitability results within the acceptance criteria. A stability-indicating study was also carried out and indicated that this method can also be used for purity and degradation evaluation of these formulations.

  2. Simultaneous determination of short-to-medium lived nuclides in Ghanaian food items using INAA and Compton suppression counting

    International Nuclear Information System (INIS)

    Nyarko, B.J.B.; Fletcher, J.J.; Zwicker, B.; Chatt, A.

    2006-01-01

    An instrumental neutron activation analysis (INAA) method was developed for the simultaneous determination of 19 elements in 10 individual food items from Ghana. The samples were irradiated for 1 minutes in a neutron flux of 2.5 x 10 11 n x cm -2 x s -1 at the Dalhousie University Slowpoke-2 reactor (DUSR) facility. After a 2-minute decay the samples were counted using a Compton suppression gamma-ray spectrometry system for 10 minutes to quantify Ba, Br, Ca, Cl, Co, Cu, Dy, K, Mg, Mn, Na, Rb, S, Sr, Th, Ti, U, V and Zn. The analytical procedure namely, irradiation, decay and counting times were optimized for quick turn-around time for simultaneous determination of the nineteen elements. White-seeded beans (Phaseolus coccineus), one of the most commonly consumed foodstuff in Ghana, were found to contain the highest level of the 19 elements determined, viz. K (1.4%) and Sorghum spp. the lowest level viz. Dy (2.2 ng x g -1 ). Two NIST SRMs were used for internal quality control. The concentrations of most of the elements were found to be within ±6% of the certified or information values. The precisions were calculated from six replicate measurements and were found to be within 10%. (author)

  3. A new electrochemical sensor for the simultaneous determination of acetaminophen and codeine based on porous silicon/palladium nanostructure.

    Science.gov (United States)

    Ensafi, Ali A; Ahmadi, Najmeh; Rezaei, Behzad; Abarghoui, Mehdi Mokhtari

    2015-03-01

    A porous silicon/palladium nanostructure was prepared and used as a new electrode material for the simultaneous determination of acetaminophen (ACT) and codeine (COD). Palladium nanoparticles were assembled on porous silicon (PSi) microparticles by a simple redox reaction between the Pd precursor and PSi in an aqueous solution of hydrofluoric acid. This novel nanostructure was characterized by different spectroscopic and electrochemical techniques including scanning electron microscopy, X-ray diffraction, energy dispersive X-ray spectroscopy, fourier transform infrared spectroscopy and cyclic voltammetry. The high electrochemical activity, fast electron transfer rate, high surface area and good antifouling properties of this nanostructure enhanced the oxidation peak currents and reduced the peak potentials of ACT and COD at the surface of the proposed sensor. Simultaneous determination of ACT and COD was explored using differential pulse voltammetry. A linear range of 1.0-700.0 µmol L(-1) was achieved for ACT and COD with detection limits of 0.4 and 0.3 µmol L(-1), respectively. Finally, the proposed method was used for the determination of ACT and COD in blood serum, urine and pharmaceutical compounds. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. Simultaneous determination of dysprosium, holmium and erbium in high purity rare earth oxides by second order derivative spectrophotometry

    International Nuclear Information System (INIS)

    Anbu, M.; Prasada Rao, T.; Iyer, C. S. P.; Damodaran, A. D.

    1996-01-01

    High purity individual rare earth oxides are increasingly used as major components in lasers (Y 2 O 3 ), phosphors (YVO 3 , Eu 2 O 3 ), magnetic bubble memory films (Gd 2 O 3 ) and refractive-index lenses and fibre optics (La 2 O 3 ). The determination of individual lanthanides in high purity rare earth oxides is a more important and difficult task. This paper reports the utilization of higher order derivative spectrophotometry for the simultaneous determination of dysprosium, holmium and erbium in high purity rare earth oxides. The developed procedure is simple, reliable and allows the determination of 0.001 to 0.2% of dysprosium, holmium and erbium in several rare earth. (author). 9 refs, 2 figs, 2 tabs

  5. Simultaneous Determination of Preservatives (Methyl Paraben and Propyl Paraben in Sucralfate Suspension Using High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Rajesh M. Kashid

    2011-01-01

    Full Text Available A reversed phase HPLC method that allows the separation and simultaneous determination of the preservatives methyl paraben (M.P. and propyl paraben (P.P. is described. The separations were effected by using an initial mobile phase of water: acetonitrile (50:50 on Inertsil C18 to elute P.P. and M.P. The detector wavelength was set at 205 nm. Under these conditions, separation of the two components was achieved in less than 10 min. Analytical characteristics of the separation such as precision, specificity, linear range and reproducibility were evaluated. The developed method was applied for the determination of preservative M.P. and P.P. at concentration of 0.01 mg/mL and 0.1 mg/mL respectively. The method was successfully used for determining both compounds in sucralfate suspension.

  6. Simultaneous determination of oxalic, citric, nitrilotriacetic and ethylenediamenetetraacetic acids by gas liquid chromatography of their methyl esters

    International Nuclear Information System (INIS)

    Eskell, C.J.; Pick, M.E.

    1980-04-01

    A procedure for simultaneous determination of ethylenediaminetetraacetic acid (EDTA), nitrilotriacetic acid (NTA), citric acid and oxalic acid by gas liquid chromatography is described. The involatile acids are first concerted to their volatile methyl ester derivatives by reaction with boron trifluoride in methanol. Transition metal ions (Fe 3+ , Cr 3+ and Ni 2+ ) which will be present in decontamination liquors from nuclear reactors, and form strong chelates with the acids, have been shown to cause no interference to the esterification reaction. The esters were separated by temperature programming on a 3.5 metre capillary column packed with 3% OV1 on Diatomite CQ and were detected by flame ionisation. (author)

  7. Simultaneous Determination of Preservatives (Methyl Paraben and Propyl Paraben) in Sucralfate Suspension Using High Performance Liquid Chromatography

    OpenAIRE

    M. Kashid, Rajesh; G. Singh, Santosh; Singh, Shrawan

    2011-01-01

    A reversed phase HPLC method that allows the separation and simultaneous determination of the preservatives methyl paraben (M.P.) and propyl paraben (P.P.) is described. The separations were effected by using an initial mobile phase of water: acetonitrile (50:50) on Inertsil C18 to elute P.P. and M.P. The detector wavelength was set at 205 nm. Under these conditions, separation of the two components was achieved in less than 10 min. Analytical characteristics of the separation such as precisi...

  8. Simultaneous determination of the intravenous and oral pharmacokinetic parameters of D,L-verapamil using stable isotope-labelled verapamil.

    Science.gov (United States)

    Eichelbaum, M; Somogyi, A; von Unruh, G E; Dengler, H J

    1981-01-01

    Following i.v. administration, the plasma concentration-time curve of verapamil could best be described by either a mono- or biexponential equation. Total plasma clearance (1.26 1/min) approached liver blood flow (1.51/min), so it can be concluded that its clearance is liver blood flow-dependent. Although absorption was almost complete after oral administration, absolute bioavailability (20%) was low, due to extensive hepatic first-pass metabolism. The approach using stable isotope-labelled and unlabelled drug permits simultaneous administration by the intravascular and extravascular routes, thus allowing determination of absolute bioavailability in a single experiment.

  9. Simple, simultaneous gravimetric determination of calcite and dolomite in calcareous soils

    Science.gov (United States)

    Literature pertaining to determination of calcite and dolomite is not modern and describes slow methods that require expensive specialized apparatus. The objective of this paper was to describe a new method that requires no specialized equipment. Linear regressions and correlation coefficients for...

  10. Simultaneous multielement determination of chewing and snuff tobaccos used in India by INAA

    International Nuclear Information System (INIS)

    Mishra, U.C.; Shaikh, G.N.

    1986-01-01

    Trace elements present in Indian cigarette tobacco and cigarette smoke were reported earlier. This paper presents trace element concentrations in chewing and snuff tobaccos determined by INAA. The levels of Br, Co, Cr, Fe, Mn, Zn, etc., present in different brands of chewing and snuff tobaccos are compared in two types of tobacco as well as with similar data from other countires. (author)

  11. Simultaneous polarographic determination of micro amounts of vanadium(V) and molybdenum(VI)

    International Nuclear Information System (INIS)

    Rao, V.S.N.; Rao, S.B.

    1979-01-01

    A simple and sensitive polarographic method has been developed for the determination of micro quantities of vanadium(V) and molybdenum(VI), based on the reduction of bromate, which is catalysed by these metal ions in the presence of 2,4-dihydroxyacetophenone oxime. Interference by various cations and anions has been investigated. (author)

  12. Simultaneous determination of seven flavonoids in Epimedium by liquid chromatography-tandem mass spectrometry method

    Institute of Scientific and Technical Information of China (English)

    Cai Sheng Wu; Bao Lin Guo; Yu Xin Sheng; Jin Lan Zhang

    2008-01-01

    In this paper, a sensitive and specific liquid chromatography-electrospray ionisation-mass spectrometry (LC-ESI-MS) method has been developed and validated for the identification and determination of seven flavonoids, namely epimedin A, epimedin B, epimedin C, icariin, sagittatoside B, 2"-0-rhamnosyl icariside II, and baohuoside I in Epimedium from different sources.

  13. Spectroscopic characterization of Simultaneous determination of Albendazol from the sugar cane (Saccharum officinarum L.) wax

    International Nuclear Information System (INIS)

    Marrero Delange, David; Cora Medina, Miriam; Laguna Granja, Abilio; Gonzalez Canavaciolo, Victor L

    2013-01-01

    D-003, an active pharmaceutical ingredient (API) purified from sugar cane (Saccharum officinarum L.) wax with cholesterol-lowering and antioxidant effects, is composed of a mixture of free saturated very long chain fatty acids (VLCFAs), each within specific relative concentration ranges as determined by the gas chromatography (GC). However, the spectroscopic characterization of D-003 had not been previously reported

  14. Dot immunoassay for the simultaneous determination of postvaccination immunity against pertussis, diphtheria, and tetanus.

    Science.gov (United States)

    Khramtsov, Pavel; Bochkova, Maria; Timganova, Valeria; Zamorina, Svetlana; Rayev, Mikhail

    2017-06-01

    A dot immunoassay for simultaneous semiquantitative detection of IgG against tetanus toxoid (Ttx) and diphtheria toxoid (Dtx) and qualitative detection of anti-Bordetella pertussis IgGs in human blood serum using carbon nanoparticles functionalized with streptococcal protein G was developed. Inactivated B. pertussis cells in suspension form were used as an antigen in the immunoassay. Pertussis, tetanus, and diphtheria antigens were separately spotted onto nitrocellulose strips, and then the immunostrips were successively incubated with blood sera and a suspension of carbon nanoparticles. The immunostrips were then scanned with a flatbed scanner, and the images obtained were processed with ImageJ. One hundred fifty-five venous blood serum samples from children vaccinated with diphtheria, tetanus, and whole-cell pertussis (DTwP) vaccine were tested in comparison with a conventional ELISA and agglutination test. The total time required for analysis of 32 serum samples was less than 3 h. Comparison between the results of the dot immunoassay and the corresponding ELISA/agglutination test revealed a high level of agreement (Cohen's kappa between 0.765 and 0.813). The lower limit of quantification was 0.06 IU/ml for anti-Ttx and anti-Dtx. The intra-assay coefficients of variation were less than 15% for anti-Ttx and anti-Dtx and less than 10% for anti-pertussis. The diagnostic sensitivity of detection of the antibody protection level was 93.5% for anti-Ttx [95% confidence interval (CI) 83.5-97.9%], 92.4% for anti-Dtx (95% CI 80.9297.5%), and 90.2% for anti-pertussis (95% CI 75.9-96.8%). The diagnostic specificity was 90.9% for anti-Ttx (95% CI 57.1-99.5%), 85% for anti-Dtx (95% CI 61.1-96.0%), and 89.3% for anti-pertussis (95%CI 80.8-94.5%). The dot immunoassay developed does not require expensive reading equipment, and allows detection of antibodies against three antigens in a single analysis. The immunostrips can be stored for a long time without changes in the

  15. Determinants for simultaneous binding of copper and platinum to human chaperone Atox1: hitchhiking not hijacking.

    Directory of Open Access Journals (Sweden)

    Maria E Palm-Espling

    Full Text Available Cisplatin (CisPt is an anticancer agent that has been used for decades to treat a variety of cancers. CisPt treatment causes many side effects due to interactions with proteins that detoxify the drug before reaching the DNA. One key player in CisPt resistance is the cellular copper-transport system involving the uptake protein Ctr1, the cytoplasmic chaperone Atox1 and the secretory path ATP7A/B proteins. CisPt has been shown to bind to ATP7B, resulting in vesicle sequestering of the drug. In addition, we and others showed that the apo-form of Atox1 could interact with CisPt in vitro and in vivo. Since the function of Atox1 is to transport copper (Cu ions, it is important to assess how CisPt binding depends on Cu-loading of Atox1. Surprisingly, we recently found that CisPt interacted with Cu-loaded Atox1 in vitro at a position near the Cu site such that unique spectroscopic features appeared. Here, we identify the binding site for CisPt in the Cu-loaded form of Atox1 using strategic variants and a combination of spectroscopic and chromatographic methods. We directly prove that both metals can bind simultaneously and that the unique spectroscopic signals originate from an Atox1 monomer species. Both Cys in the Cu-site (Cys12, Cys15 are needed to form the di-metal complex, but not Cys41. Removing Met10 in the conserved metal-binding motif makes the loop more floppy and, despite metal binding, there are no metal-metal electronic transitions. In silico geometry minimizations provide an energetically favorable model of a tentative ternary Cu-Pt-Atox1 complex. Finally, we demonstrate that Atox1 can deliver CisPt to the fourth metal binding domain 4 of ATP7B (WD4, indicative of a possible drug detoxification mechanism.

  16. Simultaneous determination of mass and thermal accommodation coefficients from temporal evolution of an evaporating water microdroplet

    International Nuclear Information System (INIS)

    Zientara, M; Jakubczyk, D; Derkachov, G; Kolwas, K; Kolwas, M

    2005-01-01

    Scattering of coherent light by an evaporating droplet of pure water several micrometres in size was investigated. The droplet was levitated in an electrodynamic trap placed in a small climatic chamber. The evolution of the droplet radius and the evolution dynamics were investigated by means of analysing the scattering patterns with the aid of Mie theory. A numerical model of droplet evolution, incorporating the kinetic effects near the droplet surface, was constructed. Application of this model to the experimental data allowed us to determine the mass and thermal accommodation coefficients to be α C = 0.12 ± 0.02 and α T = 0.65 ± 0.09, respectively. This model enabled us to determine with high precision the temperature evolution of the droplet and the relative humidity in the droplet vicinity

  17. Derivative spectrophotometric method for simultaneous determination of zofenopril and fluvastatin in mixtures and pharmaceutical dosage forms.

    Science.gov (United States)

    Stolarczyk, Mariusz; Maślanka, Anna; Apola, Anna; Rybak, Wojciech; Krzek, Jan

    2015-09-05

    Fast, accurate and precise method for the determination of zofenopril and fluvastatin was developed using spectrophotometry of the first (D1), second (D2), and third (D3) order derivatives in two-component mixtures and in pharmaceutical preparations. It was shown, that the developed method allows for the determination of the tested components in a direct manner, despite the apparent interference of the absorption spectra in the UV range. For quantitative determinations, "zero-crossing" method was chosen, appropriate wavelengths for zofenopril were: D1 λ=270.85 nm, D2 λ=286.38 nm, D3 λ=253.90 nm. Fluvastatin was determined at wavelengths: D1 λ=339.03 nm, D2 λ=252.57 nm, D3 λ=258.50 nm, respectively. The method was characterized by high sensitivity and accuracy, for zofenopril LOD was in the range of 0.19-0.87 μg mL(-1), for fluvastatin 0.51-1.18 μg mL(-1), depending on the class of derivative, and for zofenopril and fluvastatin LOQ was 0.57-2.64 μg mL(-1) and 1.56-3.57 μg mL(-1), respectively. The recovery of individual components was within the range of 100±5%. For zofenopril, the linearity range was estimated between 7.65 μg mL(-1) and 22.94 μg mL(-1), and for fluvastatin between 5.60 μg mL(-1) and 28.00 μg mL(-1). Copyright © 2015 Elsevier B.V. All rights reserved.

  18. Method and apparatus for simultaneous determination of fluid mass flow rate, mean velocity and density

    International Nuclear Information System (INIS)

    Hamel, W.R.

    1984-01-01

    This invention relates to a new method and new apparatus for determining fluid mass flow rate and density. In one aspect of the invention, the fluid is passed through a straight cantilevered tube in which transient oscillation has been induced, thus generating Coriolis damping forces on the tube. The decay rate and frequency of the resulting damped oscillation are measured, and the fluid mass flow rate and density are determined therefrom. In another aspect of the invention, the fluid is passed through the cantilevered tube while an electrically powered device imparts steady-state harmonic excitation to the tube. This generates Coriolis tube-damping forces which are dependent on the mass flow rate of the fluid. Means are provided to respond to incipient flow-induced changes in the amplitude of vibration by changing the power input to the excitation device as required to sustain the original amplitude of vibration. The fluid mass flow rate and density are determined from the required change in power input. The invention provides stable, rapid, and accurate measurements. It does not require bending of the fluid flow

  19. A pre-anodized inlaying ultrathin carbon paste electrode for simultaneous determination of uric acid and folic acid

    International Nuclear Information System (INIS)

    Huo, Jing’e; Shangguan, Enbo; Li, Quanmin

    2013-01-01

    Graphical abstract: In 0.10 mol/L PBS (pH 6.00), oxidation reaction occurred at the PAIUCPE owing to uric acid (UA) loss electrons, while oxygen dissolved in the feed was reduced at the platinum electrode. Furthermore, the effect of electrode reaction at the platinum electrode on that of working electrode is detailedly discussed. Highlights: ► The simultaneous determination of UA and FA is achieved at the PAIUCPE. ► The effect of reaction at the Pt electrode on that of working electrode is discussed. ► The effect of pH on peak currents is detailedly explained for the first time. -- Abstract: A pre-anodized inlaying ultrathin carbon paste electrode (PAIUCPE) was prepared by electrochemical pretreatment. The scanning electron microscope (SEM) was applied to characterize the surface morphology of PAIUCPE and the performance of the electrode was characterized by cyclic voltammetry (CV). The results indicated that PAIUCPE displayed excellent electrocatalysis for the oxidation of uric acid (UA) and folic acid (FA). The separated extent between the two oxidation peaks of UA and FA was 324 mV, which was enough for the simultaneous detection. In 0.10 mol/L PBS (pH 6.00), the linear scan voltammetry (LSV) response of UA and FA increased linearly with the concentration in the range of 4.0 × 10 −6 –3.5 × 10 −4 mol/L and 3.0 × 10 −6 –2.0 × 10 −4 mol/L with the detection limits of 1.1 × 10 −7 mol/L and 1.5 × 10 −7 mol/L, respectively. It was successfully used to determine UA and FA in human urine simultaneously

  20. Simultaneous determination of nikethamide and lidocaine in human blood and cerebrospinal fluid by high performance liquid chromatography.

    Science.gov (United States)

    Chen, Lili; Liao, Linchuan; Zuo, Zhong; Yan, Youyi; Yang, Lin; Fu, Qiang; Chen, Yu; Hou, Junhong

    2007-04-11

    Nikethamide and lidocaine are often requested to be quantified simultaneously in forensic toxicological analysis. A simple reversed-phase high performance liquid chromatography (RP-HPLC) method has been developed for their simultaneous determination in human blood and cerebrospinal fluid. The method involves simple protein precipitation sample treatment followed by quantification of analytes using HPLC at 263 nm. Analytes were separated on a 5 microm Zorbax Dikema C18 column (150 mm x 4.60 mm, i.d.) with a mobile phase of 22:78 (v/v) mixture of methanol and a diethylamine-acetic acid buffer, pH 4.0. The mean recoveries were between 69.8 and 94.4% for nikethamide and between 78.9 and 97.2% for lidocaine. Limits of detection (LODs) for nikethamide and lidocaine were 0.008 and 0.16 microg/ml in plasma and 0.007 and 0.14 microg/ml in cerebrospinal fluid, respectively. The mean intra-assay and inter-assay coefficients of variation (CVs) for both analytes were less than 9.2 and 10.8%, respectively. The developed method was applied to blood sample analyses in eight forensic cases, where blood concentrations of lidocaine ranged from 0.68 to 34.4 microg/ml and nikethamide ranged from 1.25 to 106.8 microg/ml. In six cases cerebrospinal fluid analysis was requested. The values ranged from 20.3 to 185.6 microg/ml of lidocaine and 8.0 to 72.4 microg/ml of nikethamide. The method is simple and sensitive enough to be used in toxicological analysis for simultaneous determination of nikethamide and lidocaine in blood and cerebrospinal fluid.

  1. New fluorescence spectroscopic method for the simultaneous determination of alkaloids in aqueous extract of green coffee beans.

    Science.gov (United States)

    Yisak, Hagos; Redi-Abshiro, Mesfin; Chandravanshi, Bhagwan Singh

    2018-05-11

    There is no fluorescence spectroscopic method for the determination of trigonelline and theobromine in green coffee beans. Therefore, the objective of this study was to develop a new fluorescence spectroscopic method to determine the alkaloids simultaneously in the aqueous extract of green coffee beans. The calibration curves were linear in the range 2-6, 1-6, 1-5 mg/L for caffeine, theobromine and trigonelline, respectively, with R 2  ≥ 0.9987. The limit of detection and limit of quantification were 2, 6 and 7 µg/L and 40, 20 and 20 µg/L for caffeine, theobromine and trigonelline, respectively. Caffeine and trigonelline exhibited well separated fluorescence excitation spectra and therefore the two alkaloids were selectively quantified in the aqueous extract of green coffee. While theobromine showed overlapping fluorescence excitation spectra with caffeine and hence theobromine could not be determined in the aqueous extract of green coffee beans. The amount of caffeine and trigonelline in the three samples of green coffee beans were found to be 0.95-1.10 and 1.00-1.10% (w/w), respectively. The relative standard deviations (RSD ≤ 4%) of the method for the three compounds of interest were of very good. The accuracy of the developed analytical method was evaluated by spiking standard caffeine and trigonelline to green coffee beans and the average recoveries were 99 ± 2% for both the alkaloids. A fast, sensitive and reliable fluorescence method for the simultaneous determination of caffeine and trigonelline in the aqueous extract of green coffee beans was developed and validated. The developed method reflected an effective performance to the direct determination of the two alkaloids in the aqueous extract of green coffee beans.

  2. Simultaneous determination of ascorbic acid, dopamine and uric acid using high-performance screen-printed graphene electrode.

    Science.gov (United States)

    Ping, Jianfeng; Wu, Jian; Wang, Yixian; Ying, Yibin

    2012-04-15

    A disposable and sensitive screen-printed electrode using an ink containing graphene was developed. This electrode combined the advantages of graphene and the disposable characteristic of electrode, which possessed wide potential window, low background current and fast electron transfer kinetics. Compared with the electrodes made from other inks, screen-printed graphene electrode (SPGNE) showed excellent electrocatalytic activity for the oxidation of ascorbic acid (AA), dopamine (DA), and uric acid (UA). Three well-defined sharp and fully resolved anodic peaks were found at the developed electrode. Differential pulse voltammetry was used to simultaneous determination of AA, DA, and UA in their ternary mixture. In the co-existence system of these three species, the linear response ranges for the determination of AA, DA, and UA were 4.0-4500 μM, 0.5-2000 μM, and 0.8-2500 μM, respectively. The detection limits (S/N=3) were found to be 0.95 μM, 0.12 μM, and 0.20 μM for the determination of AA, DA, and UA, respectively. Furthermore, the SPGNE displayed high reproducibility and stability for these species determination. The feasibility of the developed electrode for real sample analysis was investigated. Results showed that the SPGNE could be used as a sensitive and selective sensor for simultaneous determination of AA, DA, and UA in biological samples, which may provide a promising alternative in routine sensing applications. Copyright © 2012 Elsevier B.V. All rights reserved.

  3. 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.

  4. Simultaneous determination of paracetamol and ibuprofen in pharmaceutical samples by differential pulse voltammetry using a boron-doped diamond electrode

    Energy Technology Data Exchange (ETDEWEB)

    Lima, Amanda B.; Guimaraes, Carlos F.R.C.; Verly, Rodrigo M.; Silva, Leonardo M. da [Universidade Federal dos Vales do Jequitinhonha e Mucuri (UFVJM), Diamantina, MG (Brazil). Departamento de Quimica; Torres, Livia M.F.C.; Carvalho, Junior, Alvaro D.; Santos, Wallans T. P. dos, E-mail: wallanst@ufvjm.edu.br [Universidade Federal dos Vales do Jequitinhonha e Mucuri (UFVJM), Diamantina, MG (Brazil). Departamento de Farmacia

    2014-03-15

    This work presents a simple, fast and low-cost methodology for the simultaneous determination of paracetamol (PC) and ibuprofen (IB) in pharmaceutical formulations by differential pulse voltammetry using a boron-doped diamond (BDD) electrode. A well-defined oxidation peak was observed using the BDD electrode for each analyte (0.85 V for PC and 1.72 V for IB (vs. Ag/AgCl)) in 0.1 mol L{sup -1} H{sub 2}SO{sub 4} solution containing 10% (v/v) of ethanol. Calibration curves for the simultaneous determination of PC and IB showed a linear response for both drugs in a concentration range of 20 to 400 μmol L{sup -1} (r{sup 2} = 0.999), with a detection limit of 7.1 μmol L{sup -1} for PC and 3.8 μmol L{sup -1} for IB. The addition-recovery studies in samples were about 100% and the results were validated by chromatographic methods. (author)

  5. Development and Validation of HPLC Method for the Simultaneous Determination of Five Food Additives and Caffeine in Soft Drinks

    Directory of Open Access Journals (Sweden)

    Bürge Aşçı

    2016-01-01

    Full Text Available Box-Behnken design was applied to optimize high performance liquid chromatography (HPLC conditions for the simultaneous determination of potassium sorbate, sodium benzoate, carmoisine, allura red, ponceau 4R, and caffeine in commercial soft drinks. The experimental variables chosen were pH (6.0–7.0, flow rate (1.0–1.4 mL/min, and mobile phase ratio (85–95% acetate buffer. Resolution values of all peak pairs were used as a response. Stationary phase was Inertsil OctaDecylSilane- (ODS- 3V reverse phase column (250 × 4.6 mm, 5 μm dimensions. The detection was performed at 230 nm. Optimal values were found 6.0 pH, 1.0 mL/min flow rate, and 95% mobile phase ratio for the method which was validated by calculating the linearity (r2>0.9962, accuracy (recoveries ≥ 95.75%, precision (intraday variation ≤ 1.923%, interday variation ≤ 1.950%, limits of detection (LODs, and limits of quantification (LOQs parameters. LODs and LOQs for analytes were in the range of 0.10–0.19 μg/mL and 0.33–0.63 μg/mL, respectively. The proposed method was applied successfully for the simultaneous determination of the mixtures of five food additives and caffeine in soft drinks.

  6. Development and validation of an HPLC method for simultaneous determination of trimethoprim and sulfamethoxazole in human plasma.

    Science.gov (United States)

    Sayar, Esin; Sahin, Selma; Cevheroglu, Semsettin; Hincal, A Atilla

    2010-09-01

    The combination of trimethoprim (TMP) and sulfamethoxazole (SMX) is used in the treatment of many common infections such as urinary, respiratory and gastrointestinal tract infections. The aim of this study was to determine TMP and SMX simultaneously in human plasma samples by high performance liquid chromatography (HPLC) using antipyrine as the internal standard. Separation of the compounds was achieved on a reverse-phase C8 column packed with 5 microm dimethyl octadecylsilyl bonded amorphous silica (4.6 mm x 250 mm) column using a mobile phase consisted of potassium hydrogen phosphate, acetonitrile, methanol and water adjusted to pH 6.2. The mobile phase was delivered at a flow rate of 1 mL min- and the effluent was monitored using Max plot technique at 25 derees C. Retention times were 5 min for TMP, 7 min for antipyrine and 9 min for SMX. Quantitation limits were 10 ng mL(-1) for TMP and 50 ng mL(-1) for SMX. Our findings indicated that the developed HPLC method was precise, accurate, specific and sensitive for simultaneous determination of TMP and SMX. Proposed HPLC method was successfully applied for the analysis of TMP and SMX in human plasma after oral administration of a co-trimoxazole tablet to human volunteers.

  7. Simultaneous determination of Cr, Ga, In and V in soil and water samples by tungsten coil atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Donati, George L.; Kron, Benjamin E. [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States); Jones, Bradley T. [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States)], E-mail: jonesbt@wfu.edu

    2009-06-15

    Tungsten coil atomic emission spectrometry is employed for the simultaneous determination of Cr, Ga, In, and V. Both V and In are detected by this technique for the first time. The atomizer is a simple, inexpensive tungsten filament extracted from a mass-produced, commercially-available 150 W, 15 V microscope bulb. A 25 {mu}l sample aliquot is placed directly on the coil and a small constant-current power source is used to carefully dry, ash and atomize the sample. Analytical signals are detected with a Czerny-Turner spectrograph and a charge coupled device detector. Multiple emission lines from all 4 elements are monitored simultaneously in a 54 nm spectral window. Concentration limits of detection are in the {mu}g l{sup - 1} range for all elements, and the absolute limits of detection are 0.2, 2, 0.5, and 10 ng for Cr, Ga, In, and V, respectively. Even lower values may be obtained by combining the signals for the multiple emission lines of a single element. The method precision is typically better than 5.0% relative standard deviation, and sometimes as good as 0.95% (Ga). Standard reference materials of soil and water are used to check the method accuracy. After a simple acid extraction, the values determined by the method presented no significant difference from the reported values at the 95% confidence level.

  8. A novel paper-based assay for the simultaneous determination of Rh typing and forward and reverse ABO blood groups.

    Science.gov (United States)

    Noiphung, Julaluk; Talalak, Kwanrutai; Hongwarittorrn, Irin; Pupinyo, Naricha; Thirabowonkitphithan, Pannawich; Laiwattanapaisal, Wanida

    2015-05-15

    We propose a new, paper-based analytical device (PAD) for blood typing that allows for the simultaneous determination of ABO and Rh blood groups on the same device. The device was successfully fabricated by using a combination of wax printing and wax dipping methods. A 1:2 blood dilution was used for forward grouping, whereas whole blood could be used for reverse grouping. A 30% cell suspension of A-cells or B-cells was used for haemagglutination on the reverse grouping side. The total assay time was 10 min. The ratio between the distance of red blood cell movement and plasma separation is the criterion for agglutination and indicates the presence of the corresponding antigen or antibody. The proposed PAD has excellent reproducibility in that the same blood groups, namely A, AB, and O, were reported by using different PADs that were fabricated on the same day (n=10). The accuracy for detecting blood group A (n=12), B (n=13), AB (n=9), O (n=14), and Rh (n=48) typing were 92%, 85%, 89%, 93%, and 96%, respectively, in comparison with the conventional slide test method. The haematocrit of the sample affects the accuracy of the results, and appropriate dilution is suggested before typing. In conclusion, this study proposes a novel method that is straightforward, time-saving, and inexpensive for the simultaneous determination of ABO and Rh blood groups, which is promising for use in developing countries. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. A binderless, covalently bulk modified electrochemical sensor: Application to simultaneous determination of lead and cadmium at trace level

    Energy Technology Data Exchange (ETDEWEB)

    Gunigollahalli Kempegowda, Raghu [Department of Studies in Chemistry, Bangalore University, Central College Campus, Bangalore 560001 (India); Malingappa, Pandurangappa, E-mail: mprangachem@gmail.com [Department of Studies in Chemistry, Bangalore University, Central College Campus, Bangalore 560001 (India)

    2012-05-30

    Highlights: Black-Right-Pointing-Pointer Proposed sensor is a new type of binderless covalent bulk modified electrode. Black-Right-Pointing-Pointer Surface can be easily renewed by simple mechanical polishing using emery sheets. Black-Right-Pointing-Pointer Free from modifier leaching during electrochemical measurements. Black-Right-Pointing-Pointer Provides long term storage stability with good reproducibility. Black-Right-Pointing-Pointer Nanomolar level detection limit achieved with selectivity. - Abstract: A new type of covalent binderless bulk modified electrode has been fabricated and used in the simultaneous determination of lead and cadmium ions at nanomolar level. The modification of graphitic carbon with 4-amino salicylic acid was carried out under microwave irradiation through the amide bond formation. The electrochemical behavior of the fabricated electrode has been carried out to decipher the interacting ability of the functional moieties present on the modifier molecules toward the simultaneous determination of Pb{sup 2+} and Cd{sup 2+} ions using cyclic and differential pulse anodic stripping voltammetry. The possible mode of interaction of functional groups with metal ions is proposed based on the pKa values of the modifier functionalities present on the surface of graphitic carbon particles. The analytical utility of the proposed sensor has been validated by measuring the lead and cadmium content from pretreated waste water samples of lead acid batteries.

  10. High performance liquid chromatography for simultaneous determination of xipamide, triamterene and hydrochlorothiazide in bulk drug samples and dosage forms.

    Science.gov (United States)

    Abd El-Hay, Soad S; Hashem, Hisham; Gouda, Ayman A

    2016-03-01

    A novel, simple and robust high-performance liquid chromatography (HPLC) method was developed and validated for simultaneous determination of xipamide (XIP), triamterene (TRI) and hydrochlorothiazide (HCT) in their bulk powders and dosage forms. Chromatographic separation was carried out in less than two minutes. The separation was performed on a RP C-18 stationary phase with an isocratic elution system consisting of 0.03 mol L(-1) orthophosphoric acid (pH 2.3) and acetonitrile (ACN) as the mobile phase in the ratio of 50:50, at 2.0 mL min(-1) flow rate at room temperature. Detection was performed at 220 nm. Validation was performed concerning system suitability, limits of detection and quantitation, accuracy, precision, linearity and robustness. Calibration curves were rectilinear over the range of 0.195-100 μg mL(-1) for all the drugs studied. Recovery values were 99.9, 99.6 and 99.0 % for XIP, TRI and HCT, respectively. The method was applied to simultaneous determination of the studied analytes in their pharmaceutical dosage forms.

  11. Simultaneous determination of paracetamol and ibuprofen in pharmaceutical samples by differential pulse voltammetry using a boron-doped diamond electrode

    International Nuclear Information System (INIS)

    Lima, Amanda B.; Guimaraes, Carlos F.R.C.; Verly, Rodrigo M.; Silva, Leonardo M. da; Torres, Livia M.F.C.; Carvalho Junior, Alvaro D.; Santos, Wallans T. P. dos

    2014-01-01

    This work presents a simple, fast and low-cost methodology for the simultaneous determination of paracetamol (PC) and ibuprofen (IB) in pharmaceutical formulations by differential pulse voltammetry using a boron-doped diamond (BDD) electrode. A well-defined oxidation peak was observed using the BDD electrode for each analyte (0.85 V for PC and 1.72 V for IB (vs. Ag/AgCl)) in 0.1 mol L -1 H 2 SO 4 solution containing 10% (v/v) of ethanol. Calibration curves for the simultaneous determination of PC and IB showed a linear response for both drugs in a concentration range of 20 to 400 μmol L -1 (r 2 = 0.999), with a detection limit of 7.1 μmol L -1 for PC and 3.8 μmol L -1 for IB. The addition-recovery studies in samples were about 100% and the results were validated by chromatographic methods. (author)

  12. Screen-printed electrodes modified with carbon nanotubes or graphene for simultaneous determination of melatonin and serotonin

    International Nuclear Information System (INIS)

    Gomez, Federico José Vicente; Martín, Aída; Escarpa, Alberto; Silva, María Fernanda

    2015-01-01

    Single-walled carbon nanotubes (SWCNT), multi-walled carbon nanotubes (MWCNT) and graphene have been tested as carbon allotropes for the modification of carbon screen-printed electrodes (CSPEs) to simultaneously determine melatonin (MT) and serotonin (5-HT). Two groups of CSPEs, both 4 mm in diameter, were explored: The first includes commercial SWCNT, MWCNT and graphene, the second includes SWCNT, MWCNT, graphene oxide nanoribbons and reduced nanoribbons that were drop casted on the electrodes. The carbon nanomaterials enhanced the electroactive area in the following order: CSPE simultaneous determination of 5-HT and MT at the working potentials of +50 mV and +390 mV (vs. Ag), respectively. The use of carbon nanomaterials, in particular of graphene oxide nanoribbons on CSPEs, represents an excellent and disposable tool for sensing the two target molecules in even small sample volumes. Figures of merit for MT and 5-HT include (a) detection limit of 1.1 and 0.4 μM for MT and 5-HT, respectively; (b) an inter-electrode reproducibility with RSD ≤ 8 %; (c) 120 s response time, and (d) recoveries (in case of spiked samples) ranging from 94 to 103 % (with an RSD < 1 %). (author)

  13. Simultaneous DPV determination of morphine and codeine using dsDNA modified screen printed electrode strips coupled with electromembrane extraction

    Directory of Open Access Journals (Sweden)

    Rouhollah Feizbakhsh

    2016-01-01

    Full Text Available In this work a sensitive electrochemical sensor for simultaneous determination of morphine and codeine constructed by application of disposable screen printed carbon electrode strips (SPCE modified by double strand (ds calf thymus DNA. According to the results of the modified SPCE strips and experimented parameters, we observed a considerable shift between potentials of morphine and codeine current peaks. Related to these observed shifts, we studied on the effect of the concentration of modifier and pH value on the anodic oxidation pattern of morphine and codeine in the case of optimize the method to get better signals with maximum potential distance. Also to boosting the LODs of this electroanalytical method coupled with an electro-membrane preconcentration (EME step. The calibration curve which was plotted by the variation of differential pulse voltammetry (DPV currents as a function of different morphine and codeine concentration were linear within the range of 0.7– 40 µM and 2.3- 40 µM for morphine and codeine respectively. Also the limits of detection were 0.07 µM and 0.23 µM, respectively. Finally, the proposed method was able to determine morphine and codeine simultaneously and effectively in urinary real samples

  14. Simultaneous determination of 14N and 15N isotopes in opium by proton induced γ-ray emission technique

    International Nuclear Information System (INIS)

    Pritty Rao; Reddy, G.L.N.; Vikram Kumar, S.; Ramana, J.V.; Raju, V.S.; Sanjiv Kumar

    2012-01-01

    The paper describes the simultaneous determination of 14 N and 15 N isotopes in opium by proton induced γ-ray emission (PIGE) technique. The isotopic ratio of 14 N and 15 N is a useful parameter for assigning provenance of (seized) illicit drugs. The measurement, non-destructive in nature, is performed on pellets made up of opium powders and is based on the prompt detection of 2.313 and 4.4 MeV γ-rays emanating from 14 N(p,p'γ) 14 N and 15 N(p,αγ) 12 C nuclear reactions respectively, induced simultaneously by 3.6-3.8 MeV proton beam. Positive as well as negative deviations from the natural isotopic abundance (99.63:0.37) were observed in the samples. The precision of the measurements is about 4%. The methodology provides an easy and rapid approach to determine the isotopic ratio of 14 N and 15 N and has been used for the first time in the analysis of opium. (author)

  15. Simultaneous square-wave voltammetric determination of aspartame and cyclamate using a boron-doped diamond electrode.

    Science.gov (United States)

    Medeiros, Roberta Antigo; de Carvalho, Adriana Evaristo; Rocha-Filho, Romeu C; Fatibello-Filho, Orlando

    2008-07-30

    A simple and highly selective electrochemical method was developed for the simultaneous determination of aspartame and cyclamate in dietary products at a boron-doped diamond (BDD) electrode. In square-wave voltammetric (SWV) measurements, the BDD electrode was able to separate the oxidation peak potentials of aspartame and cyclamate present in binary mixtures by about 400 mV. The detection limit for aspartame in the presence of 3.0x10(-4) mol L(-1) cyclamate was 4.7x10(-7) mol L(-1), and the detection limit for cyclamate in the presence of 1.0x10(-4) mol L(-1) aspartame was 4.2x10(-6) mol L(-1). When simultaneously changing the concentration of both aspartame and cyclamate in a 0.5 mol L(-1) sulfuric acid solution, the corresponding detection limits were 3.5x10(-7) and 4.5x10(-6) mol L(-1), respectively. The relative standard deviation (R.S.D.) obtained was 1.3% for the 1.0x10(-4) mol L(-1) aspartame solution (n=5) and 1.1% for the 3.0x10(-3) mol L(-1) cyclamate solution. The proposed method was successfully applied in the determination of aspartame in several dietary products with results similar to those obtained using an HPLC method at 95% confidence level.

  16. Simultaneous Determination of Cyclosporine A, Tacrolimus, Sirolimus, and Everolimus in Whole-Blood Samples by LC-MS/MS

    Directory of Open Access Journals (Sweden)

    Mustafa Karapirli

    2012-01-01

    Full Text Available Objectives. Cyclosporine A (CyA, tacrolimus (TRL, sirolimus (SIR, and everolimus (RAD are immunosuppressive drugs frequently used in organ transplantation. Our aim was to confirm a robust sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS method for determination of CyA, TRL, SIR, and RAD in whole-blood samples. Materials and Methods. We used an integrated online solid-phase extraction-LC-MS/MS system and atmospheric pressure ionization tandem mass spectrometry (API-MS/MS in the multiple reaction monitoring (MRM detection mode. CyA, TRL, SIR, and RAD were simultaneously analyzed in whole blood treated with precipitation reagent taken from transplant patients. Results. System performance parameters were suitable for using this method as a high-throughput technique in clinical practice. The high concentration of one analyte in the sample did not affect the concentration of other analytes. Total analytical time was 2.5 min, and retention times of all analytes were shorter than 2 minutes. Conclusion. This LC-MS/MS method can be preferable for therapeutic drug monitoring of these immunosuppressive drugs (CyA, TRL, SRL, and RAD in whole blood. Sample preparation was too short and simple in this method, and it permits robust, rapid, sensitive, selective, and simultaneous determination of these drugs.

  17. Graphitic carbon nitride nanosheets doped graphene oxide for electrochemical simultaneous determination of ascorbic acid, dopamine and uric acid

    International Nuclear Information System (INIS)

    Zhang, Hanqiang; Huang, Qitong; Huang, Yihong; Li, Feiming; Zhang, Wuxiang; Wei, Chan; Chen, Jianhua; Dai, Pingwang; Huang, Lizhang; Huang, Zhouyi; Kang, Lianping; Hu, Shirong; Hao, Aiyou

    2014-01-01

    Graphical abstract: Schematic drawing of electrochemical oxidize AA, DA and UA on graphitic carbon nitride nanosheets-graphene oxide composite modified electrode. - Highlights: • Synthesize g-C 3 N 4 , GO and CNNS-GO composite. • CNNS-GO composite was the first time for simultaneous determination of AA, DA and UA. • CNNS-GO/GCE displays fantastic selectivity and sensitivity for AA, DA and UA. • CNNS-GO/GCE was applied to detect real sample with satisfactory results. - Abstract: Graphitic carbon nitride nanosheets with a graphite-like structure have strong covalent bonds between carbon and nitride atoms, and nitrogen atoms in the carbon architecture can accelerate the electron transfer and enhance electrical properties effectually. The graphitic carbon nitride nanosheets-graphene oxide composite was synthesized. And the electrochemical performance of the composite was investigated by cyclic voltammetry and differential pulse voltammetry ulteriorly. Due to the synergistic effects of layer-by-layer structures by π-π stacking or charge-transfer interactions, graphitic carbon nitride nanosheets-graphene oxide composite can improved conductivity, electro-catalytic and selective oxidation performance. The proposed graphitic carbon nitride nanosheets-graphene oxide composite modified electrode was employed for simultaneous determination of ascorbic acid, dopamine and uric acid in their mixture solution, it exhibited distinguished sensitivity, wide linear range and low detection limit. Moreover, the modified electrode was applied to detect urine and dopamine injection sample, and then the samples were spiked with certain concentration of three substances with satisfactory recovery results

  18. Simultaneous determination of moxifloxacin and cefixime by first and ratio first derivative ultraviolet spectrophotometry

    Directory of Open Access Journals (Sweden)

    Attimarad Mahesh

    2012-09-01

    Full Text Available Abstract Background The new combination of moxifloxacin HCl and cefixime trihydrate is approved for the treatment of lower respiratory tract infections in adults. At initial formulation development and screening stage a fast and reliable method for the dissolution and release testing of moxifloxacin and cefixime were highly desirable. The zero order overlaid UV spectra of moxifloxacin and cefixime showed >90% overlapping. Hence, simple, accurate precise and validated two derivative spectrophotometric methods have been developed for the determination of moxifloxacin and cefixime. Methods In the first derivative spectrophotometric method varying concentration of moxifloxacin and cefixime were prepared and scanned in the range of 200 to 400 nm and first derivative spectra were calculated (n = 1. The zero crossing wavelengths 287 nm and 317.9 nm were selected for determination of moxifloxacin and cefixime, respectively. In the second method the first derivative of ratio spectra was calculated and used for the determination of moxifloxacin and cefixime by measuring the peak intensity at 359.3 nm and 269.6 nm respectively. Results Calibration graphs were established in the range of 1–16 μg /mL and 1–15 μg /mL for both the drugs by first and ratio first derivative spectroscopic methods respectively with good correlation coefficients. Average accuracy of assay of moxifloxacin and cefixime were found to be 100.68% and 98 93%, respectively. Relative standard deviations of both inter and intraday assays were less than 1.8%. Moreover, recovery of moxifloxacin and cefixime was more than 98.7% and 99.1%, respectively. Conclusions The described derivative spectrophotometric methods are simple, rapid, accurate, precise and excellent alternative to sophisticated chromatographic techniques. Hence, the proposed methods can be used for the quality control of the cited drugs and can be extended for routine analysis of the drugs in formulations.

  19. Rapid and simultaneous determination of Strontium-89 and Strontium-90 in seawater.

    Science.gov (United States)

    Tayeb, Michelle; Dai, Xiongxin; Sdraulig, Sandra

    2016-03-01

    A rapid method has been developed for the direct determination of radiostrontium ((89)Sr and (90)Sr) released in seawater in the early phase of an accident. The method employs a fast and effective pre-concentration of radiostrontium by Sr-Ca co-precipitation followed by separation of radiostrontium using extraction chromatography technique. Radiostrontium is effectively separated in the presence of excessive dominant salts of seawater. Čerenkov and liquid scintillation assay (LSA) techniques are used to determine (89)Sr and (90)Sr. Sample preparation time is approximately 4 h for a set of 10 samples. The method was validated using spiked seawater samples at various activity ratios of (89)Sr:(90)Sr ranging from 1:10 to 9:1. The mean chemical recovery of Sr was 85 ± 3%. (90)Sr showed variable relative bias which enhanced with increasing ratio of (89)Sr:(90)Sr and was in the range ± 21%. The highest biases of (90)Sr determination were due to lower activity concentrations of (90)Sr and are regarded as acceptable in emergency situations with elevated levels of radiostrontium in the sample. The minimum detectable concentration (MDC) of (90)Sr and (89)Sr varied at different (89)Sr:(90)Sr ratios. For 0.1 L seawater and 15 min counting time on a low background Hidex liquid scintillation counter (LSC), the MDC of (90)Sr was in the range of 1.7-3.5 Bq L(-1) and MDC of (89)Sr was in the range 0.5-2.4 Bq L(-1). Copyright © 2016 Elsevier Ltd. All rights reserved.

  20. Determinants of the ZAR/USD exchange rate and policy implications: A simultaneous-equation model

    Directory of Open Access Journals (Sweden)

    Yu Hsing

    2016-12-01

    Full Text Available This paper examines the determinants of the South African rand/US dollar (ZAR/USD exchange rate based on demand and supply analysis. Applying the EGARCH method, the paper finds that the ZAR/USD exchange rate is positively associated with the South African government bond yield, US real GDP, the US stock price and the South African inflation rate and negatively influenced by the 10-year US government bond yield, South African real GDP, the South African stock price, and the US inflation rate. The adoption of a free floating exchange rate regime has reduced the value of the rand vs. the US dollar.

  1. Simultaneous determination of hydroxylamine and phenol using a nanostructure-based electrochemical sensor.

    Science.gov (United States)

    Moghaddam, Hadi Mahmoudi; Beitollahi, Hadi; Tajik, Somayeh; Malakootian, Mohammad; Maleh, Hassan Karimi

    2014-11-01

    The electrochemical oxidation of hydroxylamine on the surface of a carbon paste electrode modified with carbon nanotubes and 2,7-bis(ferrocenyl ethyl)fluoren-9-one is studied. The electrochemical response characteristics of the modified electrode toward hydroxylamine and phenol were investigated. The results showed an efficient catalytic activity of the electrode for the electro-oxidation of hydroxylamine, which leads to lowering its overpotential. The modified electrode exhibits an efficient electron-mediating behavior together with well-separated oxidation peaks for hydroxylamine and phenol. Also, the modified electrode was used for determination of hydroxylamine and phenol in some real samples.

  2. Simultaneous determination of stable carbon, oxygen, and hydrogen isotopes in cellulose.

    Science.gov (United States)

    Loader, N J; Street-Perrott, F A; Daley, T J; Hughes, P D M; Kimak, A; Levanič, T; Mallon, G; Mauquoy, D; Robertson, I; Roland, T P; van Bellen, S; Ziehmer, M M; Leuenberger, M

    2015-01-06

    A technological development is described through which the stable carbon-, oxygen-, and nonexchangeable hydrogen-isotopic ratios (δ(13)C, δ(18)O, δ(2)H) are determined on a single carbohydrate (cellulose) sample with precision equivalent to conventional techniques (δ(13)C 0.15‰, δ(18)O 0.30‰, δ(2)H 3.0‰). This triple-isotope approach offers significant new research opportunities, most notably in physiology and medicine, isotope biogeochemistry, forensic science, and palaeoclimatology, when isotopic analysis of a common sample is desirable or when sample material is limited.

  3. Simultaneous determination of twelve trace elements in estuarine and sea water using pre-irradiation chromatography

    International Nuclear Information System (INIS)

    Greenberg, R.R.; Kingston, H.M.

    1982-01-01

    A procedure is described for the preconcentration of 100 m of estuarine and seawater into a solid sample using Chelex-100 resin. This solid sample weighs less than half a gram and contains the transition metals and many other elements of interest, but is essentially free from the alkali metals, the alkaline earth metals, and the halogens. The concentrations of Co, Cr, Cu, Fe, Mn, Mo, Ni, Sc, Th, U, V and Zn have been determined in seawater when this procedure was coupled to neutron activation analysis. (author)

  4. Simultaneous determination of sulphaquinoxaline and amprolium in veterinary mixture by HPLC and first derivative ultraviolet spectrophotometry

    International Nuclear Information System (INIS)

    El-Sattar, Osama Abd

    2002-01-01

    Two simple and reliable methods are described for the determination of sulphaquinoxaline (SQX) and amprolium (AMP) combined in veterinary powder. The first method depends on high performance liquid chromatography on a reversed phase column (Bondapak-C18) using mobile phase consisting of acetonitrile-methanol-water-phosphoric acid (30: 5: 55: 0.7, by volumes) at a flow rate of 1 ml min with UV detection at 254 nm. The detection limits were 0.2 ug ml and 0.35 ug ml and linearity ranges were 2-20 ug ml and 4-40ug ml for SQX and AMP, respectively. The second one deals with the first derivative (D) spectrophotometry with zero-crossing measurement at 253 nm and 226 nm for SQX and AMP respectively. The detection limits were 0.3 ug ml and linearity ranges were 1-18 ug ml and 4-32 ug-ml for SQX and AMP respectively. The proposed procedures were successfully applied to the determination of these drugs in laboratory prepared mixtures with mean percentage recovery ranged from 98.50 to 99.75 and in commercial preparation ranged from 103.85 to 104.85. (author)

  5. Vapor permeation-stepwise injection simultaneous determination of methanol and ethanol in biodiesel with voltammetric detection.

    Science.gov (United States)

    Shishov, Andrey; Penkova, Anastasia; Zabrodin, Andrey; Nikolaev, Konstantin; Dmitrenko, Maria; Ermakov, Sergey; Bulatov, Andrey

    2016-02-01

    A novel vapor permeation-stepwise injection (VP-SWI) method for the determination of methanol and ethanol in biodiesel samples is discussed. In the current study, stepwise injection analysis was successfully combined with voltammetric detection and vapor permeation. This method is based on the separation of methanol and ethanol from a sample using a vapor permeation module (VPM) with a selective polymer membrane based on poly(phenylene isophtalamide) (PA) containing high amounts of a residual solvent. After the evaporation into the headspace of the VPM, methanol and ethanol were transported, by gas bubbling, through a PA membrane to a mixing chamber equipped with a voltammetric detector. Ethanol was selectively detected at +0.19 V, and both compounds were detected at +1.20 V. Current subtractions (using a correction factor) were used for the selective determination of methanol. A linear range between 0.05 and 0.5% (m/m) was established for each analyte. The limits of detection were estimated at 0.02% (m/m) for ethanol and methanol. The sample throughput was 5 samples h(-1). The method was successfully applied to the analysis of biodiesel samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  6. [Simultaneous determination of two saponnins in anemarrhenae rhizoma by HPLC-ELSD].

    Science.gov (United States)

    Chen, Qianliang; Sun, Xiaoming; Wang, Wenquan; Ma, Changhua

    2011-02-01

    To establish an HPLC-ELSD method for determination of Anemarsaponin C and Anemarsaponin A III in Anemarrhenae Rhizoma. Kromasil C18 column(4.6 mm x 250 mm, 5 microm) was used as stationary phase. Mobile phase was methanol-water gradient with the flow rate of 1 mL x min(-1); the temperature of the drift tube and evaporation was 50 degrees C and 70 degrees C respectively. The gas pressure was 1.03 x 10(5) Pa. There are good linearity in the range 0.310-3.10 microg of anemarsaponin C (lgA = 1.254 2lgM + 5.734 7, r = 0.999 5) and in the range 0.323-3.23 microg (lgA = 1.328 41gM + 5. 937, r = 0.999 6) of anemarsaponin A III. The average recovery of anemarsaponin C and anemarsaponin A III was 98.1% with RSD 2.1% and 97.3% with RSD 1.5% (n = 6) respectively. The method is rapid and accurate. It is suitable for quality control of Anemarrhenae Rhizoma. The result of determination reveals that the quality of Anemarrhenae Rhizoma from different places of north China are of notable difference.

  7. Chemometric methods for the simultaneous determination of some water-soluble vitamins.

    Science.gov (United States)

    Mohamed, Abdel-Maaboud I; Mohamed, Horria A; Mohamed, Niveen A; El-Zahery, Marwa R

    2011-01-01

    Two spectrophotometric methods, derivative and multivariate methods, were applied for the determination of binary, ternary, and quaternary mixtures of the water-soluble vitamins thiamine HCI (I), pyridoxine HCI (II), riboflavin (III), and cyanocobalamin (IV). The first method is divided into first derivative and first derivative of ratio spectra methods, and the second into classical least squares and principal components regression methods. Both methods are based on spectrophotometric measurements of the studied vitamins in 0.1 M HCl solution in the range of 200-500 nm for all components. The linear calibration curves were obtained from 2.5-90 microg/mL, and the correlation coefficients ranged from 0.9991 to 0.9999. These methods were applied for the analysis of the following mixtures: (I) and (II); (I), (II), and (III); (I), (II), and (IV); and (I), (II), (III), and (IV). The described methods were successfully applied for the determination of vitamin combinations in synthetic mixtures and dosage forms from different manufacturers. The recovery ranged from 96.1 +/- 1.2 to 101.2 +/- 1.0% for derivative methods and 97.0 +/- 0.5 to 101.9 +/- 1.3% for multivariate methods. The results of the developed methods were compared with those of reported methods, and gave good accuracy and precision.

  8. Simultaneous separation and determination of four uncaria alkaloids by capillary electrophoresis using dual cyclodextrin system.

    Science.gov (United States)

    Li, Lou; Xu, Liying; Chen, Meng; Zhang, Guangbin; Zhang, Hongfen; Chen, Anjia

    2017-07-15

    The purpose of this study was to develop a simple, quick and precise capillary zone electrophoresis method (CZE) for the separation and determination of uncaria alkaloids using dual cyclodextrins as additives for the separation. The four analytes were baseline separated within 15min at the applied voltage of 15kV with a running buffer (pH 5.7) consisting of 40.0mM phosphate buffer, 161.7mM 2-hydroxypropyl-β-cyclodextrin (HP-β-CD) and 2.21mM mono-(6-ethylenediamine-6-deoxy)-β-cyclodextrin (ED-β-CD). Under the optimum conditions, a good linearity was achieved with correlation coefficients from 0.9989 to 0.9992. The detection limits and the quantitation limits ranged from 0.63 to 0.98μg/mL and from 2.08 to 3.28μg/mL, respectively. Excellent accuracy and precision were obtained. Recoveries of the analytes varied from 97.1 to 103.2%. This method was suitable for the quantitative determination of these alkaloids in the stem with hook of Uncaria rhynchophylla and the formulations of Uncaria rhynchophylla. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. [Simultaneous determination of aspartame and alitame in jellies and preserved fruits by HPLC].

    Science.gov (United States)

    Jiang, Dingguo; Fang, Congrong; Yang, Dajin

    2012-05-01

    To establish a determination method for aspartame and alitame in jellies and preserved fruits. Aspartame and alitame in jellies were extracted with 80% methanol at 70 degrees C. Preserved fruits were homogenized with water and then were extracted with 50% methanol. A chromatographic column Zorbax SB-C18 was used; the mobile phase was methanol/water (40 + 60, volume ratio), and a diode array detector was used for the detection at wavelength 200 nm. The limits of quantification of aspartame and alitame were both 8 mg/kg for jellies and both 20 mg/kg for preserved fruits; the calibration curves were linear in the range of tested concentration. The correlation coefficients were better than 0.9996. The average recovery rates were in the range of 98.1% -101.2%, the relative standard deviations were 2.21% - 4.10%. The method is simple, practical, accurate, reliable and successful in the determination of aspartame and alitame in jellies and preserved fruits from various brands on markets.

  10. Method of simultaneous continuous determination of transfer rates of iron and chromium into solution during Fe-Cr alloys dissolution

    International Nuclear Information System (INIS)

    Shirinov, T.I.; Florianovich, G.M.; Skuratnik, Ya.B.

    1978-01-01

    Radiometry method of simultaneous continuous registration of transfer rates of iron and chromium into solution from Fe-Cr alloys with various composition has been developed. Using gamma-spectrometer components of Fe-Cr alloys can be determined with high sensitivity in separate samples according to Fe 59 and Cr 51 radioactive labels, obtained by neutron activation. The above method is applied to estimate Fe and Cr transfer rates into H 2 SO 4 solution at the temperature of 50 deg from Fe - 28% Cr alloy during its active dissolution. It is established, that beginning with some seconds of alloy and solution contact, its components transfer into the solution in the same composition, as in the alloy. The method enables to determine Fe with the accuracy of up to 5% and Cr with that of up to 10%

  11. Validation of HPLC method for the simultaneous and quantitative determination of 12 UV-filters in cosmetics.

    Science.gov (United States)

    Nyeborg, M; Pissavini, M; Lemasson, Y; Doucet, O

    2010-02-01

    The aim of the study was the validation of a high-performance liquid chromatography (HPLC) method for the simultaneous and quantitative determination of twelve commonly used organic UV-filters (phenylbenzimidazole sulfonic acid, benzophenone-3, isoamyl p-methoxycinnamate, diethylamino hydroxybenzoyl hexyl benzoate, octocrylene, ethylhexyl methoxycinnamate, ethylhexyl salicylate, butyl methoxydibenzoylmethane, diethylhexyl butamido triazone, ethylhexyl triazone, methylene bis-benzotriazolyl tetramethylbutylphenol and bis-ethylhexyloxyphenol methoxyphenyl triazine) contained in suncare products. The separation and quantitative determination was performed in <30 min, using a Symmetry Shield(R) C18 (5 microm) column from Waters and a mobile phase (gradient mode) consisting of ethanol and acidified water. UV measurements were carried out at multi-wavelengths, according to the absorption of the analytes.

  12. A novel technique for the simultaneous determination of 210Pb and 210Po using a crown ether

    International Nuclear Information System (INIS)

    Vajda, N.; LaRosa, J.; Zeisler, R.; Danesi, P.; Kis-Benedek, Gy.

    1997-01-01

    A simple radiochemical procedure has been developed to separate lead and polonium simultaneously from different environmental and biological materials. After adding 208 Po tracer and lead carrier, samples are decomposed using mineral acids. Lead and polonium are selectively retained from 2M HCl solution by the bis-4,4'(5')-t-butyl-cyclohexano-18-crown-6-ether; polonium is stripped with 6 M HNO 3 while lead is stripped with 6 M HCL solution. A polonium source is prepared by spontaneous deposition onto a silver disk. The activity concentration of 210 Po is determined by isotope dilution alpha spectrometry. Lead is precipitated as oxalate; the chemical recovery is determined by gravimetry. The activity concentration of 210 Pb is calculated from the liquid scintillation spectrum. (author)

  13. Simultaneous determination of aerosol optical thickness and water-leaving radiance from multispectral measurements in coastal waters

    Science.gov (United States)

    Shi, Chong; Nakajima, Teruyuki

    2018-03-01

    Retrieval of aerosol optical properties and water-leaving radiance over ocean is challenging since the latter mostly accounts for ˜ 10 % of the satellite-observed signal and can be easily influenced by the atmospheric scattering. Such an effort would be more difficult in turbid coastal waters due to the existence of optically complex oceanic substances or high aerosol loading. In an effort to solve such problems, we present an optimization approach for the simultaneous determination of aerosol optical thickness (AOT) and normalized water-leaving radiance (nLw) from multispectral satellite measurements. In this algorithm, a coupled atmosphere-ocean radiative transfer model combined with a comprehensive bio-optical oceanic module is used to jointly simulate the satellite-observed reflectance at the top of atmosphere and water-leaving radiance just above the ocean surface. Then, an optimal estimation method is adopted to retrieve AOT and nLw iteratively. The algorithm is validated using Aerosol Robotic Network - Ocean Color (AERONET-OC) products selected from eight OC sites distributed over different waters, consisting of observations that covered glint and non-glint conditions from the Moderate Resolution Imaging Spectroradiometer (MODIS) instrument. Results show a good consistency between retrieved and in situ measurements at each site. It is demonstrated that more accurate AOTs are determined based on the simultaneous retrieval method, particularly in shorter wavelengths and sunglint conditions, where the averaged percentage difference (APD) of retrieved AOT is generally reduced by approximate 10 % in visible bands compared with those derived from the standard atmospheric correction (AC) scheme, since all the spectral measurements can be used jointly to increase the information content in the inversion of AOT, and the wind speed is also simultaneously retrieved to compensate the specular reflectance error estimated from the rough ocean surface model. For the

  14. Simultaneous Determination of Lactulose and Lactose in Conserved Milk by HPLC-RID

    Directory of Open Access Journals (Sweden)

    Michelle Fernandes Silveira

    2015-01-01

    Full Text Available Heat treatment is applied to dairy products to ensure microbiological quality and increase the shelf life. However, a suitable control of this process is necessary to guarantee nutritional and sensory quality. The aim of this study is to adapt the high performance liquid chromatography (HPLC method for determination of lactulose and lactose content in commercial samples of UHT and sweetened condensed milk. The HPLC method used showed a good resolution of the analytes evaluated. The analyzed UHT milk samples presented levels for lactulose in accordance with the limit recommended by the International Dairy Federation. There was no significant variation in lactulose concentration for sweetened condensed milk samples. However, one sweetened condensed milk sample showed lactose level lower than the established values (10–12%.

  15. H-Point Standard Addition Method for Simultaneous Determination of Eosin and Erytrosine

    Directory of Open Access Journals (Sweden)

    Amandeep Kaur

    2011-01-01

    Full Text Available A new, simple, sensitive and selective H-point standard addition method (HPSAM has been developed for resolving binary mixture of food colorants eosin and erythrosine, which show overlapped spectra. The method is based on the complexation of food dyes eosin and erythrosine with Fe(III complexing reagent at pH 5.5 and solubilizing complexes in triton x-100 micellar media. Absorbances at the two pairs of wavelengths, 540 and 550 nm (when eosin acts as analyte or 518 and 542 nm (when erythrosine act as analyte were monitored. This method has satisfactorily been applied for the determination of eosin and erythrosine dyes in synthetic mixtures and commercial products.

  16. SIMULTANEOUS DETERMINATION OF PARACETAMOL AND IBUPROFENE MIXTURES BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

    Directory of Open Access Journals (Sweden)

    Sophi Damayanti

    2010-06-01

    Full Text Available Analytical method for the determination of paracetamol and ibuprofene mixtures has been developed by High Performance Liquid Chromatography using C-18 column and acetinitrile - phosphate buffer pH = 4.5 (75:25 containing 0.075% sodium hexanesulfunate as a mobile phase. The detector was set at 215 nm. Using such conditions, retention time for paracetamol and ibuprofen was 4.89 and 7.11 min, respectively. The recovery for paracetamol and ibuprofen was found to be 101.07± 0.73% and 102.02 ± 1.58%, respectively. The detector limits of the method was 1.30 and 1.60 μg/mL with the relative standard deviation (RSD 0.74 and 1.52% for paracetamol and ibuprofen, respectively.   Keywords: paracetamol, ibuprofen, multi-component, validation, HPLC.

  17. Simultaneous determination of five flavonoids in saussurea involucrata by capillary electrophoresis

    International Nuclear Information System (INIS)

    Li, Y.; Zhong, H.; Zhong, H.

    2013-01-01

    A method of determination of five flavonoids in Saussurea involucrata by beta-cyclodextrin modified capillary zone electrophoresis has been developed.The effects of buffer pH and buffer concentration, applied voltage and beta-CD concentrations on the separation were systematically investigated. The optimum condition providing baseline separation of all compounds within 8 min was obtained in the 20 mmol per liter borax buffer (pH 9.2), 20 kV applied voltage and 8 mmol per liter beta-CD. The linearity, detection limits, limits of quantification, reproducibility and recovery were satisfactory. The beta-cyclodextrin modified capillary zone electrophoresis method proposed here has been satisfactorily employed to analyze S. involucrate samples. (author)

  18. [Simultaneous determination of multiple elements in airborne particulate samples by X-ray fluorescence spectrometry].

    Science.gov (United States)

    Takada, T; Hitosugi, M; Kadowaki, T; Kudo, M

    1983-07-01

    An energy dispersive X-ray fluorescence spectrometer (EDX) has been applied to determine multielements in the workplace air. The standards for X-ray fluorescence analysis were prepared by the chelate precipitation method on polyvinyl chloride (PVC) membrane filter. And, the specimens were prepared to deposit various metal compounds of different chemical forms by the suspension method on PVC membrane filter, and they were determined with EDX and atomic absorption spectrometer (AAS). The results obtained were as follows. Though there is a difference by each element, an amount less than 3 microgram/cm2 per unit area makes it possible to undergo multielement analysis, that is, is has no influence on fine particle effect (particle size; under 5 microns). Then, effects of the X-ray intensity by different chemical forms are negligible. At the presence the neighboring element and other elements this technique showed greater precision by carrying out on corrective treatment, etc. The coefficient of variation of this technique was in the range of 2.5-6.5% at DDTC-Cu of 0.5-5.0 micrograms/cm2, with the limit of detection for As : 0.002 microgram/cm2, Zn : 0.003 microgram/cm2, Pb : 0.003 microgram/cm2, Cu : 0.004 microgram/cm2, Ni : 0.003 microgram/cm2, Fe : 0.005 microgram/cm2, Mn : 0.008 microgram/cm2, Cr : 0.013 microgram/cm2, respectively. Aerosols collected at the workplace were analyzed with EDX and AAS, and the obtained results showed good agreement with such regression line as y = 1.04 chi + 0.04, the coefficient of correlation being r = 0.995. From these results, this technique was found to be a very excellent method for monitoring of multielements in the workplace air.

  19. Simultaneous determination of equivalence volumes and acid dissociation constants from potentiometric titration data.

    Science.gov (United States)

    Papanastasiou, G; Ziogas, I

    1995-06-01

    New iterative methods for analysis of potentiometric titration data of (a) mixtures of weak monoprotic acids with their conjugate bases, (b) solutions of polyprotic (di- and triprotic) acids, and (c) mixtures of two diprotic acids are presented. These methods, using data exclusively resulting from the acidic region of the titration curve permits the accurate determination of the analytical concentration of one or more acids even if the titration is stopped well before the end point of the titration. For the titration of a solution containing a conjugate acid/base pair, the proposed procedure enables the extraction of the initial composition of the mixture, as well as the dissociation constant of the concerned acid. Thus, it is possible by this type of analysis to distinguish whether a weak acid has been contaminated by a strong base and define the extent of the contamination. On the other hand, for the titration of polyprotic acids, the proposed approach enables the extraction of the accurate values of the equivalence volume and the dissociation constants K(i) even when the ionization stages overlap. Finally, for the titration of a mixture of two diprotic acids the proposed procedure enables the determination of the composition of the mixture even if the sum of the concentrations of the acids is not known. This method can be used in the analysis of solutions containing two diastereoisomeric forms of a weak diprotic acid. The test of the proposed procedures by means of ideal and Monte Carlo simulated data revealed that these methods are fairly applicable even when the titration data are considerably obscured by 'noise' or contain an important systematic error. The proposed procedures were also successfully applied to experimental titration data.

  20. Simultaneous determination of piracetam and vincamine by spectrophotometric and high-performance liquid chromatographic methods.

    Science.gov (United States)

    El-Saharty, Yasser Shaker Ibrahim

    2008-01-01

    A mixture of piracetam and vincamine was determined by 3 different methods. The first was the determination of piracetam and vincamine using the ratio-spectra first-derivative (DD1) spectrophotometric technique at 209 and 293 nm in concentration ranges of 10-45 and 2-14 microg/mL with mean recoveries of 99.22 +/- 0.72 and 99.67 +/- 0.79%, respectively. The second method was based on the resolution of the 2 components by bivariate calibration depending on a mathematic algorithm that provides simplicity and rapidity. The method depended on quantitative evaluation of the absorbencies at 210 and 225 nm in concentration ranges of 5-45 and 2-14 microg/mL, with mean recoveries of 100.33 +/- 0.54 and 100.44 +/- 0.98% for piracetam and vincamine, respectively. The third method was reversed-phase liquid chromatography using 0.05 M potassium dihydrogen phosphate-methanol (50 + 50, v/v) as the mobile phase, with the pH adjusted to 3.5 with phosphoric acid. The eluent was monitored at 215 nm in concentration ranges of 5-100 and 2-200 microg/mL, with mean recoveries of 99.62 +/- 0.67 and 99.32 +/- 0.85% for piracetam and vincamine, respectively. The suggested procedures were checked using laboratory-prepared mixtures and were successfully applied for the analysis of their pharmaceutical preparation. The methods retained their accuracy and precision when applying the standard addition technique. The results obtained by applying the proposed methods were statistically analyzed and compared with those obtained by the manufacturer's method.

  1. A comparison of simultaneous plasma, atomic absorption, and iron colorimetric determinations of major and trace constituents in acid mine waters

    Science.gov (United States)

    Ball, J.W.; Nordstrom, D. Kirk

    1994-01-01

    Sixty-three water samples collected during June to October 1982 from the Leviathan/Bryant Creek drainage basin were originally analyzed by simultaneous multielement direct-current plasma (DCP) atomic-emission spectrometry, flame atomic-absorption spectrometry, graphite-furnace atomic-absorption spectrometry (GFAAS) (thallium only), ultraviolet-visible spectrometry, and hydride-generation atomic-absorption spectrometry.Determinations were made for the following metallic and semi-metallic constituents: AI, As, B, Ba, Be, Bi, Cd, Ca, Cr, Co, Cu, Fe(11), Fe(total), Li, Pb, Mg, Mn, Mo, Ni, K, Sb, Se, Si, Na, Sr, TI, V, and Zn. These samples were re-analyzed later by simultaneous multielement inductively coupled plasma (ICP) atomic-emission spectrometry and Zeeman-corrected GFAAS to determine the concentrations of many of the same constituents with improved accuracy, precision, and sensitivity. The result of this analysis has been the generation of comparative concentration values for a significant subset of the solute constituents. Many of the more recently determined values replace less-than-detection values for the trace metals; others constitute duplicate analyses for the major constituents. The multiple determinations have yielded a more complete, accurate, and precise set of analytical data. They also have resulted in an opportunity to compare the performance of the plasma-emission instruments operated in their respective simultaneous multielement modes. Flame atomic-absorption spectrometry was judged best for Na and K and hydride-generation atomic-absorption spectrometry was judged best for As because of their lower detection limit and relative freedom from interelement spectral effects. Colorimetric determination using ferrozine as the color agent was judged most accurate, precise, and sensitive for Fe. Cadmium, lead, and vanadium concentrations were too low in this set of samples to enable a determination of whether ICP or DCP is a more suitable technique. Of

  2. Poly(alizarin red)/Graphene modified glassy carbon electrode for simultaneous determination of purine and pyrimidine

    Energy Technology Data Exchange (ETDEWEB)

    Ba Xi; Luo Liqiang [Department of Chemistry, Shanghai University, Shanghai 200444 (China); Ding Yaping, E-mail: wdingyp@sina.com [Department of Chemistry, Shanghai University, Shanghai 200444 (China); Zhang Zhen [Department of Chemistry, Shanghai University, Shanghai 200444 (China); Chu Yuliang [Instrumental Analysis and Research Center, Shanghai University, Shanghai 200444 (China); Wang Bijun; Ouyang Xiaoqian [Department of Chemistry, Shanghai University, Shanghai 200444 (China)

    2012-11-08

    Graphical abstract: DPVs of PAR/Graphene/GCE (a) and the bare GCE (c) in 0.1 M PBS containing 50.0 {mu}M G, 50.0 {mu}M A, 100.0 {mu}M T and 100.0 {mu}M C, (b) PAR/Graphene/GCE in 0.1 M PBS. Highlights: Black-Right-Pointing-Pointer The sensor exhibited well-separated peaks and low detection limit. Black-Right-Pointing-Pointer The sensor possesses high sensitivity and wide linear range. Black-Right-Pointing-Pointer The sensor was used for simultaneous detection of G, A, T and C successfully. Black-Right-Pointing-Pointer The sensor was applied in a fish sperm DNA sample with satisfactory results. Black-Right-Pointing-Pointer The proposed sensor has good stability and reproducibility. - Abstract: In this work, a poly(alizarin red)/Graphene composite film modified glassy carbon electrode (PAR/Graphene/GCE) was prepared for simultaneous determination of four DNA bases (guanine, adenine, thymine and cytosine) without any pretreatment. The morphology and interface property of PAR/Graphene films were examined by scanning electron microscopy and electrochemical impedance spectroscopy. The PAR/Graphene/GCE exhibited excellent electrocatalytic activity toward purine (guanine and adenine) and pyrimidine (thymine and cytosine) in 0.1 M phosphate buffer solution (pH 7.4). Under optimum conditions, differential pulse voltammetry was used to detect the oxidation of purine and pyrimidine. The results showed that PAR/Graphene/GCE exhibited well-separated peaks, low detection limit, high sensitivity and wide linear range for simultaneous detection of purine and pyrimidine. The proposed sensor also has good stability and reproducibility. Furthermore, the modified electrode was applied for the detection of DNA bases in a fish sperm DNA sample with satisfactory results.

  3. Poly(alizarin red)/Graphene modified glassy carbon electrode for simultaneous determination of purine and pyrimidine

    International Nuclear Information System (INIS)

    Ba Xi; Luo Liqiang; Ding Yaping; Zhang Zhen; Chu Yuliang; Wang Bijun; Ouyang Xiaoqian

    2012-01-01

    Graphical abstract: DPVs of PAR/Graphene/GCE (a) and the bare GCE (c) in 0.1 M PBS containing 50.0 μM G, 50.0 μM A, 100.0 μM T and 100.0 μM C, (b) PAR/Graphene/GCE in 0.1 M PBS. Highlights: ► The sensor exhibited well-separated peaks and low detection limit. ► The sensor possesses high sensitivity and wide linear range. ► The sensor was used for simultaneous detection of G, A, T and C successfully. ► The sensor was applied in a fish sperm DNA sample with satisfactory results. ► The proposed sensor has good stability and reproducibility. - Abstract: In this work, a poly(alizarin red)/Graphene composite film modified glassy carbon electrode (PAR/Graphene/GCE) was prepared for simultaneous determination of four DNA bases (guanine, adenine, thymine and cytosine) without any pretreatment. The morphology and interface property of PAR/Graphene films were examined by scanning electron microscopy and electrochemical impedance spectroscopy. The PAR/Graphene/GCE exhibited excellent electrocatalytic activity toward purine (guanine and adenine) and pyrimidine (thymine and cytosine) in 0.1 M phosphate buffer solution (pH 7.4). Under optimum conditions, differential pulse voltammetry was used to detect the oxidation of purine and pyrimidine. The results showed that PAR/Graphene/GCE exhibited well-separated peaks, low detection limit, high sensitivity and wide linear range for simultaneous detection of purine and pyrimidine. The proposed sensor also has good stability and reproducibility. Furthermore, the modified electrode was applied for the detection of DNA bases in a fish sperm DNA sample with satisfactory results.

  4. Enzymatic biosensor of horseradish peroxidase immobilized on Au-Pt nanotube/Au-graphene for the simultaneous determination of antioxidants

    Energy Technology Data Exchange (ETDEWEB)

    Wu, Long; Yin, Wenmin; Tang, Kun; Li, Dian; Shao, Kang; Zuo, Yunpeng; Ma, Jing; Liu, Jiawei; Han, Heyou, E-mail: hyhan@mail.hzau.edu.cn

    2016-08-24

    A new electrochemical method has been proposed for the simultaneous determination of butylated hydroxyanisole (BHA) and propyl gallate (PG) in food matrices based on enzymatic biosensors. Spiny Au-Pt nanotubes (SAP NTs) was first synthesized and demonstrated to exhibit intrinsic peroxidase and catalase-like activity. The structure of SAP NTs provides large surface area and favorable medium for electron transfer, on which HRP were immobilized and acted as enzymatic biosensor for the simultaneous detection of BHA and PG. The results revealed that BHA and PG both have well-defined oxidation waves with peak potentials of 624 and 655 mV, respectively. Under the optimal conditions, the method behaved satisfactory analytical performance towards BHA and PG with a wide linear range of 0.3–50 mg L{sup −1} and 0.1–100 mg L{sup −1}, as well as a detection limit of 0.046 mg L{sup −1} and 0.024 mg L{sup −1} (3σ/slope), respectively. Besides, the proposed method exhibits good sensitivity, stability and reproducibility, providing an alternative to fabricate electrode and construct sensitive biosensors. - Highlights: • SAP NTs was synthesized and demonstrated to exhibit intrinsic peroxidase and catalase-like activity. • The structure of SAP NTs provides larger surface area and more favorable medium for electron transfer. • Horseradish peroxidase immobilized on Au-Pt nanotube/Au-graphene acted as enzymatic biosensor. • The simultaneous detection of BHA and PG in food matrices was achieved based on enzymatic biosensors.

  5. Simultaneous determination of seven informative Y chromosome SNPs to differentiate East Asian, European, and African populations.

    Science.gov (United States)

    Muro, Tomonori; Iida, Reiko; Fujihara, Junko; Yasuda, Toshihiro; Watanabe, Yukina; Imamura, Shinji; Nakamura, Hiroaki; Kimura-Kataoka, Kaori; Yuasa, Isao; Toga, Tomoko; Takeshita, Haruo

    2011-05-01

    Identification of the population origin of an individual is very useful for crime investigators who need to narrow down a suspect based on specimens left at a crime scene. Single nucleotide polymorphisms of the Y chromosome (Y-SNPs) are a class of markers of interest to forensic investigators because many of the markers indicate regional specificity, thus providing useful information about the geographic origin of a subject. We selected seven informative Y-SNPs (M168, M130, JST021355, M96, P126, P196, and P234) to differentiate the three major population groups (East Asian, European, and African) and used them to develop forensic application. SNP genotyping was carried out by multiplex PCR reaction and multiplex single base extension (MSBE) reaction followed by capillary electrophoresis of extension products. This method can be used to assign a haplogroup from both degraded male DNA samples and DNA samples containing a mixture of female and male DNA through PCR primers that generate small amplicons (less than about 150 bp) and are highly specific for targets on the Y chromosome. The allelic state of each marker was definitively determined from a total of 791 males from the three major population groups. As expected, samples from the three major population groups showed Y-haplogroups common in the region of provenance: Y haplogroups C, D, and O for East Asians; IJ and R1 for Europeans; and AB and E for Africans. Published by Elsevier Ireland Ltd.

  6. Simultaneous determination of organophosphorous insecticides in bean samples by gas chromatography - flame photometric detection

    Directory of Open Access Journals (Sweden)

    Keyller Bastos Borges

    2014-02-01

    Full Text Available The indiscriminate use of organophosphorous pesticides (OPPs in crops may leave residues in food and may cause poisoning in the applicators. A method was developed for the determination of five OPPs in bean samples by Gas Chromatography-Flame Photometric Detection (GC-FPD. Validation parameters comprised linearity between 0.24 and 8.56 μg g-1 (r = 0.9985 for diazinon; 0.23 and 8.14 μg g-1 (r = 0.9959 for methyl parathion; 0.28 and 10.25 μg g-1 (r = 0.9987 for methyl pirimiphos; 0.52 and 18.87 μg g-1 (r = 0.9955 for malathion; 0.86 and 13.67 μg g-1 (r = 0.9919 for ethion. The limits of quantification (equal to those of detection were the lowest rates of ranges mentioned above for each compound. The extraction method showed approximately 95% recovery, with CV% < 15%. Although twenty-eight bean samples obtained in the southern region of the state of Minas Gerais,Brazil, were analyzed, they failed to match any of the OPPs under analysis. The absence of OPPs in the samples could be due to the degradation that occurred between the use of OPPs and bean commercialization, levels below the detection /quantification limits and the non-use of OPPs in bean cultivation.

  7. Simultaneous determination of octylphenol, nonylphenol, Bis(2-ethylehxyl) phathalate in biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Kim, J.H. [Jeonju University, Chonju (Korea)

    2001-04-01

    A comprehensive analytical method of endocrine disruptors[i.e., nonylphenol (NP), octylphenol (OP), bis (2-ethylhexyl) phthalate (BEHP) in meat or pork samples was developed. The method employed closed culture tube extraction with dichloromethane and solvent exchange to iso-hexane and SPE 92g) aminopropyl column, followed by determination on gas chromatography linked to mass spectrometry (GC/MS) operated in the single ion monitoring (SIM) mode. For the multipoint recovery of nonylphenol, octylphenol and bis (2-ethylhexyl) phthalate OP, NP were shown good recoveries in 0.125 {approx} 1.25 {mu}g/g range of concentration, and BEHP more good recoveries on 0.0125 {approx} 12.5 {mu}g/g wide range of concentration. The present method was applied to beef or pork samples of mart and butcher in Cheonju city and near cheonju. The range of concentrations was respectively, 0.06 {approx} 0.24 {mu}g/g in bis (2-ethylhexyl)phthalate (BEHP), but octylphenol (OP) was not dec ted in any samples. This method provides a powerful analytical tool to investigate a wide range of endocrine disruptors in biological samples of limited quantity. (author). 24 refs., 5 tabs., 3 figs.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2000-06-01

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

  9. Simultaneous determination of Rn-220 and Rn-222 concentrations in atmospheres by cellulose nitrate ionographic detectors

    International Nuclear Information System (INIS)

    Lobao, N.

    1977-01-01

    A method for the indoor determination of airborne radon and radon daughters is described, based in the utilization of cellulose nitrate (CN) ionographic detectors (LR-115-Kodak-Pathe) These track-etching detectors are coupled to an air sample and to a difusion chamber respectively. In the first system ambient air is pulled through a fiber glass filter for collection of airborne radon daughters (Flow: 230 ml/min). In the second system, the cellulose nitrate detectors is coupled/min). In the second system, the cellulose nitrate detectors is coupled to a difusion chamber electrostatic precipitator arrangement. Here the CN detector will register only the alpha particles given off by the decay products of Rn-222 formed within the sensitive volume of electrostatic precipitator. The construction of calibration curves for the two systems using adequate steady-state concentrations of Rn-220 and Rn-222 in an exposure chamber (1 cubic meter), will allow the use of the system for measurement of measurement of averaged integrated radon concentrations. The CN attached to the CN attached to the air sampler is exposed in the reference atmosphere with and without a mylar filter for discrimination of alpha particles with different energies Field sampling indicated however, that efficiency of the two systems are still low for the measurement of environmental levels of Rn-220 and Rn-222 within houses of the AENR, recommendations for efficienty improvement of the system are proposed [pt

  10. Studies on dosage of HIDANTOL-F by simultaneous determination of serum phenobarbital and diphenylhydantoin

    Energy Technology Data Exchange (ETDEWEB)

    Yamada, Hideo; Tanno, Munehiko; Muraki, Toshio; Fuse, Masaaki.

    1987-10-01

    In order to investigate causes of untoward effects frequently observed in elderly patients on HIDANTOL-F which contains 300 mg of phenobarbital(PB), 100 mg of diphenylhydantoin(DPH) and 200 mg of Na benzoate-caffein, blood levels of both PB and DPH were measured by radioimmunoassay. About half of the patients showed blood levels of PB distributed in therapeutic range, some of which were very cross to toxic range. None of the blood samples except one, however, was in therapeutic range in regard to DPH. There was some degree of correlation between blood levels of these two drugs (r = 0.53). Absolute doses of PB and blood levels showed linear relationship, while DPH was curvelinear in shape in regard to doseblood level relation, suggestive of MichaelisMenten pharmacokinetics. Taking account of blood levels of these two drugs in the present study, phenobarbital must be responsible for untoward effects of HIDANTOL-F as well as anticonvulsive effect. Synergistic effect and mutual influences over pharmacokinetics of PB and DPH were discussed. Ratio of several drugs in case of combination therapy should be determined on the basis of study on pharmacokinetics and interaction of drugs.

  11. Simultaneous HPLC method for determination of sodium trimethoprim phenylpropanol disulphonate and sodium sulfaquinoxaline in veterinary drugs

    Directory of Open Access Journals (Sweden)

    Puangkaew Lakkanatinaporn

    2004-11-01

    Full Text Available A simple HPLC method has been developed for the separation and determination of sodium trimethoprim phenylpropanol disulphonate and sodium sulfaquinoxaline in veterinary preparations. Both drugs were separated well on a Kromasil C18 column (5 µm, 150 × 4.6 mm using a mixture of acetonitrile and 0.5% triethylamine in 1% acetic acid, pH 3 (18:82, v/v as the mobile phase at the flow rate of 1.5 ml/ min. The presence of both substances was monitored by UV absorption detection at 271 nm. The retention times of sodium trimethoprim phenylpropanol disulphonate and sodium sulfaquinoxaline were 3.2 and 16.0 min, respectively. The performance of the developed method was tested. Linear responses of both drugs were achieved between 48-145% of labeled amount over the concentration ranges of 35-101 µg/ml and 102-306 µg/ ml for sodium trimethoprim phenylpropanol disulphonate and sodium sulfaquinoxaline with correlation coefficients (R2 of 0.9980 and 0.9998, respectively. Accuracy expressed in term of recoveries were 101.4± 1.21% (n=6 for sodium trimethoprim phenylpropanol disulphonate and 99.7±0.92% (n=6 for sodium sulfaquinoxaline. Precision of the method in terms of the relative standard deviation is not more than 2% in all cases. These figures of merit indicated the validity of the developed method.

  12. High precision optical measurement of displacement and simultaneous determinations of piezoelectric coefficients

    Science.gov (United States)

    Gamboa, Bryan M.; Malladi, Madhuri; Vadlamani, Ramya; Guo, Ruyan; Bhalla, Amar

    2016-09-01

    PZT are also well known for their applications in Micro Electrical Mechanical Systems (MEMS). It is necessary to study the piezoelectric coefficients of the materials accurately in order to design a sensor as an example, which defines their strain dependent applications. Systematic study of the electro mechanic displacement measurement was conducted and compared using a white light fiber optic sensor, a heterodyne laser Doppler vibrometer, and a homodyne laser interferometry setup. Frequency dependent measurement is conducted to evaluate displacement values well below and near the piezoelectric resonances. UHF-120 ultra-high frequency Vibrometer is used to measure the longitudinal piezoelectric displacement or x33 and the MTI 2000 FotonicTM Sensor is used to measure the transverse piezoelectric displacement or x11 over 100Hz to 2MHz. A Multiphysics Finite Element Analysis method, COMSOL, is also adopted in the study to generate a three dimensional electromechanical coupled model based on experimentally determined strains x33 and x11 as a function of frequency of the electric field applied. The full family of piezoelectric coefficients of the poled electronic ceramic PZT, d33, d31, and d15, can be then derived, upon satisfactory simulation of the COMSOL. This is achieved without the usual need of preparation of piezoelectric resonators of fundamental longitudinal, transversal, and shear modes respectively.

  13. Studies on dosage of HIDANTOL-F by simultaneous determination of serum phenobarbital and diphenylhydantoin

    International Nuclear Information System (INIS)

    Yamada, Hideo; Tanno, Munehiko; Muraki, Toshio; Fuse, Masaaki.

    1987-01-01

    In order to investigate causes of untoward effects frequently observed in elderly patients on HIDANTOL-F which contains 300 mg of phenobarbital(PB), 100 mg of diphenylhydantoin(DPH) and 200 mg of Na benzoate-caffein, blood levels of both PB and DPH were measured by radioimmunoassay. About half of the patients showed blood levels of PB distributed in therapeutic range, some of which were very cross to toxic range. None of the blood samples except one, however, was in therapeutic range in regard to DPH. There was some degree of correlation between blood levels of these two drugs (r = 0.53). Absolute doses of PB and blood levels showed linear relationship, while DPH was curvelinear in shape in regard to doseblood level relation, suggestive of MichaelisMenten pharmacokinetics. Taking account of blood levels of these two drugs in the present study, phenobarbital must be responsible for untoward effects of HIDANTOL-F as well as anticonvulsive effect. Synergistic effect and mutual influences over pharmacokinetics of PB and DPH were discussed. Ratio of several drugs in case of combination therapy should be determined on the basis of study on pharmacokinetics and interaction of drugs. (author)

  14. Simultaneous determination of phenylethanoid glycosides and aglycones by capillary zone electrophoresis with running buffer modifier.

    Science.gov (United States)

    Dong, Shuqing; Gao, Ruibin; Yang, Yan; Guo, Mei; Ni, Jingman; Zhao, Liang

    2014-03-15

    Although the separation efficiency of capillary electrophoresis (CE) is much higher than that of other chromatographic methods, it is sometimes difficult to adequately separate the complex ingredients in biological samples. This article describes how one effective and simple way to develop the separation efficiency in CE is to add some modifiers to the running buffer. The suitable running buffer modifier β-cyclodextrin (β-CD) was explored to fast and completely separate four phenylethanoid glycosides and aglycones (homovanillyl alcohol, hydroxytyrosol, 3,4-dimethoxycinnamic acid, and caffeic acid) in Lamiophlomis rotata (Lr) and Cistanche by capillary zone electrophoresis with ultraviolet (UV) detection. It was found that when β-CD was used as running buffer modifier, a baseline separation of the four analytes could be accomplished in less than 20 min and the detection limits were as low as 10(-3) mg L(-1). Other factors affecting the CE separation, such as working potential, pH value and ionic strength of running buffer, separation voltage, and sample injection time, were investigated extensively. Under the optimal conditions, a successful practical application on the determination of Lr and Cistanche samples confirmed the validity and practicability of this method. Copyright © 2014 Elsevier Inc. All rights reserved.

  15. Simultaneous determination of artificial sweeteners, preservatives, caffeine, theobromine and theophylline in food and pharmaceutical preparations by ion chromatography.

    Science.gov (United States)

    Chen, Q C; Wang, J

    2001-12-07

    A novel ion chromatographic method was proposed for the simultaneous determination of artificial sweeteners (sodium saccharin, aspartame, acesulfame-K), preservatives (benzoic acid, sorbic acid), caffeine, theobromine and theophylline. The separation was performed on an anion-exchange analytical column operated at 40 degrees C within 45 min by an isocratic elution with 5 mM aqueous NaH2PO4 (pH 8.20) solution containing 4% (v/v) acetonitrile as eluent, and the determination by wavelength-switching ultraviolet absorbance detection. The detection limits (signal-to-noise ratio 3:1) for all analytes were below the sub-microg/ml level. Under the experimental conditions, several organic acids, including citric acid, malic acid, tartaric acid and ascorbic acid, did not interfere with the determination. The method has been successfully applied to the analysis of various food and pharmaceutical preparations, and the average recoveries for real samples ranged from 85 to 104%. The levels of all analytes determined by this method were in good agreement with those obtained by the high-performance liquid chromatographic procedure. The results also indicated that ion chromatography would be possibly a beneficial alternative to conventional high-performance liquid chromatography for the separation and determination of these compounds.

  16. Simultaneous determination of selenium and tellurium in native sulfur by atomic absorption spectrophotometry

    International Nuclear Information System (INIS)

    Arikawa, Yoshiko; Hirai, Shoji; Ozawa, Takejiro.

    1979-01-01

    A method for the determination of selenium and tellurium in native sulfur has been investigated by means of atomic absorption spectrophotometry. Native sulfur collected from around fumarole or volcanic crater is ground down into powder, a portion of which weighing 1 g is subjected to analysis. A 2.6% (w/v) sodium hydroxide solution is added by 10 ml to the sample in a teflon beaker, and the mixture is then heated on a hot plate. Sulfur is decomposed and dissolved in the form of disulfide and thiosulfate. A 30% hydrogenperoxide solution is added by 10 ml to oxidize them to sulfate. At the same time selenium and tellurium contained in the sulfur sample are also thought to be oxidized to Se(VI) and Te(VI) states. The solution is neutralized with hydrochloric acid and diluted with distilled water to 100 ml. The sample solution thus prepared is sprayed into the air-acetylene flame of the atomic absorption spectrophotometer. The absorbance is measured at 195.9 nm for selenium and 214.2 nm for tellurium. Calibration curve is prepared by measuring the absorbances of the solutions prepared as follows. One gram portions of pure sulfur (99.9999%) are decomposed as for the samples. After neutralization, standard solutions containing each same amount of selenium and tellurium (0 -- 1000 μg) are added to the sulfur solution and then diluted with water to 100 ml. The standard deviations were estimated to be 50.4 ppm for selenium at 756 ppm and 16.6 ppm for tellurium at 587 ppm. For the check of the reliability of the method, results were compared with those obtained by neutron activation analysis. Results obtained by both methods showed good agreement. (author)

  17. Simultaneous determination of household and market-oriented activities of women in rural Pakistan.

    Science.gov (United States)

    Alderman, H; Chishti, S

    1991-01-01

    Researchers applied data from the 1985-1986 Labour Force Survey in Pakistan to a model which focused on household composition variables and human assets such as education to examine determinants of female labor force participation in the framework of their labor on other productive tasks in the household in rural areas. Monthly household labor decreased by 1.8 days for each additional adult woman in the household and by 1.4 days for each 10-15 year old girl. On the other hand, an extra teenage boy added as much to each woman's workload as did an additional 5-9 year old child (.37 days). Each additional 6 year old child increased the workload 1.3 days/month and this did not include child care activities. Women who had attended primary school worked in the household 1.4 days less than those who did not attend any school. Moreover those who attended school beyond primary school worked in the household 3.7 days less than those who did not attend any school. both of these differences were statistically significant. Yet educated women worked more outside the house than uneducated women (1.2 days for those with primary education and 2.4 days for those with post primary education). The government should promote increased female school participation by increasing its investment in schooling to lower the costs to households. Further it could provide opportunities for educated women to be employed in their own communities. Thus they can envision education in their private interest (both in social and financial terms). If these efforts are not done, however, demand and supply considerations may continue to restrain schooling for females.

  18. Validation of an HPLC method for the simultaneous determination of eletriptan and UK 120.413

    Directory of Open Access Journals (Sweden)

    LJILJANA ZIVANOVIC

    2006-11-01

    Full Text Available Arapid and sensitive RPHPLCmethod was developed for the routine control analysis of eletriptan hydrobromide and its organic impurity UK 120.413 in Relpax® tablets. The chromatography was performed at 20 °Cusing a C18 XTerraTM (5 m, 150 × 4,6 mm column at a flow rate 1.0 ml/min. The drug and its impurity were detected at 225 nm. The mobile phase consisted of TEA (1 % – methanol (67.2:32.8 v/v, the pH of which was adjusted to 6.8 with 85 % orthophosphoric acid. Quantification was accomplished by the internal standard method. The developed RP HPLC method was validated by testing: accuracy, precision, repeatibility, specificity, detection limit, quantification limit, linearity, robustness and sensitivity. High linearity of the analytical procedure was confirmed over the concentration range of 0.05 – 1.00 mg/ml for eletriptan hydrobromide and from 0.10 – 1.50 µg/ml for UK 120.413, with correlation coefficients greater than r = 0.995. The low value of the RSD expressed the good repeatability and precision of the method. Experimental design and a response surface method were used to test robustness of the analytical procedure and to evaluate the effect of variation of the method parameters, namely the mobile phase composition, pH and temperature. They showed small deviations from the method setting. The good recovery and low RSD confirm the suitability of the proposed RP HPLC method for the routine determination of eletriptan hydrobromide and its impurity UK 120.413 in Relpax® tables.

  19. Simultaneous determination of lead, cadmium and zinc in Metro Manila air particulates by anodic stripping voltammetry

    International Nuclear Information System (INIS)

    Castaneda, Soledad S.

    1999-02-01

    Air particulate samples were collected from two monitoring stations in Metro Manila using a 'Gent' type dichotomous sampler for pollutant source apportionment studies. Samples were collected in two fractions: a fine fraction with aerodynamic diameter, d p p 3 : HCL: HF, 4: 1: 1) for at least 20 minutes with subsequent heating at lower power settings for a total of 20 minutes more, effectively decomposed the sample with complete recovery of the elements. The digests were evaporated to near dryness to eliminate the troublesome effect of HF and HNO 3 and to decrease acidity of the electrolytic solution to pH ≥ 2. At pH 2, the addition of at least 0.01 M KCl was needed to improve sensitivity. The formation of Zn-Cu intermetallic compounds which interfered in the accurate quantitation of zinc was eliminated by addition of gallium as a 'third' element. The amount of gallium needed varied from sample to sample and was affected by the pH of the solution. The DPASV parameters found to be optimum for the analysis of the air particulate samples are as follows: pulse amplitude, 50 mV; scan rate, 10 mV/sec; E dep , - 1.30 V; t dep , 2 min; and RDE rotation rate, 1500 rpm. Detection limits of 0.2 ppb for zinc, 0.6 ppb for lead, and 0.05 ppb for cadmium in the sample matrix were obtained. The standard addition method was found to be reliable for the quantitative determination of the analytes in the sample. All R 2 values obtained were > 0.9900 at 95% confidence level. Validation of the established analytical methodology by analyzing certified reference standards and performing parallel analysis by GF-AAS and flame AAS showed acceptable accuracy of the DPASV measurements. (Author)

  20. Stability-indicating RP-HPLC method for the simultaneous determination of escitalopram oxalate and clonazepam.

    Science.gov (United States)

    Kakde, Rajendra B; Satone, Dinesh D; Gadapayale, Kamalesh K; Kakde, Megha G

    2013-07-01

    The objective of the current study was to develop a validated, specific stability-indicating reversed-phase liquid chromatographic (LC) method for the quantitative determination of escitalopram oxalate and clonazepam and their related substances in bulk drugs and pharmaceutical dosage forms in the presence of degradation products. Forced degradation studies were performed on the pure drugs of escitalopram oxalate and clonazepam, as per the stress conditions prescribed by the International Conference on Harmonization (ICH) using acid, base, oxidation, thermal stress and photolytic degradation to show the stability-indicating power of the method. Significant degradation was observed during acid and alkaline hydrolysis and no degradation was observed in other stress conditions. The chromatographic method was optimized using the samples generated from forced degradation studies. Good resolution between the peaks corresponded to the active pharmaceutical ingredients, escitalopram oxalate and clonazepam, and degradation products from the analyte were achieved on an ODS Hypersil C18 column (250 × 4.6 mm) using a mobile phase consisting of a mixture of acetonitrile-50 mM phosphate buffer + 10 mM triethylamine (70:30, v/v). The detection was conducted at 268 nm. The limit of detection and the limit of quantitation for escitalopram oxalate and clonazepam were established. The stress test solutions were assayed against the qualified working standards of escitalopram oxalate and clonazepam, which indicated that the developed LC method was stability-indicating. Validation of the developed LC method was conducted as per ICH requirements. The developed LC method was found to be suitable to check the quality of bulk samples of escitalopram oxalate and clonazepam.

  1. A validated HPTLC method for the quantification of friedelin in Putranjiva roxburghii Wall extracts and in polyherbal formulations

    Directory of Open Access Journals (Sweden)

    Kedar Kalyani Abhimanyu

    2017-06-01

    Full Text Available In present study HPTLC method was developed and validated for the determination of friedelin in Putranjiva roxburghii Wall (family: Euphorbiaceae leaf, bark extract and in polyherbal formulations. Analysis of samples were performed on TLC aluminium precoated plate (60 F254 by using mobile phase toluene: chloroform (9:1 v/v. Plate was derivatized with vanillin sulphuric acid and scanned at 580 nm. Developed method found to give compact spot for friedelin at Rf value 0.43 ± 0.01. The method was validated using International Council for Harmonization (ICH guidelines including linearity, precision, accuracy, and robustness. Friedelin was found to be present in leaf extract of Putranjiva roxburghii Wall (0.003% w/w, in bark (0.04% w/w, formulation 1 (0.002% w/w and formulation 2 (0.035% w/w. A good linearity relationship was found to be (100–500 ng spot−1 with correlation coefficient (r2 value of 0.9892 for friedelin. Limit of detection and limit of quantitation was found to be 32.15, 97.44 ng/band respectively for friedelin. The developed method was found to be accurate and precise with 0.78%, 0.9% (%RSD for interday and intraday precision. Accuracy of the method was performed by recovery studies at three different concentration levels and the average percentage recovery was found to be 98.55% for friedelin. The proposed method for the quantitation of friedelin was found to be simple, specific, accurate and robust in Putranjiva roxburghii Wall and polyherbal formulations.

  2. Simultaneous determination of vasicine and vasicinone by High-performance liquid chromatography in roots of eight Sida species.

    Science.gov (United States)

    Subramanya, M D; Pai, Sandeep R; Ankad, Gireesh M; Hegde, Harsha V; Roy, Subarna; Hoti, S L

    2016-01-01

    Sida L. is a medicinally important genus widely used in conventional systems of medicine in India. The present study aims toward simultaneous determination of two bioactive compounds vasicine and vasicinone in root extracts of eight Sida spp. from Western Ghats, India. Determination of vasicine and vasicinone was undertaken in methanolic root extracts (10% w/v) of Sida acuta , Sida cordata , Sida cordifolia , Sida rhombifolia , Sida spinosa , Sida indica , Sida retusa and Sida mysorensis by high performance liquid chromatography (HPLC) method. The standards were prepared with the concentration of mg/mL. Data were expressed as mean values of three reading and relative standard deviations. The separation was achieved on a Waters, Nova-Pack, C18 (250 mm × 4.6 mm, 5 μ) column, with acetonitrile - 0.1 M phosphate buffer-glacial acetic acid (15: 85: 1, v/v/v) as solvent system at a flow-rate of 1.0 mL/min. The effluent was monitored using ultraviolet detection at a wavelength of 300 nm. Both calibration curves of standard showed good linear regression ( R 2 > 0.994). The limit of detection and the limit of quantification for vasicine was 0.110 and 0.333 μg/mL and for vasicinone was 0.059 and 0.179 μg/mL respectively. The vasicine content was highest in S. cordifolia (9.891 ± 0.495 μg/100 mg) and vasicinone content was rich in S. cordata (33.013 ± 1.651 μg/100 mg.) The content of vasicinone was higher than vasicine. HPLC method provides simple, accurate, and reproducible quantitative analysis for simultaneous determination of vasicine and vasicinone. Among the selected Sida species, S. cordifolia and S. cordata were found to be rich in the vasicine and vasicinone contents, respectively.

  3. Simultaneous in situ derivatization and ultrasound-assisted dispersive magnetic solid phase extraction for thiamine determination by spectrofluorimetry.

    Science.gov (United States)

    Tarigh, Ghazale Daneshvar; Shemirani, Farzaneh

    2014-06-01

    A simple and rapid method for the simultaneous in situ derivatizaion, preconcentration and extraction of thiamine (vitamin B1) as a model analyte was developed by a novel quantitative method, namely ultrasound-assisted dispersive magnetic solid phase extraction spectrofluorimetry (USA-DMSPE-FL) from different real samples. This method consists of sample preparation, in situ derivatization, exhaustive extraction and clean up by a single process. High extraction efficiency and in situ derivatization in a short period of time is the main advantages of this procedure. For this purpose, the reusable magnetic multi-wall carbon nanotube (MMWCNT) nanocomposite was used as an adsorbent for preconcentration and determination of thiamine. Thiamine was, simultaneously, in situ derivatized as thiochrome by potassium hexacyanoferrate (III) and adsorbed on MMWCNT in an ultrasonic water bath. The MMWCNTs were then collected using an external magnetic field. Subsequently, the extracted thiochrome was washed from the surface of the adsorbent and determined by spectrofluorimetry. The developed method, which has been analytically characterized under its optimal operating conditions, allows the detection of the analyte in the samples with method detection limits of 0.37 µg L(-1). The repeatability of the method, expressed as the relative standard deviation (RSD, n=6), varies between 2.0% and 4.8% in different real samples, while the enhancement factor is 197. The proposed procedure has been applied for the determination of thiamine in biological (serum and urine), pharmaceutical (multivitamin tablet and B complex syrup) and foodstuff samples (cereal, wheat flour, banana and honey) with the good recoveries in the range from 90% to 105%. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. Simultaneous determination of free and total glycerol in biodiesel by capillary electrophoresis using multiple short-end injection.

    Science.gov (United States)

    Spudeit, Daniel Alfonso; Piovezan, Marcel; Dolzan, Maressa D; Vistuba, Jacqueline Pereira; Azevedo, Mônia Stremel; Vitali, Luciano; Leal Oliveira, Marcone Augusto; Oliveira Costa, Ana Carolina; Micke, Gustavo Amadeu

    2013-12-01

    A rapid method for the simultaneous determination of free glycerol (FG) and total glycerol (TG) in biodiesel by CE using a short-end multiple injection (SE/MI) configuration system is described. The sample preparation for FG involves the extraction of glycerol with water and for TG a saponification reaction is carried out followed by extraction as in the case of FG. The glycerol extracted in both cases is submitted to periodate oxidation and the iodate ions formed are measured on a CE-SE/MI system. The relevance of this study lies in the fact that no analytical procedure has been previously reported for the determination of TG (or of FG and TG simultaneously) by CE. The optimum conditions for the saponification/extraction process were 1.25% KOH and 25°C, with a time of only 5 min, and biodiesel mass in the range of 50.0-200.0 mg can be used. Multiple injections were performed hydrodynamically with negative pressure as follows: 50 mbar/3s (FG sample); 50 mbar/6s (electrolyte spacer); 50 mbar/3s (TG sample). The linear range obtained was 1.55-46.5 mg/L with R(2) > 0.99. The LOD and LOQ were 0.16 mg/L and 0.47 mg/L, respectively for TG. The method provides acceptable throughput for application in quality control and monitoring biodiesel synthesis process. In addition, it offers simple sample preparation (saponification process), it can be applied to a variety biodiesel samples (soybean, castor, and waste cooking oils) and it can be used for the determination of two key parameters related to the biodiesel quality with a fast separation (less than 30 s) using an optimized CE-SE/MI system. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Simultaneous determination of eugenol, isoeugenol and methyleugenol in fish fillet using gas chromatography coupled to tandem mass spectrometry.

    Science.gov (United States)

    Ke, Changliang; Liu, Qi; Li, Liudong; Chen, Jiewen; Wang, Xunuo; Huang, Ke

    2016-09-15

    Gas chromatography (GC) coupled with triple quadrupole tandem mass spectrometry (MS/MS) operated in electron ionization mode (EI) has been shown to have advantages in the trace analysis of chemical compounds. Employing the instrument, a method has been built to simultaneously determine eugenol, isoeugenol' and methyleugenol, which have been widely used as fish anesthetic, in the fish fillet. Procedure for the sample preparation was achieved by using hexane extraction followed by phenyl solid phase extraction (SPE) cleanup, which was free of such steps as rotary evaporation and nitrogen blowing by taking the volatility of eugenol and its isomers into consideration. The method was validated by conducting recovery studies on fortified fish fillet samples at four concentrations. The linearity in the range of 5-500μg·L(-1) was forced through the origin giving a coefficient of determination (r(2)) greater than 0.9982. Limits of detection (LODs) for eugenol, isoeugenol' and methyleugenol were 0.4, 1.2' and 0.2μg·kg(-1), respectively. The limits of quantification (LOQs) were 1.2, 4' and 0.7μg·kg(-1) for eugenol, isoeugenol' and methyleugenol, respectively. The recoveries for eugenol and its isomers ranged from 76.4 to 99.9% with relative standard deviations (RSD) in a range from 2.18 to 15.5%. This method is quick, simple and suitable for determining the residues of eugenol, isoeugenol and methyleugenol simultaneously in batch samples of fish fillet. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. An Improved Enzymatic Indirect Method for Simultaneous Determinations of 3-MCPD Esters and Glycidyl Esters in Fish Oils.

    Science.gov (United States)

    Miyazaki, Kinuko; Koyama, Kazuo

    2017-10-01

    The enzymatic indirect method for simultaneous determinations of 3-chloro-1, 2-propanediol fatty acid esters (3-MCPD-Es) and glycidyl fatty acid esters (Gly-Es) make use of lipase from Candida cylindracea (previously referred to as C. rugosa). Because of low substrate specificity of the lipase for esters of polyunsaturated fatty acids (PUFA), such as docosahexaenoic acid (DHA) and eicosapentaenoic acid (EPA), fish oils high in PUFAs are currently excluded from the range of application of the method. The objective of this study was to make the enzymatic indirect method applicable to fats and oils containing PUFAs. By using a Burkholderia cepacia lipase, and by removing sodium bromide from hydrolysis step and adding it after completion of the hydrolysis step, satisfactory recovery rates of 91-109% for 3-MCPD, and 91-110% for glycidol (Gly) were obtained from an EPA and DHA concentrated sardine oil, three DHA concentrated tuna oils, two fish oils, and five fish-oil based dietary supplements spiked with DHA-esters or oleic acid-esters of 3-MCPD and Gly at 20 mg/kg. Further, results from unspiked samples of seven fish oil based dietary supplements and five DHA concentrated tuna oils analyzed by the improved enzymatic indirect method were compared with the results analyzed by AOCS Cd 29a. For all 3-MCPD, 2-MCPD and Gly, the 95% confidence intervals determined by the weighted Deming regression for slopes and intercepts contained the value of 1 and 0, respectively. It was therefore concluded that the results from the two methods were not statistically different. These results suggest that fish oils high in PUFAs may be included in the range of application for the improved enzymatic indirect method for simultaneous determinations of 3-MCPD and Gly esters in fats and oils.

  7. Simultaneous determination of piracetam and its four impurities by RP-HPLC with UV detection.

    Science.gov (United States)

    Arayne, M Saeed; Sultana, Najma; Siddiqui, Farhan Ahmed; Mirza, Agha Zeeshan; Qureshi, Faiza; Zuberi, M Hashim

    2010-08-01

    A simple and rapid high-performance liquid chromatographic method for the separation and determination of piracetam and its four impurities, 2-oxopyrrolidin-1-yl)acetic acid, pyrrolidin-2-one, methyl (2-oxopyrrolidin-1-yl)acetate, and ethyl (2-oxopyrrolidin-1-yl)acetate, was developed. The separation was achieved on a reversed-phase C(18) Nucleosil column (25 cm x 0.46 cm, 10 microm). The mobile phase is composed of an aqueous solution containing 0.2 g/L of triethyl amine-acetonitrile (85:15, v/v). The pH of the mobile phase was adjusted to 6.5 with phosphoric acid at a flow rate of 1 mL/min at ambient temperature and UV detection at 205 nm. The developed method was found to give good separation between the pure drug and its four related substance. The polynomial regression data for the calibration plots showed good linear relationship in the concentration range of 50-10,000 ng/mL, 25-10,000 ng/mL, 45-10,000 ng/mL, 34-10,000 ng/mL, and 55-10,000 ng/mL, respectively, with r(2) = 0.9999. The method was validated for precision, accuracy, ruggedness, and recovery. The minimum quantifiable amounts were found to be 50 ng/mL of piracetam, 25 ng/mL of 2-oxopyrrolidin-1-yl)acetic acid, 45 ng/mL of pyrrolidin-2-one, 34 ng/mL of methyl (2-oxopyrrolidin-1-yl)acetate, and 55 ng/mL of ethyl (2-oxopyrrolidin-1-yl)acetate. Statistical analysis proves that the method is reproducible and selective for the estimation of piracetam as well as its related substance. As the method could effectively separate the drug from the related substances, it can be employed as a stability-indicating one. The proposed method shows high efficiency, allowing the separation of the main component piracetam from other impurities.

  8. A validated RP-HPLC method for simultaneous determination of propranolol and valsartan in bulk drug and gel formulation

    Science.gov (United States)

    Imam, Syed Sarim; Ahad, Abdul; Aqil, Mohammed; Sultana, Yasmin; Ali, Asgar

    2013-01-01

    Objective: A simple, precise, and stability indicating high performance liquid chromatography (HPLC) method was developed and validated for the simultaneous determination of propranolol hydrochloride and valsartan in pharmaceutical dosage form. Materials and Methods: The method involves the use of easily available inexpensive laboratory reagents. The separation was achieved on Hypersil ODS C-18 column (250*4.6 mm, i.d., 5 μm particle size) with isocratic flow with UV detector. The mobile phase at a flow rate of 1.0 mL/min consisted of acetonitrile, methanol, and 0.01 M disodium hydrogen phosphate (pH 3.5) in the ratio of 50:35:15 v/v. Results: A linear response was observed over the concentration range 5-50 μg/mL of propranolol and the concentration range 4-32 μg/mL of valsartan. Limit of detection and limit of quantitation for propranolol were 0.27 μg/mL and 0.85 μg/mL, and for valsartan were 0.45 μg/mL and 1.39 μg/mL, respectively. The method was successfully validated in accordance to ICH guidelines acceptance criteria for linearity, accuracy, precision, specificity, robustness. Conclusion: The analysis concluded that the method was selective for simultaneous estimation of propranolol and valsartan can be potentially used for the estimation of these drugs in combined dosage form. PMID:23559826

  9. Simultaneous electrochemical determination of dopamine and paracetamol on multiwalled carbon nanotubes/graphene oxide nanocomposite-modified glassy carbon electrode.

    Science.gov (United States)

    Cheemalapati, Srikanth; Palanisamy, Selvakumar; Mani, Veerappan; Chen, Shen-Ming

    2013-12-15

    In the present study, multiwalled carbon nanotubes (MWCNT)/graphene oxide (GO) nanocomposite was prepared by homogenous dispersion of MWCNT and GO and used for the simultaneous voltammetric determination of dopamine (DA) and paracetamol (PA). The TEM results confirmed that MWCNT walls were wrapped well with GO sheets. The MWCNT/GO nanocomposite showed superior electrocatalytic activity towards the oxidation of DA and PA, when compared with either pristine MWCNT or GO. The major reason for the efficient simultaneous detection of DA and PA at nanocomposite was the synergistic effect between MWCNT and GO. The electrochemical oxidation of DA and PA was investigated by cyclic voltammetry, differential pulse voltammetry and amperometry. The nanocomposite modified electrode showed electrocatalytic oxidation of DA and PA in the linear response range from 0.2 to 400 µmol L(-1) and 0.5 to 400 µmol L(-1) with the detection limit of 22 nmol L(-1) and 47 nmol L(-1) respectively. The proposed sensor displayed good selectivity, sensitivity, stability with appreciable consistency and precision. © 2013 Elsevier B.V. All rights reserved.

  10. Effect of Body Position on Energy Expenditure of Preterm Infants as Determined by Simultaneous Direct and Indirect Calorimetry.

    Science.gov (United States)

    Bell, Edward F; Johnson, Karen J; Dove, Edwin L

    2017-04-01

    Background  Indirect calorimetry is the standard method for estimating energy expenditure in clinical research. Few studies have evaluated indirect calorimetry in infants by comparing it with simultaneous direct calorimetry. Our purpose was (1) to compare the energy expenditure of preterm infants determined by these two methods, direct calorimetry and indirect calorimetry; and (2) to examine the effect of body position, supine or prone, on energy expenditure. Study Design  We measured energy expenditure by simultaneous direct (heat loss by gradient-layer calorimeter corrected for heat storage) and indirect calorimetry (whole-body oxygen consumption and carbon dioxide production) in 15 growing preterm infants during two consecutive interfeeding intervals, once in the supine position and once in the prone position. Results  The mean energy expenditure for all measurements in both positions did not differ significantly by the method used: 2.82 (standard deviation [SD] 0.42) kcal/kg/h by direct calorimetry and 2.78 (SD 0.48) kcal/kg/h by indirect calorimetry. The energy expenditure was significantly lower, by 10%, in the prone than in the supine position, whether examined by direct calorimetry (2.67 vs. 2.97 kcal/kg/h, p  Direct calorimetry and indirect calorimetry gave similar estimates of energy expenditure. Energy expenditure was 10% lower in the prone position than in the supine position. Thieme Medical Publishers 333 Seventh Avenue, New York, NY 10001, USA.

  11. Simultaneous Determination of 6-Mercaptopurine and its Oxidative Metabolites in Synthetic Solutions and Human Plasma using Spectrophotometric Multivariate Calibration Methods

    Directory of Open Access Journals (Sweden)

    Mohammad-Reza Rashidi

    2011-06-01

    Full Text Available Introduction: 6-Mercaptopurine (6MP is an important chemotherapeutic drug in the conventional treatment of childhood acute lymphoblastic leukemia (ALL. It is catabolized to 6-thiouric acid (6TUA through 8-hydroxo-6-mercaptopurine (8OH6MP or 6-thioxanthine (6TX intermediates. Methods: High-performance liquid chromatography (HPLC is usually used to determine the contents of therapeutic drugs, metabolites and other important biomedical analytes in biological samples. In the present study, the multivariate calibration methods, partial least squares (PLS-1 and principle component regression (PCR have been developed and validated for the simultaneous determination of 6MP and its oxidative metabolites (6TUA, 8OH6MP and 6TX without analyte separation in spiked human plasma. Mixtures of 6MP, 8-8OH6MP, 6TX and 6TUA have been resolved by PLS-1 and PCR to their UV spectra. Results: Recoveries (% obtained for 6MP, 8-8OH6MP, 6TX and 6TUA were 94.5-97.5, 96.6-103.3, 95.1-96.9 and 93.4-95.8, respectively, using PLS-1 and 96.7-101.3, 96.2-98.8, 95.8-103.3 and 94.3-106.1, respectively, using PCR. The NAS (Net analyte signal concept was used to calculate multivariate analytical figures of merit such as limit of detection (LOD, selectivity and sensitivity. The limit of detections for 6MP, 8-8OH6MP, 6TX and 6TUA were calculated to be 0.734, 0.439, 0.797 and 0.482 µmol L-1, respectively, using PLS and 0.724, 0.418, 0783 and 0.535 µmol L-1, respectively, using PCR. HPLC was also applied as a validation method for simultaneous determination of these thiopurines in the synthetic solutions and human plasma. Conclusion: Combination of spectroscopic techniques and chemometric methods (PLS and PCR has provided a simple but powerful method for simultaneous analysis of multicomponent mixtures.

  12. Simultaneous Determination of Ibuprofen and Caffeine in Urine Samples by Combining MCR-ALS and Excitation-emission Data

    Directory of Open Access Journals (Sweden)

    Masoumeh Mohammadnejad

    2016-06-01

    Full Text Available Second order advantage of excitation-emission fluorescence matrix was applied for the simultaneous determination of ibuprofen and caffeine. The proposed method is based on the measurement of the native fluorescence and recording emission spectra of ibuprofen and caffeine in different excitation wavelengths. The mixture of these compounds was resolved by multivariate curve resolution coupled with alternative least squares (MCR-ALS on constructed matrix. The EEM spectra were recorded at excitation wavelengths from 250-275 nm; the emission wavelengths ranged from 275-400 nm. For each particular quantitative determination, an augmented matrix was defined. The resolution of each augmented-data matrix gave an estimation of the excitation and emission spectra of the species included in the model. Ibuprofen and caffeine were determined in concentration range from 0.10-8.00 and 0.50-15.00 mg ml-1, respectively. The minimal sample pretreatment and relatively low running cost, make this method a good alternative to existing methods for determination of the analytes in urine samples.

  13. Simultaneous determination of ethanol's four types of non-oxidative metabolites in human whole blood by liquid chromatography tandem mass spectrometry

    DEFF Research Database (Denmark)

    Zhang, Xinyu; Zheng, Feng; Lin, Zebin

    2017-01-01

    The importance of ethanol non-oxidative metabolites as the specific biomarkers of alcohol consumption in clinical and forensic settings is increasingly acknowledged. Simultaneous determination of these metabolites can provide a wealth of information like drinking habit and history, but it was dif......The importance of ethanol non-oxidative metabolites as the specific biomarkers of alcohol consumption in clinical and forensic settings is increasingly acknowledged. Simultaneous determination of these metabolites can provide a wealth of information like drinking habit and history...

  14. HPTLC Fingerprint Analysis: A Quality Control for Authentication of Herbal Phytochemicals

    Science.gov (United States)

    Ram, Mauji; Abdin, M. Z.; Khan, M. A.; Jha, Prabhakar

    Authentication and consistent quality are the basic requirement for Indian traditional medicine (TIM), Chinese traditional herbal medicine (TCHM), and their commercial products, regardless of the kind of research conducted to modernize the TIM and TCHM. The complexities of TIM and TCHM challenge the current official quality control mode, for which only a few biochemical markers were selected for identification and quantitative assay. Referring too many unknown factors existed in TIM and TCHM, it is impossible and unnecessary to pinpoint qualitatively and quantitatively every single component contained in the herbal drug. Chromatographic fingerprint is a rational option to meet the need for more effective and powerful quality assessment to TIM and TCHM. The optimized chromatographic fingerprint is not only an alternative analytical tool for authentication, but also an approach to express the various pattern of chemical ingredients distribution in the herbal drugs and preserve such "database" for further multifaced sustainable studies. Analytical separation techniques, for example, high-performance liquid chromatography (HPLC), gas chromatography (GC) and mass spectrometry (MS) were among the most popular methods of choice used for quality control of raw material and finished herbal product. Fingerprint analysis approach using high-performance thin-layer chromatography (HPTLC) has become the most potent tool for quality control of herbal medicines because of its simplicity and reliability. It can serve as a tool for identification, authentication, and quality control of herbal drugs. In this chapter, attempts are being made to expand the use of HPTLC and at the same time create interest among prospective researcher in herbal analysis. The developed method can be used as a quality control tool for rapid authentication from a wide variety of herbal samples. Some examples demonstrated the role of fingerprinting in quality control and assessment.

  15. Simultaneous determination of soil density and moisture by gamma ray attenuation from Cs137 and Am241

    International Nuclear Information System (INIS)

    Barros Ferraz, E.S. de.

    1974-09-01

    The method of simultaneous bulk density and soil moisture determination by attenuation of 241 Am and 137 Cs gamma-radiation is introduced and studied with details. Theoretical considerations are made about the attenuation process in the absorbers, the form of solving the problem of two unknowns; the sensitivity of the method; the influences of the resolution time of the electronic counting equipment, and of the compton scattering in the sample. From the methodological point of view studies are made about the influence of the geometry, adjustment of counting system, choice of radiation sources, attenuation coeficients and the manner of obtaining reliable measurements. It is also presented some applications of the method, its use in soil-water movement studies, in soil profile compaction studies, and specially in swelling soils

  16. Simultaneous determination of dopamine and uric acid using layer-by-layer graphene and chitosan assembled multilayer films.

    Science.gov (United States)

    Weng, Xuexiang; Cao, Qingxue; Liang, Lixin; Chen, Jianrong; You, Chunping; Ruan, Yongmin; Lin, Hongjun; Wu, Lanju

    2013-12-15

    Multilayer films containing graphene (Gr) and chitosan (CS) were prepared on glassy carbon electrodes with layer-by-layer (LBL) assembly technique. After being characterized with cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and scanning electron microscopy (SEM), the electrochemical sensor based on the resulted films was developed to simultaneously determine dopamine (DA) and uric acid (UA). The LBL assembled electrode showed excellent electrocatalytic activity towards the oxidation of DA and UA. In addition, the self-assembly electrode possessed an excellent sensing performance for detection of DA and UA with a linear range from 0.1 μM to 140 µM and from 1.0 µM to 125 µM with the detection limit as low as 0.05 µM and 0.1 µM based on S/N=3, respectively. © 2013 Elsevier B.V. All rights reserved.

  17. Simultaneous determination of vancomycin and ceftazidime in cerebrospinal fluid in craniotomy patients by high-performance liquid chromatography.

    Science.gov (United States)

    Ye, Guangming; Cai, Xuejian; Wang, Biao; Zhou, Zhongxian; Yu, Xiaohua; Wang, Weibin; Zhang, Jiandong; Wang, Yuhai; Dong, Jierong; Jiang, Yunyun

    2008-11-04

    A simple, accurate and rapid method for simultaneous analysis of vancomycin and ceftazidime in cerebrospinal fluid (CSF), utilizing high-performance liquid chromatography (HPLC), has been developed and thoroughly validated to satisfy strict FDA guidelines for bioanalytical methods. Protein precipitation was used as the sample pretreatment method. In order to increase the accuracy, tinidazole was chosen as the internal standard. Separation was achieved on a Diamonsil C18 column (200 mm x 4.6mm I.D., 5 microm) using a mobile phase composed of acetonitrile and acetate buffer (pH 3.5) (8:92, v/v) at room temperature (25 degrees C), and the detection wavelength was 240 nm. All the validation data, such as accuracy, precision, and inter-day repeatability, were within the required limits. The method was applied to determine vancomycin and ceftazidime concentrations in CSF in five craniotomy patients.

  18. Simultaneous determination of the content of serotonin, dopamine, noradrenaline and adrenaline in pancreatic islets isolated from fed and starved mice

    Energy Technology Data Exchange (ETDEWEB)

    Hansen, S E; Hedeskov, C J [Copenhagen Univ. (Denmark)

    1977-01-01

    A highly sensitive double isotope method for the simultaneous determination of serotonin, dopamine, noradrenaline and adrenaline has been developed. Advantages and limitations of the method are discussed. The mentioned biogenic amines are all present in isolated pancreatic islet tissue from albino mice in concentrations ranging from approximately 5-30 ..mu..mol per kg wet weight (0.8-5 x 10/sup -3/ pmol/ng DNA). A somewhat higher content of these amines, especially dopamine, was found in pancreatic acinar tissue. The hypothesis that the impaired glucose-induced insulin secretion during starvation partly is caused by an increased content of biogenic amines in the pancreatic islets was not supported by our experiments which showed an unchanged islet content of these amines after 48 h starvation.

  19. Simultaneous determination of the content of serotonin, dopamine, noradrenaline and adrenaline in pancreatic islets isolated from fed and starved mice

    International Nuclear Information System (INIS)

    Hansen, S.E.; Hedeskov, C.J.

    1977-01-01

    A highly sensitive double isotope method for the simultaneous determination of serotonin, dopamine, noradrenaline and adrenaline has been developed. Advantages and limitations of the method are discussed. The mentioned biogenic amines are all present in isolated pancreatic islet tissue from albino mice in concentrations ranging from approximately 5-30 μmol per kg wet weight (0.8-5 x 10 -3 pmol/ng DNA). A somewhat higher content of these amines, especially dopamine, was found in pancreatic acinar tissue. The hypothesis that the impaired glucose-induced insulin secretion during starvation partly is caused by an increased content of biogenic amines in the pancreatic islets was not supported by our experiments which showed an unchanged islet content of these amines after 48 h starvation. (author)

  20. Simultaneous HPLC Determination of Chlordiazepoxide and Mebeverine HCl in the Presence of Their Degradation Products and Impurities

    Directory of Open Access Journals (Sweden)

    Rania N. El-Shaheny

    2015-01-01

    Full Text Available A simple, rapid, and sensitive RP-HPLC method was developed and validated for the simultaneous determination of chlordiazepoxide (CDO and mebeverine HCl (MBV in the presence of CDO impurity (2-amino-5-chlorobenzophenone, ACB and MBV degradation product (veratric acid, VER. Separation was achieved within 9 min on a BDS Hypersil phenyl column (4.5 mm × 250 mm, 5 µm particle size using a mobile phase consisting of acetonitrile: 0.1 M potassium dihydrogen phosphate: triethylamine (35 : 65 : 0.2, v/v/v in an isocratic mode at a flow rate of 1 mL/min. The pH of the mobile phase was adjusted to 4.5 with orthophosphoric acid and UV detection was set at 260 nm. A complete validation procedure was conducted. The proposed method exhibited excellent linearity over the concentration ranges of 1.0–100.0, 10.0–200.0, 2.0–40.0, and 2.0–40.0 µg/mL for CDO, MBV, VER, and ACB, respectively. The proposed method was applied for the simultaneous determination of CDO and MBV in their coformulated tablets with mean percentage recoveries of 99.75 ± 0.62 and 98.61 ± 0.38, respectively. The results of the proposed method were favorably compared with those of a comparison HPLC method using Student t-test and the variance ratio F-test. The chemical structure of MBV degradation product was ascertained by mass spectrometry and IR studies.

  1. Local activity determines functional connectivity in the resting human brain: a simultaneous FDG-PET/fMRI study.

    Science.gov (United States)

    Riedl, Valentin; Bienkowska, Katarzyna; Strobel, Carola; Tahmasian, Masoud; Grimmer, Timo; Förster, Stefan; Friston, Karl J; Sorg, Christian; Drzezga, Alexander

    2014-04-30

    Over the last decade, synchronized resting-state fluctuations of blood oxygenation level-dependent (BOLD) signals between remote brain areas [so-called BOLD resting-state functional connectivity (rs-FC)] have gained enormous relevance in systems and clinical neuroscience. However, the neural underpinnings of rs-FC are still incompletely understood. Using simultaneous positron emission tomography/magnetic resonance imaging we here directly investigated the relationship between rs-FC and local neuronal activity in humans. Computational models suggest a mechanistic link between the dynamics of local neuronal activity and the functional coupling among distributed brain regions. Therefore, we hypothesized that the local activity (LA) of a region at rest determines its rs-FC. To test this hypothesis, we simultaneously measured both LA (glucose metabolism) and rs-FC (via synchronized BOLD fluctuations) during conditions of eyes closed or eyes open. During eyes open, LA increased in the visual system, and the salience network (i.e., cingulate and insular cortices) and the pattern of elevated LA coincided almost exactly with the spatial pattern of increased rs-FC. Specifically, the voxelwise regional profile of LA in these areas strongly correlated with the regional pattern of rs-FC among the same regions (e.g., LA in primary visual cortex accounts for ∼ 50%, and LA in anterior cingulate accounts for ∼ 20% of rs-FC with the visual system). These data provide the first direct evidence in humans that local neuronal activity determines BOLD FC at rest. Beyond its relevance for the neuronal basis of coherent BOLD signal fluctuations, our procedure may translate into clinical research particularly to investigate potentially aberrant links between local dynamics and remote functional coupling in patients with neuropsychiatric disorders.

  2. A New HPLC-ELSD Method for Simultaneous Determination of N-Acetylglucosamine and N-Acetylgalactosamine in Dairy Foods

    Directory of Open Access Journals (Sweden)

    Ho Jin Kim

    2015-01-01

    Full Text Available A rapid high performance liquid chromatographic method with evaporative light scattering detection (HPLC-ELSD, using a carbohydrate column, was developed for simultaneous determination of N-acetylglucosamine (GlcNAc and N-acetylgalactosamine (GalNAc in dairy foods. Sample preparation was performed by precipitation using acetonitrile. The limits of detection were 2.097 mg/L for GlcNAc and 3.247 mg/L for GalNAc. The limits of quantification were 6.043 mg/L for GlcNAc and 9.125 mg/L for GalNAc. Accuracy ranged from 96.4 to 105.7% for GlcNAc and from 97.1 to 104.1% for GalNAc. The precision of the method was <1.7% for GlcNAc and <2.2% for GalNAc. The mean recovery of the method was measured by spiking samples with 30.0–120.0 mg/L GlcNAc or 12.5–50.0 mg/L GalNAc and was found to be 95.1–105.5% for GlcNAc and 99.5–105.9% for GalNAc. The stability test results of standard solutions stored at 4, 20, and 40°C were 96.2–104.7% for GlcNAc and 98.0–106.5% for GalNAc. This study determined GlcNAc and GalNAc in dairy foods using HPLC-ELSD method. This rapid, simultaneous quantitation method might be useful as a mean of convenient quality control of dairy foods.

  3. Simultaneous determination of sulpiride and mebeverine by HPLC method using fluorescence detection: application to real human plasma

    Directory of Open Access Journals (Sweden)

    Walash Mohamed I

    2012-02-01

    Full Text Available Abstract A new simple, rapid and sensitive reversed-phase liquid chromatographic method was developed and validated for the simultaneous determination of sulpiride (SUL and mebeverine Hydrochloride (MEB in the presence of their impurities and degradation products. The separation of these compounds was achieved within 6 min on a 250 mm, 4.6 mm i.d., 5 m particle size Waters®-C18 column using isocractic mobile phase containing a mixture of acetonitrile and 0.01 M dihydrogenphosphate buffer (45:55 at pH = 4.0. The analysis was performed at a flow rate of 1.0 mL/min with fluorescence-detection at excitation 300 nm and emission at 365 nm. The concentration-response relationship was linear over a concentration range of 10- 100 ng/mL for both MEB and SUL with a limit of detection 0.73 ng/mL and 0.85 ng/mL for MEB and SUL respectively. The proposed method was successfully applied for the analysis of both MEB and SUL in bulk with average recoveries of 100.22 ± 0.757% and 99.96 ± 0.625% respectively, and in commercial tablets with average recoveries of 100.04 ± 0.93% and 100.03 ± 0.376% for MEB and SUL respectively. The proposed method was successfully applied to the determination of MEB metabolite (veratic acid in real plasma simultaneously with SUL. The mean% recoveries (n = 3 for both MEB metabolite (veratic acid and SUL were 100.36 ± 2.92 and 99.06 ± 2.11 for spiked human plasma respectively. For real human plasma, the mean% recoveries (n = 3 were and respectively.

  4. [Simultaneous determination of ethyl carbamate and chloropropanols in flavorings by gas chromatography-triple quadrupole tandem mass spectrometry].

    Science.gov (United States)

    Xu, Xiaomin; He, Huali; Ruan, Yudi; Huang, Baifen; Zhang, Jingshun; Cai, Zengxuan; Ren, Yiping

    2013-11-01

    A simultaneous determination method for ethyl carbamate (EC) and chloropropanols (3-monochloropropane-1, 2-diol (3-MCPD) and 2-monochloropropane-1, 3-diol (2-MCPD)) in flavorings was developed by gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS). After spiked with internal standard, the sample was extracted by matrix solid-phase dispersion extraction technique with an Extrelut NT column. Hexane was used to wash the fat soluble matrix interferences and then an ethyl acetate-ethyl ether (20: 80, v/v) mixture was added to elute the analytes. The concentrated extract was detected by GC-MS/MS in multiple reaction monitoring (MRM) mode. The limits of detection (LODs) were 2, 5 and 5 microg/kg for EC, 3-MCPD and 2-MCPD, respectively. The linear ranges were 5 - 1 000 microg/kg (r = 0.9997), 10-1000 microg/kg (r = 0.999 1) and 10-1000 microg/kg (r = 0.999 5) for EC, 3-MCPD and 2-MCPD, respectively. In soy sauce, yellow rice wine, salami sauce and flavoring of instant noodle matrices, the recoveries (RSDs, n = 7) in MRM mode at the levels of 20, 100 and 400 microg/kg were 87.7%-104% (4.3%-10.7%), 90.1%-109% (2.6%-10.2%), and 90.9%-103% (3.0%-9.5%), respectively. EC, 3-MCPD and 2-MCPD were found in some real samples of the soy sauce, wine and flavoring of instant noodle. EC or 3-MCPD was found in some of the salami samples. The method is accurate, fast and suitable for the simultaneous determination of EC, 3-MCPD and 2-MCPD in flavorings.

  5. Micellar HPLC and derivative spectrophotometric methods for the simultaneous determination of fluconazole and tinidazole in pharmaceuticals and biological fluids.

    Science.gov (United States)

    Belal, F; Sharaf El-Din, M K; Eid, M I; El-Gamal, R M

    2014-04-01

    Micellar high-performance liquid chromatography (HPLC) and first-derivative ultraviolet spectrophotometry were used to simultaneously determine fluconazole (FLZ) and tinidazole (TNZ) in combined pharmaceutical dosage forms. The derivative procedure is based on the linear relationship between the drug concentration and the first derivative amplitudes at 220 and 288 nm for FLZ and TNZ, respectively. The calibration graphs were linear in the range of 1.5-9.0 µg/mL for FLZ and 10.0-60.0 µg/mL for TNZ. Furthermore, an HPLC procedure with ultraviolet detection at 210 nm was developed. For the HPLC procedure, good chromatographic separation was achieved using an ODS C18 column (250 × 4.6 mm i.d.). The mobile phase containing 0.15M sodium dodecyl sulphate, 0.3% triethylamine and 12% n-propanol in 0.02M orthophosphoric acid at pH 5.5 was pumped at a flow rate of 1 mL/min. Indapamide was used as an internal standard. The method showed good linearity over the concentration ranges of 1.5-30.0 and 10.0-200.0 µg/mL, with limits of detection of 0.36 and 2.70 µg/mL and limits of quantification of 1.1 and 8.2 µg/mL for FLZ and TNZ, respectively. The suggested methods were successfully applied for the simultaneous analysis of the drugs in their laboratory prepared mixture, co-formulated tablet and single dosage forms. Moreover the second method was also extended to the determination of the drugs in biological fluids.

  6. Development of the extraction method for the simultaneous determination of butyl-, phenyl- and octyltin compounds in sewage sludge.

    Science.gov (United States)

    Zuliani, Tea; Lespes, Gaetane; Milacic, Radmila; Scancar, Janez

    2010-03-15

    The toxicity and bioaccumulation of organotin compounds (OTCs) led to the development of sensitive and selective analytical methods for their determination. In the past much attention was assigned to the study of OTCs in biological samples, water and sediments, coming mostly from marine environment. Little information about OTCs pollution of terrestrial ecosystems is available. In order to optimise the extraction method for simultaneous determination of butyl-, phenyl- and octyltin compounds in sewage sludge five different extractants (tetramethylammonium hydroxide, HCl in methanol, glacial acetic acid, mixture of acetic acid and methanol (3:1), and mixture of acetic acid, methanol and water (1:1:1)), the presence or not of a complexing agent (tropolone), and the use of different modes of extraction (mechanical stirring, microwave and ultrasonic assisted extraction) were tested. Extracted OTCs were derivatised with sodium tetraethylborate and determined by gas chromatography coupled with mass spectrometer. Quantitative extraction of butyl-, phenyl- and octyltin compounds was obtained by the use of glacial acetic acid as extractant and mechanical stirring for 16h or sonication for 30 min. The limits of detection and quantification for OTCs investigated in sewage sludge were in the ng S ng(-1) range. Copyright (c) 2009 Elsevier B.V. All rights reserved.

  7. Quality evaluation of Shenmaidihuang Pills based on the chromatographic fingerprints and simultaneous determination of seven bioactive constituents.

    Science.gov (United States)

    Liu, Sifei; Zhang, Guangrui; Qiu, Ying; Wang, Xiaobo; Guo, Lihan; Zhao, Yanxin; Tong, Meng; Wei, Lan; Sun, Lixin

    2016-12-01

    In this study, we aimed to establish a comprehensive and practical quality evaluation system for Shenmaidihuang pills. A simple and reliable high-performance liquid chromatography coupled with photodiode array detection method was developed both for fingerprint analysis and quantitative determination. In fingerprint analysis, relative retention time and relative peak area were used to identify the common peaks in 18 samples for investigation. Twenty one peaks were selected as the common peaks to evaluate the similarities of 18 Shenmaidihuang pills samples with different manufacture dates. Furthermore, similarity analysis was applied to evaluate the similarity of samples. Hierarchical cluster analysis and principal component analysis were also performed to evaluate the variation of Shenmaidihuang pills. In quantitative analysis, linear regressions, injection precisions, recovery, repeatability and sample stability were all tested and good results were obtained to simultaneously determine the seven identified compounds, namely, 5-hydroxymethylfurfural, morroniside, loganin, paeonol, paeoniflorin, psoralen, isopsoralen in Shenmaidihuang pills. The contents of some analytes in different batches of samples indicated significant difference, especially for 5-hydroxymethylfurfural. So, it was concluded that the chromatographic fingerprint method obtained by high-performance liquid chromatography coupled with photodiode array detection associated with multiple compounds determination is a powerful and meaningful tool to comprehensively conduct the quality control of Shenmaidihuang pills. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Simultaneous Determination of Multi-Mycotoxins in Cereal Grains Collected from South Korea by LC/MS/MS

    Directory of Open Access Journals (Sweden)

    Dong-Ho Kim

    2017-03-01

    Full Text Available An improved analytical method compared with conventional ones was developed for simultaneous determination of 13 mycotoxins (deoxynivalenol, nivalenol, 3-acetylnivalenol, aflatoxin B1, aflatoxin B2, aflatoxin G1, aflatoxin G2, fumonisin B1, fumonisin B2, T-2, HT-2, zearalenone, and ochratoxin A in cereal grains by liquid chromatography-tandem mass spectrometry (LC/MS/MS after a single immunoaffinity column clean-up. The method showed a good linearity, sensitivity, specificity, and accuracy in mycotoxin determination by LC/MS/MS. The levels of 13 mycotoxins in 5 types of commercial grains (brown rice, maize, millet, sorghum, and mixed cereal from South Korea were determined in a total of 507 cereal grains. Mycotoxins produced from Fusarium sp. (fumonisins, deoxynivalenol, nivalenol, and zearalenone were more frequently (more than 5% and concurrently detected in all cereal grains along with higher mean levels (4.3–161.0 ng/g in positive samples than other toxins such as aflatoxins and ochratoxin A (less than 9% and below 5.2 ng/g in positive samples from other fungal species.

  9. Simultaneous determination of arterial input function of the internal carotid and middle cerebral arteries for dynamic susceptibility contrast MRI

    International Nuclear Information System (INIS)

    Scholdei, R.; Wenz, F.; Fuss, M.; Essig, M.; Knopp, M.V.

    1999-01-01

    Purpose: The determination of the arterial input function (AIF) is necessary for absolute quantification of the regional cerebral blood volume and blood flow using dynamic susceptibility contrast MRI. The suitability of different vessels (ICA-internal carotid artery, MCA-middle cerebral artery) for AIF determination was compared in this study. Methods: A standard 1.5 T MR system and a simultaneous dual FLASH sequence (TR/TE1/TE2/α=32/15/25/10 ) were used to follow a bolus of contrast agent. Slice I was chosen to cut the ICA perpendicularly. Slice II included the MCA. Seventeen data sets from ten subjects were evaluated. Results: The number of AIF-relevant pixels, the area under the AIF and the maximum concentration were all lower when the AIF was determined from the MCA compared to the ICA. Additionally, the mean transit time (MTT) and the time to maximum concentration (TTM) were longer in the MCA, complicating the computerized identification of AIF-relevant pixels. Data from one subject, who was examined five times, demonstrated that the intraindividual variance of the measured parameters was markedly lower than the interpersonal variance. Conclusions: It appears to be advantageous to measure the AIF in the ICA rather than the MCA. (orig.) [de

  10. Simultaneous preconcentration of Cu, Fe and Pb as methylthymol blue complexes on naphthalene adsorbent and flame atomic absorption determination

    International Nuclear Information System (INIS)

    Pourreza, Nahid; Hoveizavi, Reza

    2005-01-01

    A simultaneous preconcentration method was developed for determination of trace amounts of Cu, Fe and Pb by atomic absorption spectrometry. The method is based on the retention of their methylthymol blue complexes by naphthalene methyltrioctyl ammonium chloride adsorbent in a column. The adsorbed metal complexes were eluted from the column with nitric acid and Cu, Fe and Pb were determined by flame atomic absorption spectrometry. Several parameters such as pH of the sample solution, ligand concentration, volume of the sample and the amount of methyltrioctyl ammonium chloride loaded on naphthalene were evaluated. The effect of diverse ions on the preconcentration was also investigated. A preconcentration factor of up to 100 or more can easily be achieved depending on the volume of the sample taken. The calibration graphs were obtained in the range of 5-40, 10-100 and 10-200 ng ml -1 for Cu, Fe and Pb in the initial solution, respectively, when using 500 ml of the solution. The detection limit based on three standard deviations of the blank was 0.54, 3.1, and 4.5 ng ml -1 for Cu, Fe and Pb, respectively. The relative standard deviations (R.S.D.) of 0.62-1.4% for Cu, 1.9-3.4% for Fe and 1.0-2.2% for Pb were obtained. The method was applied to the determination of Cu, Fe and Pb in river and wastewater samples

  11. Simultaneous Determination of Hormonal Residues in Treated Waters Using Ultrahigh Performance Liquid Chromatography-Tandem Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Rayco Guedes-Alonso

    2013-01-01

    Full Text Available In the last years, hormone consumption has increased exponentially. Because of that, hormone compounds are considered emerging pollutants since several studies have determinted their presence in water influents and effluents of wastewater treatment plants (WWTPs. In this study, a quantitative method for the simultaneous determination of oestrogens (estrone, 17β-estradiol, estriol, 17α-ethinylestradiol, and diethylstilbestrol, androgens (testosterone, and progestogens (norgestrel and megestrol acetate has been developed to determine these compounds in wastewater samples. Due to the very low concentrations of target compounds in the environment, a solid phase extraction procedure has been optimized and developed to extract and preconcentrate the analytes. Determination and quantification were performed by ultrahigh performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS. The method developed presents satisfactory limits of detection (between 0.15 and 9.35 ng·L−1, good recoveries (between 73 and 90% for the most of compounds, and low relative standard deviations (under 8.4%. Samples from influents and effluents of two wastewater treatment plants of Gran Canaria (Spain were analyzed using the proposed method, finding several hormones with concentrations ranged from 5 to 300 ng·L−1.

  12. Simultaneous Determination of Tizanidine, Nimesulide, Aceclofenac and Paracetamol in Tablets and Biological Fluids Using Micellar Liquid Chromatography.

    Science.gov (United States)

    Belal, Fathalla; Omar, Mahmoud A; Derayea, Sayed; Hammad, Mohamed A; Zayed, Sahar; Saleh, Safaa F

    2018-03-01

    A simple, sensitive and rapid micellar liquid chromatographic method was developed and validated for simultaneous determination of four drugs, namely, paracetamol (PAR), tizanidine (TZD), aceclofenac (ACF) and nimesulide (NMD). Good chromatographic separation was achieved using Cyano column and micellar mobile phase consisting of 120 mM sodium dodecyl sulfate, 25 mM phosphate buffer and 10% (V/V) butanol. The pH was adjusted to three using phosphoric acid. The total retention time was below 10 min. The analysis was performed at a flow rate of 1 mL/min and a column temperature of 40°C with direct UV detection at 230 nm. Diclofenac sodium was used as the internal standard. The proposed method was validated according to the ICH guidelines and was successfully applied to the analysis of these drugs in their tablet dosage forms with high accuracy. Limits of detection were found to be 0.03, 0.07, 0.033 and 0.11 μg/mL for PAR, ACF, TZD and NMD, respectively. The high sensitivity of developed method permitted its application to the in-vitro determination of the cited drugs in spiked human plasma and urine samples, and the obtained results were satisfactory. However, PAR could not be determined in spiked human urine because its peak overlapped with that of the urine peak.

  13. Simultaneous determination of antiretroviral drugs in human hair with liquid chromatography-electrospray ionization-tandem mass spectrometry.

    Science.gov (United States)

    Wu, Yan; Yang, Jin; Duan, Cailing; Chu, Liuxi; Chen, Shenghuo; Qiao, Shan; Li, Xiaoming; Deng, Huihua

    2018-04-15

    The determination of the concentrations of antiretroviral drugs in hair is believed to be an important means for the assessment of the long-term adherence to highly active antiretroviral therapy. At present, the combination of tenofovir, lamivudine and nevirapine is widely used in China. However, there was no research reporting simultaneous determination of the three drugs in hair. The present study aimed to develop a sensitive method for simultaneous determination of the three drugs in 2-mg and 10-mg natural hair (Method 1 and Method 2). Hair samples were incubated in methanol at 37 °C for 16 h after being rinsed with methanol twice. The analysis was performed on high performance liquid chromatography tandem mass spectrometry with electronic spray ionization in positive mode and multiple reactions monitoring. Method 1 and Method 2 showed the limits of detection at 160 and 30 pg/mg for tenofovir, at 5 and 6 pg/mg for lamivudine and at 15 and 3 pg/mg for nevirapine. The two methods showed good linearity with the square of correlation coefficient >0.99 at the ranges of 416-5000 and 77-5000 pg/mg for tenofovir, 12-5000 and 15-5000 pg/mg for lamivudine and 39-50,000 and 6-50,000 pg/mg for nevirapine. They gave intra-day and inter-day coefficient of variation <15% and the recoveries ranging from 80.6 to 122.3% and from 83.1 to 114.4%. Method 2 showed LOD and LOQ better than Method 1 for tenofovir and nevirapine and matched Method 1 for lamivudine, but there was high consistency between them in the determination of the three drugs in hair. The population analysis with Method 2 revealed that the concentrations in hair were decreased with the distance of hair segment away from the scalp for the three antiretroviral drugs. Copyright © 2018 Elsevier B.V. All rights reserved.

  14. Simultaneous determination of borate, chloride and molybdate in pyrohydrolysis distillates of plant and soil samples by ion chromatography.

    Science.gov (United States)

    Mishra, Vivekchandra Guruprasad; Das, Mrinal Kanti; Shah, Dipti Jayesh; Jeyakumar, Subbiah; Tomar, Bhupendra Singh; Ramakumar, Karanam Lakshminarayana

    2018-01-12

    Determination of concentrations of micronutrients in plant samples is important in order to assess the growth and quality of plants. An ion chromatography (IC) method was developed for the simultaneous determination of B, Cl and Mo (micronutrients present in their anionic form in aqueous samples) using a gradient elution with d-mannitol and NaOH. Despite their different chemical nature, these elements could be separated from the matrix by employing pyrohydrolysis. IC was employed for their sequential determination from single aliquot injection into the IC column. It was observed that the optimised procedures developed earlier in our laboratory for the separation of B and halogens using d-Mannitol-NaOH or bicarbonate eluents could not be extended to B-Mo-Cl separation. The concentration levels of d-mannitol in the eluent required for separation of boron impeded the conductivity detection of Mo and the peak sensitivity was seen to be critically dependent on d-mannitol concentration in the eluent. In addition, d-mannitol in NaOH eluent altered the retention times of analytes (B, F - , Cl - , NO 3 - , SO 4 2- and MoO 4 2- ) which were not observed in the case of bicarbonate eluent. The current study deals with the investigation on the influence of d-mannitol on the molybdate as well as its role on the retention time. Formation of Mo-mannitol complex at different pH conditions and de-protonation of mannitol were correlated to the observed effects. Based on the observations, a gradient elution method was proposed for the simultaneous separation and determination of B, Cl and Mo in the pyrohydrolysis distillates of plant samples. The method was calibrated for B (0.05-1 mg/L), Cl (0.1-10 mg/L) and Mo (0.5-10 mg/L) and the linear regression coefficients obtained were 0.9992, 0.9998 and 0.997 respectively. The limit of detection (LOD) for B, Cl and Mo was calculated to be 19, 23 and 96 μg/L, respectively. The developed IC method after pyrohydrolytic separation of B

  15. Gradient high performance liquid chromatography method for simultaneous determination of ilaprazole and its related impurities in commercial tablets

    Directory of Open Access Journals (Sweden)

    Shang Wang

    2015-04-01

    Full Text Available A methodology (HPLC proposed in this paper for simultaneously quantitative determination of ilaprazole and its related impurities in commercial tablets was developed and validated. The chromatographic separation was carried out by gradient elution using an Agilent C8 column (4.6 mm × 250 mm, 5 μm which was maintained at 25 °C. The mobile phase composed of solvent A (methanol and solvent B (solution consisting 0.02 mmol/l monopotassium phosphate and 0.025 mmol/l sodium hydroxide was at a flow rate of 1.0 ml/min. The samples were detected and quantified at 237 nm using an ultraviolet absorbance detector. Calibration curves of all analytes from 0.5 to 3.5 μg/ml were good linearity (r ≥ 0.9990 and recovery was greater than 99.5% for each analyte. The lower limit of detection (LLOD and quantification (LOQ of this analytical method were 10 ng/ml and 25 ng/ml for all impurities, respectively. The stress studies indicated that the degradation products could not interfere with the detection of ilaprazole and its related impurities and the assay can thus be considered stability-indicating. The method precisions were in the range of 0.41–1.21 while the instrument precisions were in the range of 0.38–0.95 in terms of peak area RSD% for all impurities, respectively. This method is considered stability-indicating and is applicable for accurate and simultaneous measuring of the ilaprazole and its related impurities in commercial enteric-coated tablets.

  16. Monolayer covalent modification of 5-hydroxytryptophan on glassy carbon electrodes for simultaneous determination of uric acid and ascorbic acid

    International Nuclear Information System (INIS)

    Lin Xiangqin; Li Yongxin

    2006-01-01

    5-Hydroxytryptophan (5-HTP) was covalently grafted on the surface of glassy carbon electrodes (GCEs) using cyclic voltammetric method in a phosphate buffer solution. The prepared electrode, denoded as 5-HTP/GCE, was characterized by X-ray photoelectron spectroscopy, cyclic voltammetry and differential pulse voltammetry (DPV). Tryptophan grafted GCE (TRP/GCE) and 5-hydroxytryptamine grafted GCE (5-HTP/GCE) were also prepared by the same method for comparison. It was found that the electrocatalytic activities toward the oxidation of uric acid (UA) and ascorbic acid (AA) was in the order of 5-HT/GCE > 5-HTP/GCE > TRP/GCE for UA oxidation and 5-HT/GCE 5-HTP/GCE > TRP/GCE for AA oxidation. However, the CV current sensitivity was estimated as 4:2:1 for 5-HTP/GCE:5-HT/GCE:TRP/GCE. The DPV peaks for UA and AA oxidation appeared at 0.07 V and 0.34 V versus SCE, respectively, allowing simultaneous determination in mixtures. A linearly response in the range of: 5.0 x 10 -7 to 1.1 x 10 -5 M with the detection limit (s/n = 3) of 2.8 x 10 -7 M for UA determination, and a linear response in the range of: 5.0 x 10 -6 to 1.0 x 10 -4 M with the detection limit of 4.2 x 10 -6 M for AA determination were obtained. This electrode was used for UA and AA determinations in human urine samples satisfactorily

  17. [Simultaneous determination of 15 industrial synthetic dyes in condiment by solid phase extraction-high performance liquid chromatography].

    Science.gov (United States)

    Liu, Min; Li, Xiaolin; Bie, Wei; Wang, Minglin; Feng, Qian

    2011-02-01

    A new method was established for the determination of 15 industrial synthetic dyes in condiment by solid phase extraction-high performance liquid chromatography (SPE-HPLC). The samples were extracted by methanol-water (1:1, v/v) and purified by a solid phase extraction column. Then, the chromatographic separation was achieved on a Luna C18 column by linear gradient elution. The mobile phase was 10 mmol/L ammonium acetate-acetonitrile (containing 1% acetic acid). The results showed that the 15 industrial synthetic dyes can be separated efficiently. The recoveries of the 15 industrial synthetic dyes spiked in condiment were between 84.6% and 114.2% with the relative standard deviations of 0.9% - 10.3%. The limits of detection of this method was 0.05 - 0.18 mg/kg for the 15 industrial synthetic dyes. The method is simple, sensitive, accurate, repeatable and can be used for simultaneous determination of the 15 illegally added industrial synthetic dyes.

  18. 242Pu as tracer for simultaneous determination of 237Np and 239,240Pu in environmental samples

    DEFF Research Database (Denmark)

    Chen, Q.J.; Dahlgaard, H.; Nielsen, S.P.

    2002-01-01

    A procedure has been developed using Pu-242 as tracer for simultaneous determination of Np-237 and Pu-239,Pu-240 in environmental samples. The validity of the method has been demonstrated by ICPMS and alpha-spectroscopy for up to 10 gram soil and sediment, seawater up to 200 litres. The paper...... from Np and Pu) R-before/R-after = 1.004 +/- 3.3% (S.D n = 20) and 1 litre seawater R-before/R-after = 1.019+/-1.9% (S.D., n = 12). Results from the intercomparison samples LAEA-135, LAEA-381 and from environmental samples are presented....... describes a suitable chemical procedure for Np and Pu including a quantitative pre-concentration of neptunium and plutonium, preparation of Np4+ and Pu4+, NP(NO3)(6)(2-) and Pu(NO3)(6)(2-), The ratio of Np-237/Pu-242 (or Np-237/Pu-239) before and after the procedure has been determined using 10 g soil (free...

  19. High-performance liquid chromatographic method for the simultaneous determination of 24 fragrance allergens to study scented products.

    Science.gov (United States)

    Villa, C; Gambaro, R; Mariani, E; Dorato, S

    2007-07-27

    The European legislation on cosmetic products has recently required the declaration of 26 compounds (24 volatile chemicals and 2 natural extracts) on the label of final products when exceeding a stipulated cut-off level. In this work a rapid reliable and specific RP-HPLC method coupled with diode array detector (DAD) has been developed for the simultaneous determination and quantification of the 24 volatile chemicals: amyl cinnamal, benzyl alcohol, cinnamyl alcohol, citral, eugenol, hydroxy-citronellal, isoeugenol, amylcinnamyl alcohol, benzyl salicylate, cinnamal, coumarin, geraniol, Lyral (hydroxy-methylpentylcyclohexene carboxaldehyde), anisyl alcohol, benzyl cinnamate, farnesol, Lilial (2-(4-tert-butylbenzyl)propionaldehyde) linalool, benzyl benzoate, citronellol, hexyl cinnamal, limonene, methylheptin carbonate, alpha-isomethyl ionone (3-methyl-4-(2,6,6-trimethyl-2-cyclohexen-1-yl)-3-buten-2-one). The 24 analytes were appropriately separated over a running time of 40 min, on a C18 column using a simple gradient elution (acetonitrile/water) with flow rate from 0.7 to 1.0 ml/min and UV acquisition at 210, 254 and 280 nm. All calibration curves showed good linearity (r2>0.99) within test ranges. The method was successfully applied to the qualitative and quantitative determination of the potential allergens in four commercial scented products, with satisfactory accuracy and precision. The results indicated that this simple and efficient method can be used for quality assessment of complex matrices such us cosmetic scented products.

  20. Simultaneous determination of six quality parameters of biodiesel through 1H NMR spectroscopy and partial least squares.

    Science.gov (United States)

    Shimamoto, Gustavo G; Tubino, Matthieu

    2018-03-01

    Biodiesel quality is checked by determining several parameters. Considering the large number of analyses in this verification, as well as the disadvantages of the use of toxic solvents and waste generation, multivariate calibration is suggested to reduce the number of tests. In this work, hydrogen nuclear magnetic resonance ( 1 H NMR) spectra were used to build multivariate models, from partial least squares (PLS), in order to perform simultaneous determination of six important quality parameters of biodiesel: density at 20°C, kinematic viscosity at 40°C, iodine value, acid number, oxidative stability, and water content. 1 H NMR spectrum reflects the structures of the compounds present in biodiesel and showed suitable correlations with the six parameters. In addition, the models were appropriate to predict all parameters for external samples. Thus, the alliance between 1 H NMR spectra and PLS was shown to be applicable to extract a lot of information about biodiesel quality, significantly reducing analysis time, reagent and solvent consumption, and waste generation. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Multi-walled Carbon Nanotubes/Graphite Nanosheets Modified Glassy Carbon Electrode for the Simultaneous Determination of Acetaminophen and Dopamine.

    Science.gov (United States)

    Zhang, Susu; He, Ping; Zhang, Guangli; Lei, Wen; He, Huichao

    2015-01-01

    Graphite nanosheets prepared by thermal expansion and successive sonication were utilized for the construction of a multi-walled carbon nanotubes/graphite nanosheets based amperometric sensing platform to simultaneously determine acetaminophen and dopamine in the presence of ascorbic acid in physiological conditions. The synergistic effect of multi-walled carbon nanotubes and graphite nanosheets catalyzed the electrooxidation of acetaminophen and dopamine, leading to a remarkable potential difference up to 200 mV. The as-prepared modified electrode exhibited linear responses to acetaminophen and dopamine in the concentration ranges of 2.0 × 10(-6) - 2.4 × 10(-4) M (R = 0.999) and 2.0 × 10(-6) - 2.0 × 10(-4) M (R = 0.998), respectively. The detection limits were down to 2.3 × 10(-7) M for acetaminophen and 3.5 × 10(-7) M for dopamine (S/N = 3). Based on the simple preparation and prominent electrochemical properties, the obtained multi-walled carbon nanotubes/graphite nanosheets modified electrode would be a good candidate for the determination of acetaminophen and dopamine without the interference of ascorbic acid.

  2. Fast Simultaneous Determination of 13 Nucleosides and Nucleobases in Cordyceps sinensis by UHPLC–ESI–MS/MS

    Directory of Open Access Journals (Sweden)

    Shi-Yu Zong

    2015-12-01

    Full Text Available A reliable ultra-high-performance liquid chromatography–electrospray ionization–tandem mass spectrometry (UHPLC–ESI–MS/MS method for the fast simultaneous determination of 13 nucleosides and nucleobases in Cordyceps sinensis (C. sinensis with 2-chloroadenosine as internal standard was developed and validated. Samples were ultrasonically extracted in an ice bath thrice, and the optimum analyte separation was performed on an ACQUITY UPLCTM HSS C18 column (100 mm × 2.1 mm, 1.8 μm with gradient elution. All targeted analytes were separated in 5.5 min. Furthermore, all calibration curves showed good linear regression (r > 0.9970 within the test ranges, and the limits of quantitation and detection of the 13 analytes were less than 150 and 75 ng/mL, respectively. The relative standard deviations (RSDs of intra- and inter-day precisions were <6.23%. Recoveries of the quantified analytes ranged within 85.3%–117.3%, with RSD < 6.18%. The developed UHPLC–ESI–MS/MS method was successfully applied to determine nucleosides and nucleobases in 11 batches of C. sinensis samples from different regions in China. The range for the total content in the analyzed samples was 1329–2057 µg/g.

  3. An isocratic HPLC method for the simultaneous determination of cholesterol, cardiolipin, and DOPC in lyophilized lipids and liposomal formulations.

    Science.gov (United States)

    Simonzadeh, Ninus

    2009-04-01

    Phospholipids, such as 1,2-dioleoyl-sn-glycero-3-phosphocholine (DOPC), and 1,1',2,2'-tetramyristoyl cardiolipin, along with cholesterol, form liposomes in aqueous media and have been investigated at NeoPharm (Lake Bluff, IL) as drug-delivery systems. To accurately assess the effectiveness of various formulations involving the use of aforementioned phospholipids and cholesterol, their quantitative determination is essential. An isocratic high-performance liquid chromatographic method for the simultaneous determination of cholesterol, cardiolipin, and DOPC in various pharmaceutical formulations containing the active drug substance has consequently been developed and is presented here. The current method utilizes an ASTEC-diol analytical column and is shown to be stability-indicating and free from interference from any of the formulation excipients, such as sucrose, sodium chloride, and sodium lactate. The analytes are detected using an evaporative light scattering detector (Alltech or Polymer Laboratories). The quantitation of each lipid component is performed using non-linear regression analysis. The retention characteristics of the analytes are examined as a function of eluent composition (e.g., pH, salt content, organic to aqueous phase ratio) and column temperature. The method was validated and was found to be sensitive, specific, rugged, and cost-effective. The current method provides enhanced chromatographic separation for lipid components as well as degradation products as compared to similar methods reported in the literature. It is also inherently simpler than other similar methods reported in the literature that typically use complex gradient elution.

  4. Simultaneous identification/determination system for phentolamine and sildenafil as adulterants in soft drinks advertising roborant nutrition.

    Science.gov (United States)

    Mikami, Eiichi; Ohno, Tsutomu; Matsumoto, Hiroshi

    2002-12-04

    An easily available, simultaneous identification/determination procedure for phentolamine (PHE) and sildenafil (SIL) in adulterated dietary supplements was established by using a combination of three different analytical methods; thin-layer chromatography (TLC), liquid chromatography-mass spectrometry (LC/MS) and a high-performance liquid chromatography (HPLC)/photo-diode-array. The sample solution for TLC was applied to silica gel 60 F(254) plates with chloroform/ammonia solution (28)/methanol (70:5:3, lower layer) and chloroform/diethylamine/methanol (15:3:2) as the developing solvent. Spots were located under UV radiation at 254 nm. Mass spectra of PHE and SIL by LC/MS were investigated with electrospray ionization (ESI) interface, under both positive and negative ion mode. The HPLC analysis was performed on a column of Wakosil 5C18 (4.6 mm x 150 mm, 5 microm) with water/methanol/acetonitrile/triethylamine (580:250:170:1) adjusted with phosphoric acid to pH 3.0 as the mobile phase, and the effluent was monitored with a photo-diode-array detector. Quantitative HPLC analysis of PHE and SIL were detected at 280 nm. When this procedure was applied to commercial soft drinks, PHE and SIL were identified and determined at a concentration of 17 mg PHE and 44 mg SIL per bottle, respectively. The procedure described here is available for the screening of PHE and SIL in adulterated supplements. Copyright 2002 Elsevier Science Ireland Ltd.

  5. Net analyte signal standard addition method for simultaneous determination of sulphadiazine and trimethoprim in bovine milk and veterinary medicines.

    Science.gov (United States)

    Hajian, Reza; Mousavi, Esmat; Shams, Nafiseh

    2013-06-01

    Net analyte signal standard addition method has been used for the simultaneous determination of sulphadiazine and trimethoprim by spectrophotometry in some bovine milk and veterinary medicines. The method combines the advantages of standard addition method with the net analyte signal concept which enables the extraction of information concerning a certain analyte from spectra of multi-component mixtures. This method has some advantages such as the use of a full spectrum realisation, therefore it does not require calibration and prediction step and only a few measurements require for the determination. Cloud point extraction based on the phenomenon of solubilisation used for extraction of sulphadiazine and trimethoprim in bovine milk. It is based on the induction of micellar organised media by using Triton X-100 as an extraction solvent. At the optimum conditions, the norm of NAS vectors increased linearly with concentrations in the range of 1.0-150.0 μmolL(-1) for both sulphadiazine and trimethoprim. The limits of detection (LOD) for sulphadiazine and trimethoprim were 0.86 and 0.92 μmolL(-1), respectively. Copyright © 2012 Elsevier Ltd. All rights reserved.

  6. Fast simultaneous determination of trimethoprim and sulfamethoxazole by capillary zone electrophoresis with capacitively coupled contactless conductivity detection.

    Science.gov (United States)

    da Silva, Iranaldo Santos; Vidal, Denis Tadeu Rajh; do Lago, Claudimir Lucio; Angnes, Lúcio

    2013-04-01

    The association of trimethoprim and sulfamethoxazole is a very effective with antibiotic properties, and commonly used in the treatment of a variety of infections. Due to the importance in diseases treatment of humans and also of animals, the development of methods for their quantification in commercial formulations is highly desirable. In the present study, a rapid method for simultaneous determination of these compounds using CE with capacitively coupled contactless conductivity detection was developed. A favorable working region for both analytes was from 12.5 to 200 μmol/L (linear responses with R > 0.999 for N = 5). Other parameters calculated were sensitivity (1.28 ± 0.10/1.45 ± 0.11) min/(μmol L), RSD (4.5%/2.0%), and LOD (1.1/3.3) μmol/L for trimethoprim and sulfamethoxazole, respectively. Under this condition, the total run time was only 2.6 min. The proposed method was applied to the determination of trimethoprim and sulfamethoxazole in commercial samples and the results were compared to those obtained by using a HPLC pharmacopoeia method. This new method is advantageous for quality-control analyses of trimethoprim and sulfamethoxazole in pharmaceuticals samples, because it is rapid and precise. Moreover, it is less laborious and demands minimum amounts of reagents in comparison to the recommended method. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. A glassy carbon electrode modified with cerium phosphate nanotubes for the simultaneous determination of hydroquinone, catechol and resorcinol.

    Science.gov (United States)

    Li, Zhen; Yue, Yuhua; Hao, Yanjun; Feng, Shun; Zhou, Xianli

    2018-03-12

    A nafion film containing cerium phosphate nanotubes was pasted onto a glassy carbon electrode (GCE) to obtain a sensor for hydroquinone (HQ). The morphologies and components of the coating were characterized by transmission electron microscopy, scanning electron microscopy and energy-dispersive spectroscopy. Cyclic voltammetry and differential pulse voltammetry (DPV) showed the specific surface of the electrode to be significantly increased and the electron transfer rate to be accelerated. The modified GCE was applied to the determination of hydroquinone (HQ) via DPV. The oxidation current increases linearly in the 0.23 μM to 16 mM HQ concentration range which is as wide as five orders of magnitude. The limit of detection is 0.12 μM (based on a signal-to-noise ratio of 3), and the sensitivity is 1.41 μA·μM -1  cm -2 . The method was further applied to the simultaneous determination of HQ, catechol and resorcinol. The potentials for the three species are well separated (20, 134, and 572 mV vs SCE). Average recoveries from (spiked) real water samples are between 95.2 and 107.0%, with relative standard deviations of 0.9~2.7% (for n = 3) at three spiking levels. The method was validated by independent assays using HPLC. Graphical abstract ᅟ.

  8. GC electrode modified with carbon nanotubes and NiO for the simultaneous determination of bisphenol A, hydroquinone and catechol

    International Nuclear Information System (INIS)

    Goulart, Lorena Athie; Mascaro, Lucia Helena

    2016-01-01

    This work reports the electrochemical determination of bisphenol A (BPA), hydroquinone (HQ) and catechol (CC) using glassy carbon electrode (GCE) modified with multi-walled carbon nanotubes (MWCNT) and nickel oxide nanoparticles (NiO). MWCNT were functionalized with sulfonitric solution (3H 2 SO 4 :1HNO 3 ) and dispersed in dimethylformamide for the MWCNT/GCE manufacturing. The MWCNT/GCE was modified with NiO using cyclic potential in pH 4 maintained by an acetate buffer solution containing 0.008 mol L −1 of nickel nitrate. The concentration of the nickel solution and the number of cycles in the electrodeposition were studied. Morphological characterization of NiO/MWCNT/GCE was carried out by scanning electron microscopy and the presence of NiO was observed. The electrochemical behavior was evaluated by cyclic voltammetry and electrochemical impedance spectroscopy using BPA solution and the results were compared with those of GCE. The NiO/MWCNT/GCE presented the lowest charge transfer resistance. The electrochemical detection of BPA, HQ and CC was developed using differential pulse voltammetry. The analytical curves showed an excellent linear response and the detection limits for the simultaneous determination of BPA, HQ and CC were 2.8 × 10 −8 mol L −1 , 2.70 × 10 −8 mol L −1 and 5.9 × 10 −8 mol L −1 , respectively.

  9. Simultaneous determination of some ultraviolet-absorbing chemicals in sunscreen cosmetics using a high-performance liquid chromatography method.

    Science.gov (United States)

    Liu, T; Wu, D

    2011-10-01

    A method of gradient elution high-performance liquid chromatography (HPLC) for simultaneous determination of 11 different ultraviolet-absorbing chemicals of phenylbenzlmldazole sulphonic acid, 4-aminobenzoic acid, benzophenone-4, benzophenone-3, isoamyl p-methoxycinnamate, 4-methylbenzylidene camphor, octocrylene, ethylhexyl methoxycinnamate, homosalate, ethylhexyl salicylate, methylene bis-benzotriazolyl tetramethylbutyl phenol was developed for the application to sunscreen cosmetic products. In this study, an Agilent SB-C18 analytical column (250 × 4.6 mm, 5 μm) was utilized and methanol, tetrahydrofuran and perchloric acid aqueous solution (0.2 mL HClO(4) + 300 mL H(2)O) were used for gradient elution at a total flow rate of 1.0 mL min(-1). The optimum conditions for 11 different ultraviolet-absorbing chemicals analyses were investigated. All calibration curves showed good linear regression with UV detection (311 nm) within test ranges. The correlation coefficients were better than 0.999 in all cases. The assay was simple, selective, convenient and reproducible and is suitable for the determination of ultraviolet-absorbing chemicals in commercial sunscreen cosmetic products. The use frequency of 11 different ultraviolet absorbents in 100 sunscreen cosmetics was investigated and statistically analysed. The ultraviolet absorbent of maximum use frequency was ethylhexyl methoxycinnamate. © 2011 The Authors. ICS © 2011 Society of Cosmetic Scientists and the Société Française de Cosmétologie.

  10. A rapid method for simultaneously determining ethanol and methanol content in wines by full evaporation headspace gas chromatography.

    Science.gov (United States)

    Zhang, Chun-Yun; Lin, Neng-Biao; Chai, Xin-Sheng; Zhong-Li; Barnes, Donald G

    2015-09-15

    This work reports on a full evaporation headspace gas chromatographic (FE HS-GC) method for simultaneously determining the ethanol (EtOH) and methanol (MeOH) content in wines. A small sample (10μL) was placed in a headspace sample vial, and a near-complete mass transfer of ethanol and methanol from the liquid sample to the vapor phase was obtained within three minutes at a temperature of 105°C, which allowed the measurement of the EtOH and MeOH content in the sample by GC. The results showed excellent precision and accuracy, as shown by the reproducibilities of 1.02% and 2.11% for EtOH and MeOH, respectively, and recoveries that ranged from 96.1% to 104% for both alcohols. The method is efficient, accurate and suitable for the determination of EtOH and MeOH in wine production and quality control. Copyright © 2015 Elsevier Ltd. All rights reserved.

  11. A novel UHPLC method for the rapid and simultaneous determination of daidzein, genistein and equol in human urine.

    Science.gov (United States)

    Redruello, Begoña; Guadamuro, Lucía; Cuesta, Isabel; Álvarez-Buylla, Jorge R; Mayo, Baltasar; Delgado, Susana

    2015-11-15

    This work reports on a novel method involving reverse-phased ultra-high performance liquid chromatography (UHPLC) plus a spectrophotometric photodiode array/fluorescence (FLR) detection system for determining the concentration of equol and major soy isoflavones (daidzein and genistein) in human urine. The proposed method was validated in terms of its linearity, sensitivity, accuracy (recovery) and precision (intra- and inter-day repeatability). The isoflavone profiles of urine samples from a group of menopausal women following oral soy isoflavone supplementation were determined and compared. Screening for equol-producer status was accomplished with high sensitivity (detection limit of the FLR detector 2.93nM). The method involves a short chromatographic run time compared to conventional HPLC methods while allowing for the simultaneous and reliable quantification of daidzein, genistein and equol in human urine. It also allows for the rapid screening of multiple urine samples when testing for equol production status and checking patient adherence to isoflavone treatment regimens. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. Rapid and simple micromethod for the simultaneous determination of 3-MCPD and 3-MCPD esters in different foodstuffs.

    Science.gov (United States)

    Küsters, Markus; Bimber, Ute; Ossenbrüggen, Alexandra; Reeser, Sebastian; Gallitzendörfer, Rainer; Gerhartz, Michael

    2010-06-09

    This paper describes for the first time a micromethod for the simultaneous determination of 3-monochloropropane-1,2-diol (3-MCPD) and fatty acid esters of 3-MCPD (3-MCPD esters) in different foodstuffs. 3-MCPD and 3-MCPD esters were isolated from food products using a single extraction step separating hydrophilic and lipophilic compounds. An aliquot of the aqueous layer was analyzed for the content of 3-MCPD while a part of the organic layer was analyzed for 3-MCPD esters after cleavage with sodium methoxide. After a simple derivatization procedure with phenylboronic acid (PBA), the determination was achieved by isotope dilution GC-MS using isotope-labeled 3-MCPD and 3-MCPD ester as internal standards. The method was validated for various foodstuffs like bakery products, meat and fish products, and soups as well as seasonings with LOD of 1-2 microg/kg (3-MCPD) and 6 microg/kg (3-MCPD esters), respectively. Recoveries ranged within 95 +/- 9% and 96 +/- 10% at spiking levels of 15 and 25 microg/kg in all matrices for 3-MCPD and 84 +/- 9% and 85 +/- 7% at spiking levels of 0.05 mg/kg and 2 mg/kg for 3-MCPD esters. The method avoids tedious and laborious sample preparation and was successfully applied to the rapid screening of samples conforming to the EU performance criteria for methods of analysis for 3-MCPD.

  13. Development of a multiple immunoaffinity column for simultaneous determination of multiple mycotoxins in feeds using UPLC-MS/MS.

    Science.gov (United States)

    Hu, Xiaofeng; Hu, Rui; Zhang, Zhaowei; Li, Peiwu; Zhang, Qi; Wang, Min

    2016-09-01

    A sensitive and specific immunoaffinity column to clean up and isolate multiple mycotoxins was developed along with a rapid one-step sample preparation procedure for ultra-performance liquid chromatography-tandem mass spectrometry analysis. Monoclonal antibodies against aflatoxin B1, aflatoxin B2, aflatoxin G1, aflatoxin G2, zearalenone, ochratoxin A, sterigmatocystin, and T-2 toxin were coupled to microbeads for mycotoxin purification. We optimized a homogenization and extraction procedure as well as column loading and elution conditions to maximize recoveries from complex feed matrices. This method allowed rapid, simple, and simultaneous determination of mycotoxins in feeds with a single chromatographic run. Detection limits for these toxins ranged from 0.006 to 0.12 ng mL(-1), and quantitation limits ranged from 0.06 to 0.75 ng mL(-1). Concentration curves were linear from 0.12 to 40 μg kg(-1) with correlation coefficients of R (2) > 0.99. Intra-assay and inter-assay comparisons indicated excellent repeatability and reproducibility of the multiple immunoaffinity columns. As a proof of principle, 80 feed samples were tested and several contained multiple mycotoxins. This method is sensitive, rapid, and durable enough for multiple mycotoxin determinations that fulfill European Union and Chinese testing criteria.

  14. HPTLC analysis of hepatoprotective diterpenoid andrographolide from Andrographis paniculata nees (kalmegh)

    OpenAIRE

    Raina Archana; Kumar A; Pareek S

    2007-01-01

    A rapid, accurate and simple high performance thin layer chromatography method for quantitative estimation of andrographolide in Andrographis paniculata is described here. The assay combines separation of andrographolide on silica gel 60 F 254 HPTLC plates followed by scanning of the spots at 232 nm using a Camag Scanner 3. Thirty germplasm collections of Andrographis paniculata were evaluated for andrographolide content by this method. Andrographolide content ranged from 1.14% to...

  15. HPTLC-FLD-SERS as a facile and reliable screening tool: Exemplarily shown with tyramine in cheese

    Directory of Open Access Journals (Sweden)

    Liao Wang

    2018-04-01

    Full Text Available The serious cytotoxicity of tyramine attracted marked attention as it induced necrosis of human intestinal cells. This paper presented a novel and facile high performance thin-layer chromatography (HPTLC method tailored for screening tyramine in cheese. Separation was performed on glass backed silica gel plates, using methanol/ethyl acetate/ammonia (6/4/1 v/v/v as the mobile phase. Special efforts were focused on optimizing conditions (substrate preparation, laser wavelength, salt types and concentrations of surface enhanced Raman spectroscopy (SERS measurements directly on plates after derivatization, which enabled molecule-specific identification of targeted bands. In parallel, fluorescent densitometry (FLD scanning at 380HPTLC-FLD-SERS provided a new horizon in fast and reliable screening of sophisticated samples like food and herb drugs, striking an excellent balance between specificity, sensitivity and simplicity. Keywords: FLD, HPTLC, SERS, Screening, Tyramine

  16. Simultaneous determination of 15 phenolic constituents of Chinese black rice wine by HPLC-MS/MS with SPE.

    Science.gov (United States)

    Wang, Yutang; Liu, Yuanyuan; Xiao, Chunxia; Liu, Laping; Hao, Miao; Wang, Jianguo; Liu, Xuebo

    2014-06-01

    This study established a new method for quantitative and qualitative determination of certain components in black rice wine, a traditional Chinese brewed wine. Specifically, we combined solid-phase extraction and high-performance liquid chromatography (HPLC) with triple quadrupole mass spectrometry (MS/MS) to determine 8 phenolic acids, 3 flavonols, and 4 anthocyanins in black rice wine. First, we clean samples with OASIS HLB cartridges and optimized extraction parameters. Next, we performed separation on a SHIM-PACK XR-ODS column (I.D. 3.0 mm × 75 mm, 2.2 μm particle size) with a gradient elution of 50% aqueous acetonitrile (V/V) and water, both containing 0.2% formic acid. We used multiple-reaction monitoring scanning for quantification, with switching electrospray ion source polarity between positive and negative modes in a single chromatographic run. We detected 15 phenolic compounds properly within 38 min under optimized conditions. Limits of detection ranged from 0.008 to 0.030 mg/L, and average recoveries ranged from 60.8 to 103.1% with relative standard deviation ≤8.6%. We validated the method and found it to be sensitive and reliable for quantifying phenolic compounds in rice wine matrices. This study developed a new, reliable HPLC-MS/MS method for simultaneous determination of 15 bioactive components in black rice wine. This method was validated and found to be sensitive and reliable for quantifying phenolic compounds in rice wine. © 2014 Institute of Food Technologists®

  17. UHPLC-PDA Assay for Simultaneous Determination of Vitamin D3 and Menaquinone-7 in Pharmaceutical Solid Dosage Formulation

    Directory of Open Access Journals (Sweden)

    Muhammad Jehangir

    2017-01-01

    Full Text Available A newly developed method based on ultrahigh performance liquid chromatography (UHPLC was optimized for the simultaneous determination of vitamin D3 and menaquinone-7 (MK-7 in tablet formulation in the present study. UHPLC separation of vitamin D3 and MK-7 was performed with ACE Excel 2 C18-PFP column (2 μm, 2.1 × 100 mm at 0.6 mL min−1 flow rate, whereas the mobile phase consisted of methanol/water (19:1, v/v, phase A and isopropyl alcohol (99.9%, phase B containing 0.5% triethylamine. Isocratic separation of both the analytes was performed at 40°C by pumping the mobile phases A and B in the ratio of 50:50 (v/v, pH, 6.0. Both analytes were detected at a wavelength of 265 nm and the injection volume was 1.0 μL. The overall runtime per sample was 4.5 min with retention time of 1.26 and 3.64 min for vitamin D3 and MK-7, respectively. The calibration curve was linear from 5.0 to 100 μg mL−1 for vitamin D3 and MK-7 with a coefficient of determination (R2 ≥ 0.9981, while repeatability and reproducibility (expressed as relative standard deviation were lower than 1.46 and 2.21%, respectively. The proposed HPLC method was demonstrated to be simple and rapid for the determination of vitamin D3 and MK-7 in tablets.

  18. A novel method to determine simultaneously methane production during in vitro gas production using fully automated equipment

    NARCIS (Netherlands)

    Pellikaan, W.F.; Hendriks, W.H.; Uwimanaa, G.; Bongers, L.J.G.M.; Becker, P.M.; Cone, J.W.

    2011-01-01

    An adaptation of fully automated gas production equipment was tested for its ability to simultaneously measure methane and total gas. The simultaneous measurement of gas production and gas composition was not possible using fully automated equipment, as the bottles should be kept closed during the

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

    Directory of Open Access Journals (Sweden)

    Shi-Ying Dai

    2013-12-01

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

  20. Flow-Injection Solid Phase Partial Least-Squares Spectrophotometric Simultaneous Determination of Iron, Nickel and Zinc

    Directory of Open Access Journals (Sweden)

    Teixeira Leonardo S. G.

    2002-01-01

    Full Text Available A PLS-2 multivariate calibration method has been developed for the simultaneous determination of iron, nickel and zinc in ternary mixtures by solid phase spectrophotometry associated with flow injection analysis. Fe(II, Ni(II and Zn(II form color complexes with 1-(2-thiazolylazo-2-naphthol (TAN, immobilized on a C18 bonded silica support, at pH 6.4. The proposed procedure is based on the different reaction/retention ratios of the studied ions on the solid support. Bilinear spectrophotometric data of the analytes, fixed in the solid support, were recorded in the 400-800 nm wavelength range as a function of time and a partial least squares (PLS-2 algorithm was used to predict results of synthetic samples. The calibration set employed was integrated by 8 ternary mixture standards and a blank solution. Mixtures containing 0.040 to 0.20 mg L-1, of each species, were successfully resolved, using 3 factors for each analyte and a restricted number of absorbance data obtained in the wavelength range from 560 to 650 nm.

  1. Simultaneous Determination of Four Active Ingredients in Sargentodoxa cuneata by HPLC Coupled with Evaporative Light Scattering Detection

    Directory of Open Access Journals (Sweden)

    Di-Hua Li

    2016-01-01

    Full Text Available A HPLC coupled with evaporative light scattering detection method had been developed for the simultaneous determination of 3,4-dihydroxyphenylethyl alcohol glycoside, salidroside, chlorogenic acid, and liriodendrin in the stem of Sargentodoxa cuneata. With a C18 column, the analysis was performed using acetonitrile and 0.2% formic acid aqueous solution as mobile phase in gradient program at a flow rate of 0.9 mL/min. The optimum drift tube temperature of evaporative light scattering detection was at 105°C with the air flow rate of 2.5 L/min. The calibration curves showed good linearity during the test ranges. This method was validated for limits of detection and quantification, precision, and reproducibility. The recoveries were within the range of 96.39%–104.64%. The relative standard deviations of intraday and interday precision were less than 2.90% and 3.30%, respectively. The developed method can be successfully used to quantify the four analytes in the stem of Sargentodoxa cuneata from various regions in China.

  2. Simultaneous Determination of 11 Compounds in Gualou Guizhi Granule and Pharmacokinetics Study by UPLC-MS/MS

    Directory of Open Access Journals (Sweden)

    Chengtao Sun

    2017-01-01

    Full Text Available A rapid and sensitive ultrafast performance liquid chromatography-tandem mass spectrometry method (UPLC-MS/MS was developed for the simultaneous determination of 11 compounds in Gualou Guizhi Granule (GLGZG, including liquiritin, isoliquiritin, liquirtin apioside, isoliquiritin apioside, liquiritigenin, isoliquiritigenin, glycyrrhizic acid, glycyrrhetinic acid, paeoniflorin, albiflorin, and paeoniflorin sulfonate in rat plasma. UPLC-MS/MS assay with negative ion mode was performed on a Waters CORTECS C18 (2.1 × 100 mm, 1.6 μm with the mobile phase consisting of 0.1% aqueous formic acid (A and acetonitrile (B in gradient elution at a flow rate of 0.25 mL·min−1. The method was linear for all analytes within the detection range (r≥0.9597. The inter- and intraday precision (RSD were 2.21–6.41% and 1.67–6.18%; the inter- and intraday accuracy (recover were 92.48–114.03% and 90.23–112.04%. And the recovery rate ranged from 81.30% to 108.22%. The matrix effect values obtained for analytes ranged from 88.91% to 113.32%. This validated method was successfully applied to a pharmacokinetics study in rats after oral administration of GLGZG.

  3. Development and Validation of an HPLC Method for Simultaneous Determination of Rifampicin, Isoniazid, Pyrazinamide, and Ethambutol Hydrochloride in Pharmaceutical Formulations.

    Science.gov (United States)

    Chellini, Paula R; Lages, Eduardo B; Franco, Pedro H C; Nogueira, Fernando H A; César, Isabela C; Pianetti, Gerson A

    2015-01-01

    Tuberculosis treatment consists of a fixed dose combination of rifampicin (RIF), isoniazid (INH), pyrazinamide (PYZ), and ethambutol hydrochloride (EMB). The combined treatment using various drugs is necessary for patient curing, without recrudescence, and for prevention of drug-resistant mutants, which may occur during treatment. An HPLC-diode array detector (DAD) method for the simultaneous determination of RIF, INH, PYZ, and EMB in fixed dose combination tablets was developed and validated. Chromatographic experiments were performed on an Agilent 1200 HPLC system, and the separation was carried out on a Purospher STAR RP18e (250×4.6 mm id, 5 μm, Merck) analytical column. Gradient elution was carried out with a mobile phase of 20 mM monobasic sodium phosphate buffer with 0.2% triethylamine (pH 7.0) and acetonitrile at a flow rate of 1.5 mL/min. The total run time was 12 min, and the re-equilibration time was 5 min. EMB detection was performed at 210 nm, and RIF, INH, and PYZ were detected at 238 nm, using a DAD. The method proved to be specific, linear (r2>0.99), precise (RSD<2%), accurate, and robust and may be applied to the QC analysis of pharmaceutical formulations.

  4. Simultaneous determinations of uranium, thorium, and plutonium in soft tissues by solvent extraction and alpha-spectrometry

    International Nuclear Information System (INIS)

    Singh, N.P.; Zimmerman, C.J.; Lewis, L.L.; Wrenn, M.E.

    1984-01-01

    A radiochemical procedure for the simultaneous determination of uranium, thorium, and plutonium, in soft tissues has been developed. The weighed amounts of tissues, spiked with 232 U, 242 Pu, and 229 th tracers, are wet ashed. Uranium, thorium, and plutonium are coprecipitated with iron as hydroxides, dissolved in concentrated HCl and the acidity adjusted to 10 M. Uranium and plutonium are extracted into 20% TLA solution in xylene, leaving thorium in the aqueous phase. Plutonium is back-extracted by reducing to the trivalent state with 0.05 M NH 4 I solution in 8 M HCl, and uranium is back-extracted with 0.1 M HCl. Thorium is extracted into 20% TLA solution from 4 M HNO 3 and back-extracted with 10 M HCl. Uranium, thorium and plutonium are electrodeposited separately onto platinum discs and counted alpha-spectrometrically using surface barrier silicon diodes and a multichannel analyzer. The method was developed using bovine liver and applied to dog and human tissues. The mean radiochemical recoveries of these actinides in different organs were better than 70%. 6 references, 2 tables

  5. Development and Validation of an ICP-MS Method for Simultaneous Determination of Selected Metals in Electronic Cigarette Aerosol

    Directory of Open Access Journals (Sweden)

    Ohashi Shintaro

    2018-04-01

    Full Text Available Safety and quality standards for electronic cigarettes (e-cigarettes have been introduced regionally. In 2016, the U.S. Food and Drug Administration (FDA issued a rule to regulate e-cigarettes, requiring to report harmful and potentially harmful constituents (HPHCs. In the United Kingdom, the British Standards Institution (BSI specified the metals to be monitored for e-cigarettes. In this study, a method was developed and validated for the simultaneous determination of 13 metals (Be, Al, Cr, Fe, Co, Ni, Cu, As, Se, Ag, Cd, Sn and Pb in e-cigarette aerosol. Furthermore, matrix effects of major constituents in the aerosol were investigated using glycerol or 1,2-propylene glycol solutions. E-cigarette aerosol was generated by a rotary smoking machine according to CORESTA Recommended Method N° 81 and collected by an electrostatic precipitator coupled to an impinger containing nitric acid. The collected aerosol was dissolved in nitric acid and an aliquot of this solution was analyzed by inductively coupled plasma mass spectrometry (ICP-MS equipped with a collision/reaction cell.

  6. Simultaneous determination of ten illegal azo dyes in feed by ultra-high performance liquid chromatography tandem mass spectrometry

    Directory of Open Access Journals (Sweden)

    Piątkowska Marta

    2017-09-01

    Full Text Available Introduction: The paper presents the method of simultaneous determination of 10 illegal azo dyes in feed by ultra-high performance liquid chromatography coupled with tandem mass spectrometry technique. Material and Methods: The dyes were extracted with hexane, evaporated to dryness, and analysed. Separation was achieved in 7 min in a gradient elution using acetonitrile (A and 0.1% formic acid (B as a mobile phase. Results: The validation results showed the repeatability of the method, which was evaluated at three levels (50, 500, and 5,000 μg/kg. All the matrix calibration curves for the working ranges were linear (R2 0.9904 to 1.0, the repeatability was between 2.1% and 24%, and recoveries ranged from 77.9% to 120%. The LOD and LOQ were at 1-2 and 5-10 μg/kg for different dyes, respectively. Furthermore, the method was applied in the homogeneity tests of the in-house prepared feed containing Sudan I at the levels of 0.5, 5, and 50 mg/kg. Conclusions: A sensitive, selective, and fast multiresidue method was successfully developed and validated. Its robustness was confirmed by the analysis of an experimental feed containing Sudan I.

  7. [Simultaneous determination of six fluorescent whitening agents in plastic and paper packaging materials by high performance liquid chromatography].

    Science.gov (United States)

    Zhang, Juzhou; Ji, Shuilin; Cai, Huimei; Li, Jing; Wang, Yongxin; Wang, Jingqiu

    2017-11-08

    A novel analytical method was developed for the simultaneous determination of six fluorescent whitening agents (FWAs:FWA 135, FWA 184, FWA 185, FWA 199, FWA 378 and FWA 393) in paper and plastic food packaging materials by high performance liquid chromatography with fluorescence detection (HPLC-FLD). The sample was extracted with mixed solution of chloroform and acetonitrile (3:7, v/v), then cleaned up by HLB solid phase extraction column. Qualitative and quantitative analyses were carried out by HPLC. The sample was separated on a Phenomenex C18 column using acetonitrile and 5 mmol/L ammonium acetate aqueous solution as mobile phases. The results indicated that the linear range of FWA393 was 15-1500 μg/L and the linear ranges of the other five FWAs were 5-500 μg/L with correlation coefficients greater than 0.999. The recoveries in spiked samples were between 80.4% and 125.0% with RSDs ( n =6) of 1%-13%. Furthermore, this method was applied to analyze 12 samples in the market to verify the practicality of the method. The method showed the advantages of simplicity, high recovery and good precision, and is suitable for the detection of the six fluorescent whitening agents in food packaging materials.

  8. Simultaneous determination of eight cyclopolypeptide antibiotics in feed by high performance liquid chromatography coupled with evaporation light scattering detection.

    Science.gov (United States)

    Song, Xuqin; Xie, Jingmeng; Zhang, Meiyu; Zhang, Yingxia; Li, Jiufeng; Huang, Qiwen; He, Limin

    2018-02-15

    A high throughput, reliable and reproducible analysis strategy based on high performance liquid chromatography combined to evaporative light scattering detector (HPLC-ELSD) was developed for simultaneous determination of eight cyclopolypeptide antibiotics including vancomycin, polymyxin B (polymyxin B1 and polymyxin B2), polymyxin E (colistin A and colistin B), teicoplanin, bacitracin A, daptomycin and virginiamycin M1 in animal Feed. Feed samples were extracted with methanol-2% formic acid aqueous solution, followed by a solid-phase extraction step using a HLB cartridge. Under the optimum chromatographic conditions and ELSD parameters, target compounds were separated well on a short column filled with biphenyl stationary phase. The method was developed in accordance with pig complete feed and then extended to detect polypeptide antibiotics in piglet premix, pig feed additive, poultry complete feed and fattening pig premix. The results showed that logarithmic calibration curves of eight analytes were linear (r 2  > 0.99) within the concentration range of 5-200 mg mL -1 . The developed method provided good accuracy and precision for quantification of eight polypeptides in five kinds of feeds with recoveries ranging from 72.0% to 105.4% with relative standard deviations antibiotics in commercial feed. Copyright © 2018 Elsevier B.V. All rights reserved.

  9. Simultaneous determination of hydride and non-hydride forming elements by inductively coupled plasma optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Benzo, Z. [Instituto Venezolano de Investigaciones Cientificas, IVIC, Altos de Pipe, Caracas (Venezuela, Bolivarian Republic of); Matos-Reyes, M.N.; Cervera, M.L.; Guardia, M. de la, E-mail: m.luisa.cervera@uv.es [Department of Analytical Chemistry, University of Valencia, Valencia (Spain)

    2011-09-15

    The operating characteristics of a dual nebulization system were studied including instrumental and chemical conditions for the hydride generation and analytical figures of merit for both, hydride and non hydride forming elements. Analytical performance of the nebulization system was characterized by detection limits from 0.002 to 0.0026 {mu}g mL{sup -1} for the hydride forming elements and between 0.0034 and 0.0121 {mu}g mL{sup -1} for the non-hydride forming elements, relative standard deviation for 10 replicate measurements at 0.25 mg L{sup -1} level and recovery percentages between 97 and 103%. The feasibility of the system was demonstrated in the simultaneous determination of Ca, Cd, Co, Cr, Cu, Fe, Mg, Mn, Mo, Ni, Zn, As, Bi, Sb, Se, and Te in the NIST 1549 (non-fat milk powder), NIST 1570a (spinach leaves), DORM-2 (dogfish muscle) and TORT-2 (lobster hepatopancreas) certified samples for trace elements. Results found were in good agreement with the certified ones. (author)

  10. 1H NMR method for simultaneous identification and determination of caffeine and theophylline in human serum and pharmaceutical preparations

    International Nuclear Information System (INIS)

    Talebpour, Z.; Bijanzadeh, H.R.; Haghgoo, S.; Shamsipur, M.

    2004-01-01

    A 1 H NMR method for simultaneous identification and determination of caffeine and theophylline in pharmaceutical preparations and human serum has been developed. 1 H NMR spectrum of caffeine exhibits three sharp singlets at 2.75, 2.93 and 3.4 ppm, while that of theophyline shows two singlet peaks at 2.77 and 2.97 ppm. For the purpose of quantitative analyses of the mixtures of these two alkaloids 1 H NMR spectra of caffeine and theophylline was compared to that of maleic acid as an internal standard at the constant temperature. The suitable peaks were selected and standard deviation and reproducibility of the results were studied applying the full factorial design method. The obtained detection limits are 1.6 μgL - 1 and 1.43 μg L 1 for caffeine and theophylline, respectively. The average recoveries of the studied applying compounds in various samples, pharmaceutical preparations and human serum ranged from 90.2 to 107.5% (author)

  11. Simultaneous determination and validation of emtricitabine, rilpivirine and tenofovir from biological samples using LC and CE methods.

    Science.gov (United States)

    Gumustas, Mehmet; Caglayan, Mehmet Gokhan; Onur, Feyyaz; Ozkan, Sibel A

    2018-04-01

    A combination of antiretroviral agents is frequently used in effective treatment of the human immunodeficiency virus infection. In this study, two different separation methods are presented for the simultaneous determination of emtricitabine, rilpivirine and tenofovir from raw materials and urine samples. Developed liquid chromatography and capillary electrophoresis methods were thoroughly optimized for high analytical performances. Optimization of multiple variables at the same time by performing a minimum number of experiments was achieved by the Box-Behnken design, which is an experimental design in response surface methodology, in capillary electrophoresis. The results of the experimental design ensure minimum analysis time with well-separated analytes. Separation conditions, such as different stationary phases, pH level, organic modifiers and temperatures in liquid chromatography method, were also optimized. In particular, among stationary phases, the core-shell column especially enhanced the effectiveness of separation in liquid chromatography. Both methods were fully validated and applied to real samples. The main advantage of the developed methods is the separation of the drug combination in a short time with high efficiency and without any time-consuming steps. Copyright © 2017 John Wiley & Sons, Ltd.

  12. Improved simultaneous determination method of beta-carotene and retinol with saponification in human serum and rat liver.

    Science.gov (United States)

    Hosotani, Keisuke; Kitagawa, Masahiro

    2003-07-05

    Among the many simultaneous determination methods for carotenoid and retinoid, there are only a few reports including the saponification process. However, the yields of beta-carotene and retinol were higher when using this process. In this study, the analytical conditions, including saponification, were investigated. The extraction solvent was n-hexane and the sample solvent was HPLC mobile phase in the beta-carotene and retinol analysis. BHT as an antioxidant was added at concentrations of 0.125 and 0.025%, respectively, to ethanol and n-hexane phase in the extraction process for serum. The recovery rates were 99.7, 93.7 and 98.3% for beta-carotene, retinol and retinyl palmitate in serum, respectively, and 107.1, 92.8 and 98.8% for beta-carotene, retinol and retinyl palmitate in liver, respectively. The within-day coefficients of variation (C.V.) were 6.0% for serum and 4.7% for liver in the case of beta-carotene, 7.1% for serum, and 5.1% for liver in the case of retinol. The between-day coefficients of variation were 2.7% for serum and 2.7% for liver in the case of beta-carotene, and for retinol, 6.4% for serum and 2.7% for liver.

  13. Simultaneous determination of levocetirizine and pseudoephedrine in dog plasma by liquid chromatography-mass spectrometry in the presence of dextrocetirizine.

    Science.gov (United States)

    Ryu, Jae Kuk; Yoo, Sun Dong

    2012-01-01

    This study describes the development of a rapid and sensitive LC-ESI-MS assay for simultaneous enantioselective determination of levocetirizine and pseudoephedrine in dog plasma in the presence of dextrocetirizine. Separations were achieved on an Ultron ES-OVM chiral column using the mobile phase consisting of 10 mM aqueous NH4OAc (pH 6.6) and acetonitrile (9:1 v/v). The retention times of pseudoephedrine, dextrocetirizine, levocetirizine and diazepam (internal standard) were 5.2, 8.3, 9.6 and 11.6 min, respectively, and the total run time was less than 15 min. The assay was validated to demonstrate the linearity, accuracy and precision, recovery and stability. The calibration curves were linear over the concentration range from 1 - 200 ng/mL for levocetirizine and from 5 - 1000 ng/mL for pseudoephedrine. The developed assay was successfully applied to a pharmacokinetic study after oral administration of the racemic cetirizine (0.5 mg/kg, or 0.25 mg/kg as levocetirizine) and pseudoephedrine (12 mg/kg) in the dog. This article is open to POST-PUBLICATION REVIEW. Registered readers (see "For Readers") may comment by clicking on ABSTRACT on the issue's contents page.

  14. Accurate marker-free alignment with simultaneous geometry determination and reconstruction of tilt series in electron tomography

    International Nuclear Information System (INIS)

    Winkler, Hanspeter; Taylor, Kenneth A.

    2006-01-01

    An image alignment method for electron tomography is presented which is based on cross-correlation techniques and which includes a simultaneous refinement of the tilt geometry. A coarsely aligned tilt series is iteratively refined with a procedure consisting of two steps for each cycle: area matching and subsequent geometry correction. The first step, area matching, brings into register equivalent specimen regions in all images of the tilt series. It determines four parameters of a linear two-dimensional transformation, not just translation and rotation as is done during the preceding coarse alignment with conventional methods. The refinement procedure also differs from earlier methods in that the alignment references are now computed from already aligned images by reprojection of a backprojected volume. The second step, geometry correction, refines the initially inaccurate estimates of the geometrical parameters, including the direction of the tilt axis, a tilt angle offset, and the inclination of the specimen with respect to the support film or specimen holder. The correction values serve as an indicator for the progress of the refinement. For each new iteration, the correction values are used to compute an updated set of geometry parameters by a least squares fit. Model calculations show that it is essential to refine the geometrical parameters as well as the accurate alignment of the images to obtain a faithful map of the original structure

  15. Determine Multiple Elements Simultaneously in the Sera of Umbilical Cord Blood Samples-a Very Simple Method.

    Science.gov (United States)

    Liang, Chunmei; Li, Zhijuan; Xia, Xun; Wang, Qunan; Tao, Ruiwen; Tao, Yiran; Xiang, Haiyun; Tong, Shilu; Tao, Fangbiao

    2017-05-01

    Analyzing the concentrations of heavy metals in the sera of umbilical cord blood samples can provide useful information about prenatal exposure to environmental agents. An analytical method based on ICP-MS to simultaneously determine multiple elements in umbilical cord blood samples was developed for assessing the in utero exposure to metallic and metalloid elements. The method only required as little as 100 μL of serum diluted 1:25 for direct analysis. Matrix-matched protocol was used to eliminate mass matrix interference and kinetic energy discrimination mode was used to eliminate the polyatomic ion interference. The assay was completed on average within 4 min with the detection limits ranging from 0.0002 to 44.4 μg/L for all the targeted elements. The detection rates for most of elements were 100 % other than cadmium (Cd), lead (Pb), and mercury (Hg). The testing results of the certified reference materials were ideal. The method is simple and sensitive, so it is suitable for the monitoring of large quantities of samples.

  16. [Simultaneous determination of five effective components in Sijunzi bolus using high performance liquid chromatography-evaporation light scattering detection].

    Science.gov (United States)

    Li, Chunying; Zhang, Xiaojun

    2010-01-01

    A high performance liquid chromatographic (HPLC) method was developed for the simultaneous determination of lobetyolin, pachymic acid, glycyrrhizic acid, atractylenoide III and atractylenolide I in Sijunzi bolus. The separation was performed on an HIQ SIL C18 V column (250 mm x 4.6 mm, 5 microm) with 0.5% acetic acid-methanol as the mobile phase of gradient elution at a flow rate of 1.0 mL/min. The detection was performed with an evaporation light scattering detector (ELSD) and the sample volume was 10 microL. The temperature of drift tube and heating grade of nebulizer was respectively set at 55 degrees C and 60% at 0.2 MPa of pressure. Nitrogen gas was used as carrier gas. Under the optimized conditions, there were good linear relationships between the logarithm values of mass concentration and the peak areas of lobetyolin, pachymic acid, glycyrrhizic acid, atractylenoide III and atractylenolide I in the ranges of 0.076 - 1.21, 0.048 -0.76, 0.153 - 2.45, 0.045 - 0.72 and 0.098 - 1.56 g/L, respectively. The recoveries of the five components were between 97.13% and 100.25%, the relative standard deviations (RSDs) were between 1.23% and 2.44%. This method is simple, rapid, accurate and suitable for the quality control of Sijunzi bolus.

  17. Simultaneous quantitative determination of eight index constituents and compatibility changes in Longchai Decoction by UPLC–Q-TOF-MS

    Directory of Open Access Journals (Sweden)

    Yizhi Zhou

    2013-07-01

    Full Text Available The goal of this research was to develop a simple, rapid and sensitive method for simultaneous quantitative determination of salidroside, gardenoside, liquiritin, baicalin, wogonoside, wogonin, saikosaponin A and saikosaponin D in Longchai Decoction by ultra-performance liquid chromatography quadrupole time-of-flight mass spectrometry (UPLC–Q-TOF-MS, in order to control the quality of Longchai Decoction and to analyze the changes of chemical components before and after the compatibility of the component herb drugs. The chromatographic separation was performed on the Waters ACQUITY BEH C18 column (2.1 mm×100 mm, 1.8 μm using the mixture of acetonitrile and 0.1% (v/v methanoic acid as mobile phase with a gradient elution program at the flow rate of 0.3 mL/min and the column temperature of 30 °C. The eight components of the standards achieved baseline separation. Regression analysis revealed a linear relationship (r2>0.9998 between the contents and the peak areas of the mixed standard substances. The average recovery rates were between 99.72% and 102.13% with RSD values were less than 2.82% (n=5. The obtained results indicated that the content of index components were higher in co-decoction compared to mixed decoction. This method with a good resolution and high precision can be used for the quality control of Longchai Decoction.

  18. Simultaneous Determination of the Main Peanut Allergens in Foods Using Disposable Amperometric Magnetic Beads-Based Immunosensing Platforms

    Directory of Open Access Journals (Sweden)

    Víctor Ruiz-Valdepeñas Montiel

    2016-06-01

    Full Text Available In this work, a novel magnetic beads (MBs-based immunosensing approach for the rapid and simultaneous determination of the main peanut allergenic proteins (Ara h 1 and Ara h 2 is reported. It involves the use of sandwich-type immunoassays using selective capture and detector antibodies and carboxylic acid-modified magnetic beads (HOOC-MBs. Amperometric detection at −0.20 V was performed using dual screen-printed carbon electrodes (SPdCEs and the H2O2/hydroquinone (HQ system. This methodology exhibits high sensitivity and selectivity for the target proteins providing detection limits of 18.0 and 0.07 ng/mL for Ara h 1 and Ara h 2, respectively, with an assay time of only 2 h. The usefulness of the approach was evaluated by detecting the endogenous content of both allergenic proteins in different food extracts as well as trace amounts of peanut allergen (0.0001% or 1.0 mg/kg in wheat flour spiked samples. The developed platform provides better Low detection limits (LODs in shorter assay times than those claimed for the allergen specific commercial ELISA kits using the same immunoreagents and quantitative information on individual food allergen levels. Moreover, the flexibility of the methodology makes it readily translate to the detection of other food-allergens.

  19. Simultaneous determination of water-soluble vitamins in beverages and dietary supplements by LC-MS/MS.

    Science.gov (United States)

    Kakitani, Ayano; Inoue, Tomonori; Matsumoto, Keiko; Watanabe, Jun; Nagatomi, Yasushi; Mochizuki, Naoki

    2014-01-01

    An LC-MS/MS method was developed for the simultaneous determination of 15 water-soluble vitamins that are widely used as additives in beverages and dietary supplements. This combined method involves the following simple pre-treatment procedures: dietary supplement samples were prepared by centrifugation and filtration after an extraction step, whereas beverage samples were diluted prior to injection. Chromatographic analysis in this method utilised a multi-mode ODS column, which provided reverse-phase, anion- and cation-exchange capacities, and therefore improved the retention of highly polar analytes such as water-soluble vitamins. Additionally, the multi-mode ODS column did not require adding ion pair reagents to the mobile phase. We optimised the chromatographic separation of 15 water-soluble vitamins by adjusting the mobile phase pH and the organic solvent. We also conducted an analysis of a NIST Standard Reference Material (SRM 3280 Multi-vitamin/Multi-element tablets) using this method to verify its accuracy. In addition, the method was applied to identify the vitamins in commercial beverages and dietary supplements. By comparing results with the label values and results obtained by official methods, it was concluded that the method could be used for quality control and to compose nutrition labels for vitamin-enriched products.

  20. High-performance liquid chromatography and derivative spectrophotometry for simultaneous determination of pravastatin and fenofibrate in the dosage form

    Directory of Open Access Journals (Sweden)

    Hefnawy Mohamed M.

    2014-12-01

    Full Text Available High performance liquid chromatography (HPLC and second-order derivative spectrophotometry have been used for simultaneous determination of pravastatin (PS and fenofibrate (FF in pharmaceutical formulations. HPLC separation was performed on a phenyl HYPERSIL C18 column (125 mm × 4.6 mm i.d., 5 μm particle diameter in the isocratic mode using a mobile phase acetonitrile/0.1 % diethyl amine (50:50, V/V, pH 4.5 pumped at a flow rate of 1.0 mL min-1. Measurement was made at 240 nm. Both drugs were well resolved on the stationary phase, with retention times of 2.15 and 5.79 min for PS and FF, respectively. Calibration curves were linear (R = 0.999 for PS and 0.996 for FF in the concentration range of 5-50 and 20-200 µg mL-1 for PS and FF, respectively. Pravastatin and fenofibrate were quantitated in combined preparations also using the second-order derivative response at 237.6 and 295.1 nm for PS and FF, respectively. Calibration curves were linear, with the correlation coefficient R = 0.999 for pravastatin and fenofibrate, in the concentration range of 5-20 and 3-20 µg mL-1 for PS and FF, respectively. Both methods were fully validated and compared, the results confirmed that they were highly suitable for their intended purpose.

  1. Sensitive radioimmunoassay and enzyme-linked immunosorbent assay for the simultaneous determination of chloroquine and its metabolites in biological fluids

    International Nuclear Information System (INIS)

    Escande, C.; Chevalier, P.; Verdier, F.; Bourdon, R.

    1990-01-01

    Two new methods for the simultaneous determination of chloroquine and its two main metabolites (monodesethylchloroquine and bisdesethylchloroquine) in biological samples, radioimmunoassay (RIA) and enzyme-linked immunosorbent assay (ELISA), are described. Antiserum is produced in rabbits immunized with N-(2-carboxyethyl)desethylchloroquine:protein conjugate. Besides chloroquine, this antiserum recognizes with good affinity the two main metabolites, monodesethylchloroquine and bisdesethylchloroquine (70 and 40% of crossreaction, respectively). Amodiaquine cross reacts by 4.5%; cross reactions with monodesethylamodiaquine, bisdesethylamodiaquine, and other antimalarial drugs are less than 1%. No extraction step or sample preparation is required for either system. Sensitivity limits are, respectively, 0.70 nM (3 pg of chloroquine sulfate measured in 10 microL of plasma sample) for RIA, and 10 nM (22 pg of chloroquine sulfate measured in 5 microL of plasma sample) for ELISA. The interassay coefficients of variation are, respectively, less than 10 and less than 16% for RIA and ELISA in the range 14-410 nM (6-180 ng/mL). The results of both methods are well correlated (r = 0.97) and correlate with spectrophotometry (r = 0.98) and HPLC results (r = 0.93). Because of their high sensitivity, both methods can be used in the case of chloroquine poisoning and in the control of malaria prophylaxis and treatment

  2. Simultaneous determination of quercetin, kaempferol and isorhamnetin accumulated human breast cancer cells, by high-performance liquid chromatography.

    Science.gov (United States)

    Wang, Yi; Cao, Jiang; Weng, Jian-Hua; Zeng, Su

    2005-09-01

    Quercetin, kaempferol and isorhamnetin are the most important constituents in ginkgo flavonoids. A simple, rapid and sensitive high-performance liquid chromatography method was developed to simultaneously determine quercetin, kaempferol and isorhamnetin absorped by human breast cancer cells. Cells were treated with ginkgo flavonols and then lysed with Triton-X 100. The flavonols in the samples were measured by RP-HPLC with a C18 column after a simple extraction with a mixture of ether and acetone. The mobile phase contained phosphate buffer (pH 2.0; 10 mM) tetrahydrofuran, methanol and isopropanol (65:15:10:20, v/v/v/v). The ultraviolet detector was operated at 380 nm. The calibration curve was linear from 0.1 to 1.0 microM (r > 0.999) for each flavonol. The mean extraction efficiency was about 70%. The recovery of the assay was between 98.9 and 100.6%. The limit of detection was 0.01 microM for quercetin and kaempferol and 0.05 microM for isorhamnetin. The limit of quantitation was 0.1 microM (R.S.D.method was applied to quantify quercetin, kaempferol and isorhamnetin in human breast cancer Bcap37 and Bcap37/MDR1 cells.

  3. The application of artificial neural networks and support vector regression for simultaneous spectrophotometric determination of commercial eye drop contents

    Science.gov (United States)

    Valizadeh, Maryam; Sohrabi, Mahmoud Reza

    2018-03-01

    In the present study, artificial neural networks (ANNs) and support vector regression (SVR) as intelligent methods coupled with UV spectroscopy for simultaneous quantitative determination of Dorzolamide (DOR) and Timolol (TIM) in eye drop. Several synthetic mixtures were analyzed for validating the proposed methods. At first, neural network time series, which one type of network from the artificial neural network was employed and its efficiency was evaluated. Afterwards, the radial basis network was applied as another neural network. Results showed that the performance of this method is suitable for predicting. Finally, support vector regression was proposed to construct the Zilomole prediction model. Also, root mean square error (RMSE) and mean recovery (%) were calculated for SVR method. Moreover, the proposed methods were compared to the high-performance liquid chromatography (HPLC) as a reference method. One way analysis of variance (ANOVA) test at the 95% confidence level applied to the comparison results of suggested and reference methods that there were no significant differences between them. Also, the effect of interferences was investigated in spike solutions.

  4. Dual Wavelength RP-HPLC Method for Simultaneous Determination of Two Antispasmodic Drugs: An Application in Pharmaceutical and Human Serum

    Directory of Open Access Journals (Sweden)

    Najmul Hasan

    2013-01-01

    Full Text Available A reverse phase stability indicating HPLC method for simultaneous determination of two antispasmodic drugs in pharmaceutical parenteral dosage forms (injectable and in serum has been developed and validated. Mobile phase ingredients consist of Acetonitrile : buffer : sulfuric acid 0.1 M (50 : 50 : 0.3 v/v/v, at flow rate 1.0 mL/min using a Hibar μBondapak ODS C18 column monitored at dual wavelength of 266 nm and 205 nm for phloroglucinol and trimethylphloroglucinol, respectively. The drugs were subjected to stress conditions of hydrolysis (oxidation, base, acid, and thermal degradation. Oxidation degraded the molecule drastically while there was not so much significant effect of other stress conditions. The calibration curve was linear with a correlation coefficient of 0.9999 and 0.9992 for PG and TMP, respectively. The drug recoveries fall in the range of 98.56% and 101.24% with 10 pg/mL and 33 pg/mL limit of detection and limit of quantification for both phloroglucinol and trimethylphloroglucinol. The method was validated in accordance with ICH guidelines and was applied successfully to quantify the amount of trimethylphloroglucinol and phloroglucinol in bulk, injectable form and physiological fluid. Forced degradation studies proved the stability indicating abilities of the method.

  5. Electrochemical sensor based on graphene and mesoporous TiO2 for the simultaneous determination of trace colourants in food.

    Science.gov (United States)

    Gan, Tian; Sun, Junyong; Meng, Wen; Song, Li; Zhang, Yuxia

    2013-12-15

    Currently, synthetic colourants draw much attention as food additives. This paper investigated the simultaneous electrocatalytic oxidation of sunset yellow and tartrazine, two yellow colourants commonly present in food together, with a novel voltammetric sensor based on graphene and mesoporous TiO2 modified carbon paste electrode. Due to the high accumulation effect and great catalytic capability of graphene and mesoporous TiO2, the developed sensor exhibited well-defined and separate square wave voltammetric peaks (i.e., 272 mV) for sunset yellow tartrazine. The peak currents of sunset yellow and tartrazine increased linearly with their concentration in the ranges of 0.02-2.05 μM and 0.02-1.18 μM, respectively. And the detection limit was 6.0 and 8.0 nM for sunset yellow and tartrazine, respectively. This new sensor was applied to determine sunset yellow and tartrazine in several food sample extracts. Results suggested that the proposed sensor was sensitive, rapid and reliable. Copyright © 2013 Elsevier Ltd. All rights reserved.

  6. Self-assembly of graphitic carbon nitride nanosheets–carbon nanotube composite for electrochemical simultaneous determination of catechol and hydroquinone

    International Nuclear Information System (INIS)

    Zhang, Hanqiang; Huang, Yihong; Hu, Shirong; Huang, Qitong; Wei, Chan; Zhang, Wuxiang; Yang, Weize; Dong, Peihui; Hao, Aiyou

    2015-01-01

    Graphical abstract: Schematic diagram of hydrothermal synthesis graphitic carbon nitride nanosheets-carbon nanotube composite and theirs application for electrochemical sensing catechol and hydroquinone. - Highlights: • Self-assembly of graphitic carbon nitride nanosheets-carbon nanotube composite. • CNNS-CNT show more stronger conductivity than CNNS and CNT. • CNNS-CNT has been performed for detection of catechol and hydroquinone. • The probe was applied to detect practical samples with satisfactory results. - Abstract: In this paper, three-dimensional (3D) graphitic carbon nitride nanosheets-carbon nanotube (CNNS-CNT) composite was synthesized via hydrothermal reaction of 2D CNNS and 1D CNT-COOH by π-π stacking and electrostatic interactions. This CNNS-CNT composite was characterized by transmission electron microscope, scanning electron microscope, x-ray diffraction and fourier-transform infrared. In addition, the CNNS-CNT composite displayed excellent conductivity comparing with CNNS and CNT-COOH monomer. This composite was applied for electrochemical simultaneous determination of catechol (CC) and hydroquinone (HQ) with good sensitivity, wide linear range and low detection limit. In addition, this CNNS-CNT composite modified electrode was also applied to detect practical samples with satisfactory results

  7. Contribution to the simultaneous determination of several light elements in alkalin metals by gamma photon and charged particle activation. Application to carbon and nitrogen determination in sodium

    International Nuclear Information System (INIS)

    Bock, Patrice.

    1976-10-01

    A new γ activation method for the simultaneous determination of carbon and nitrogen in sodium is described. It makes use of the nuclear reactions: 12 C(γ,n) 11 C and 14 N(γ,n) 13 N. The process used to separate carbone-11 and nitrogen-13 from sodium with a view to their radio-activity determination is based on vacuum dissolution of the sample in a mixture of oxidizing and acid fused salts. The oxidized carbon is trapped as CO 2 on soda asbestos and the nitrogen as N 2 on molecular sieve at -196 deg C. The efficiency of the technique is estimated by means of tracer tests and by proton activation. The relative influence of competitive nuclear reactions on elements close to the above two impurities, or even on the matrix itself, is examined. The method described has a theoretical detection limit of some 10 -8 g.g -1 for the two elements in question and mean concentrations of 0.3+-0.1x10 -6 g.g -1 carbon and 1.0+-0.5x10 -6 g.g -1 nitrogen have in fact been measured in a batch of 0.5 g sodium samples [fr

  8. Single peak parameters technique for simultaneous measurements: Spectrophotometric sequential injection determination of Fe(II) and Fe(III).

    Science.gov (United States)

    Kozak, J; Paluch, J; Węgrzecka, A; Kozak, M; Wieczorek, M; Kochana, J; Kościelniak, P

    2016-02-01

    Spectrophotometric sequential injection system (SI) is proposed to automate the method of simultaneous determination of Fe(II) and Fe(III) on the basis of parameters of a single peak. In the developed SI system, sample and mixture of reagents (1,10-phenanthroline and sulfosalicylic acid) are introduced into a vessel, where in an acid environment (pH≅3) appropriate compounds of Fe(II) and Fe(III) with 1,10-phenanthroline and sulfosalicylic acid are formed, respectively. Then, in turn, air, sample, EDTA and sample again, are introduced into a holding coil. After the flow reversal, a segment of air is removed from the system by an additional valve and as EDTA replaces sulfosalicylic acid forming a more stable colorless compound with Fe(III), a complex signal is registered. Measurements are performed at wavelength 530 nm. The absorbance measured at minimum of the negative peak and the area or the absorbance measured at maximum of the signal can be used as measures corresponding to Fe(II) and Fe(III) concentrations, respectively. The time of the peak registration is about 2 min. Two-component calibration has been applied to analysis. Fe(II) and Fe(III) can be determined within the concentration ranges of 0.04-4.00 and 0.1-5.00 mg L(-1), with precision less than 2.8% and 1.7% (RSD), respectively and accuracy better than 7% (RE). The detection limit is 0.04 and 0.09 mg L(-1) for Fe(II) and Fe(III), respectively. The method was applied to analysis of artesian water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. Simultaneous determination of seven anticoagulant rodenticides in agricultural products by gel permeation chromatography and liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Saito-Shida, Shizuka; Nemoto, Satoru; Matsuda, Rieko; Akiyama, Hiroshi

    2016-11-01

    A sensitive and reliable method for the simultaneous determination of hydroxycoumarin-type (brodifacoum, bromadiolone, coumatetralyl, and warfarin) and indandione-type (chlorophacinone, diphacinone, and pindone) rodenticides in agricultural products by gel permeation chromatography (GPC) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed. The procedure involved extraction of the rodenticides from samples with acetone, followed by liquid-liquid partitioning with hexane/ethyl acetate (1:1, v/v) and 10% sodium chloride aqueous solution, then cleanup using GPC, and finally, analysis using LC-MS/MS. High recoveries from the GPC column were obtained for all rodenticides tested using a mobile phase of acetone/cyclohexane/triethylamine (400:1600:1, v/v/v). An ODS column, which contains low levels of metal impurities, gave satisfactory peak shapes for both hydroxycoumarin- and indandione-type rodenticides in the LC-MS/MS separation. The average recoveries of rodenticides from eight agricultural foods (apple, eggplant, cabbage, orange, potato, tomato, brown rice, and soybean) fortified at 0.0005-0.001 mg/kg ranged from 76 to 116%, except for bromadiolone in orange (53%) and diphacinone in soybean (54%), and the relative standard deviations ranged from 1 to 16%. The proposed method effectively removed interfering components, such as pigments and lipids, and showed high selectivity. In addition, the matrix effects were negligible for most of the rodenticide/food combinations. The results suggest that the proposed method is reliable and suitable for determining hydroxycoumarin- and indandione-type rodenticides in agricultural products.

  10. Simultaneous determination of dihydrotestosterone and its metabolites in mouse sera by LC-MS/MS with chemical derivatization.

    Science.gov (United States)

    Gorityala, Shashank; Yang, Shuming; Montano, Monica M; Xu, Yan

    2018-07-15

    Androgens play a vital role in prostate cancer development, and their elimination and blockade are essential in the disease management. DHT is the key ligand for androgen receptor (AR) in the prostate. It is locally synthesized from testosterone. In the prostate, DHT is predominantly metabolized to α-diol and β-diol. Recent studies indicate that impaired DHT catabolism is associated with prostate cancer, signifying the necessity of a sensitive quantitative method for the determination of DHT and its metabolites. In this work, an LC-MS/MS method for the simultaneous quantification of DHT and its metabolites was developed and validated. Steroid-free sera were prepared and used for the preparation of sera calibrators and quality controls (QCs). DHT and its metabolites along with their respective stable heavy isotope labeled analytes representing internal standards were first extracted with methyl tertiary-butyl ether (MTBE) and derivatized with picolinic acid (PA). The derivatized analytes were then extracted again with MTBE, dried under nitrogen and reconstituted in the mobile phase (80% methanol and 0.2% formic acid in water). Baseline chromatographic separation of the derivatized analytes was achieved isocratically on XTerra C18 column (2.1 × 100 mm) using the mobile phase at a flow rate of 0.25 mL/min. Quantitation was performed using multiple-reaction-monitoring mode with positive electrospray ionization. The method has calibration ranges from 0.0500 ng/mL to 50.0 ng/mL for DHT and its two metabolites with acceptable assay precision, accuracy, recovery, and matrix factor. It was applied to the determination of DHT and its metabolites in an animal study. Copyright © 2018 Elsevier B.V. All rights reserved.

  11. Simultaneous determination of secondary metabolites from Vinca rosea plant extractives by reverse phase high performance liquid chromatography

    Science.gov (United States)

    Siddiqui, Mohammad Jamshed Ahmad; Ismail, Zhari; Saidan, Noor Hafizoh

    2011-01-01

    Background: Vinca rosea (Apocynaceae) is one of the most important and high value medicinal plants known for its anticancer alkaloids. It is the iota of the isolated secondary metabolites used in chemotherapy to treat diverse cancers. Several high performance liquid chromatography (HPLC) methods have been developed to quantify the active alkaloids in the plant. However, this method may serve the purpose in quantification of V. rosea plant extracts in totality. Objective: To develop and validate the reverse phase (RP)-HPLC method for simultaneous determination of secondary metabolites, namely alkaloids from V. rosea plant extracts. Materials and Methods: The quantitative determination was conducted by RP-HPLC equipped with ultraviolet detector. Optimal separation was achieved by isocratic elution with mobile phase consisting of methanol:acetonitrile:ammonium acetate buffer (25 mM) with 0.1% triethylamine (15:45:40 v/v) on a column (Zorbax Eclipse plus C18, 250 mm % 4.6 mm; 5 μm). The standard markers (vindoline, vincristine, catharanthine, and vinblastine) were identified by retention time and co-injected with reference standard and quantified by external standard method at 297 nm. Results: The precision of the method was confirmed by the relative standard deviation (R.S.D.), which was lower than 2.68%. The recoveries were in the range of 98.09%-108%. The limits of detection (LOD) for each marker alkaloids were lower than 0.20 μg. Different parts of the V. rosea extracts shows different concentrations of markers, flower samples were high in vinblastine content, while methanol extract from the leaves contains all the four alkaloids in good yield, and there is no significant presence of markers in water extracts. Conclusion: HPLC method established is appropriate for the standardization and quality assurance of V. rosea plant extracts. PMID:21716929

  12. Validation of a liquid chromatography method for the simultaneous determination of sulfadimethoxine and trimethoprim and application to a stability study.

    Science.gov (United States)

    Louati, K; Mistiri, F; Kallel, M; Safta, F

    2010-03-01

    A liquid chromatography method is described for the simultaneous determination of sulfadimetoxine and trimethoprim from a veterinary formulation at the proportion of 187 mg and 40 mg respectively in presence of some excipient. The solution was subjected to different International Conference On Harmonisation prescribed stress conditions (hydrolysis, oxidation and photolysis). A stability-indicating high-performance liquid chromatography method was developed for the analysis of active substances in presence of their major degradation products. It involved a Knauer Eurospher C18 thermostated column at 25 degrees C, and 9.57 mM phosphate buffer (pH adjusted to 2.0 with orthophosphoric acid)-acetonitrile (70:30 v/v) as mobile phase. The mobile phase flow rate and sample volume injected were 1.2 mL/min and 20 microL, respectively. The selected wavelength for the determination was 248 nm. The method was validated for linearity, precision, accuracy and specificity, and then applied to a stability study of sulfadimetoxine and trimethoprim in the veterinary solution packaged in high density polyethylene plastic bottles of 1 L and 100 mL thermosealed and no thermosealed and corked by a white cap, at both accelerated and long-term conditions required by the International Conference On Harmonisation. The method developed, which separates all of the most degradation products formed under variety of conditions, proved to be simple, accurate, precise and specific. The results of the stress degradation show that the solution is more sensitive to hydrolysis. The stability studies carried out on three batches of each presentation show that the finished product remains stable for six months. Copyright 2010 Elsevier Masson SAS. All rights reserved.

  13. First liquid chromatography method for the simultaneous determination of levofloxacin, pazufloxacin, gatifloxacin, moxifloxacin and trovafloxacin in human plasma.

    Science.gov (United States)

    Sousa, Joana; Alves, Gilberto; Campos, Gonçalo; Fortuna, Ana; Falcão, Amílcar

    2013-07-01

    For the first time a simple, selective and sensitive liquid chromatography method was developed and validated for the simultaneous determination of levofloxacin (LEV), pazufloxacin (PAZ), gatifloxacin (GAT), moxifloxacin (MOX) and trovafloxacin (TRO) in human plasma. Samples were pre-treated with acetonitrile for precipitation of plasma proteins followed by evaporation and reconstitution steps. Chromatographic separation of the analytes and norfloxacin, used as internal standard (IS), was performed under gradient elution on a LiChroCART(®) Purospher Star C18 column (55mm×4mm, 3μm). The mobile phase comprised a mixture of 0.1% aqueous formic acid adjusted to pH 3.0 with triethylamine, acetonitrile and methanol pumped at a flow rate of 1.0mL/min. The detector was set at excitation/emission wavelengths of 260/455nm. Calibration curves were linear (r(2)≥0.9923) in the ranges of 0.005-5μg/mL for GAT, 0.02-5μg/mL for LEV, PAZ and MOX and 0.04-5μg/mL for TRO. The intra and interday precision did not exceed 7.32% and the intra and interday accuracy ranged from -11.73 to 8.92%. The limits of quantification were established at 0.005μg/mL for GAT, 0.02μg/mL for LEV, PAZ and MOX and 0.04μg/mL for TRO. No endogenous or tested exogenous compounds were found to interfere at the retention times of the analytes and IS. Since the proposed method proved to be reliable for the quantitative determination of LEV, PAZ, GAT, MOX and TRO it may be a useful tool for routine analysis and to support clinical pharmacokinetic and toxicological studies involving these antibiotics. Copyright © 2013 Elsevier B.V. All rights reserved.

  14. Simultaneous determination of CRP and D-dimer in human blood plasma samples with White Light Reflectance Spectroscopy.

    Science.gov (United States)

    Koukouvinos, Georgios; Petrou, Panagiota; Misiakos, Konstantinos; Drygiannakis, Dimitris; Raptis, Ioannis; Stefanitsis, Gerasimos; Martini, Spyridoula; Nikita, Dimitra; Goustouridis, Dimitrios; Moser, Isabella; Jobst, Gerhard; Kakabakos, Sotirios

    2016-10-15

    A dual-analyte assay for the simultaneous determination of C-reactive protein (CRP) and D-dimer in human blood plasma based on a white light interference spectroscopy sensing platform is presented. Measurement is accomplished in real-time by scanning the sensing surface, on which distinct antibody areas have been created, with a reflection probe used both for illumination of the surface and collection of the reflected interference spectrum. The composition of the transducer, the sensing surface chemical activation and biofunctionalization procedures were optimized with respect to signal magnitude and repeatability. The assay format involved direct detection of CRP whereas for D-dimer a two-site immunoassay employing a biotinylated reporter antibody and reaction with streptavidin was selected. The assays were sensitive with detection limits of 25ng/mL for both analytes, precise with intra- and inter-assay CV values ranging from 3.6% to 7.7%, and from 4.8% to 9.5%, respectively, for both assays, and accurate with recovery values ranging from 88.5% to 108% for both analytes. Moreover, the values determined for the two analytes in 35 human plasma samples were in excellent agreement with those received for the same samples by standard diagnostic laboratory instrumentation employing commercial kits. The excellent agreement of the results supported the validity of the proposed system for clinical application for the detection of multiple analytes since it was demonstrated that up to seven antibody areas can be created on the sensing surface and successfully interrogated with the developed optical set-up. Copyright © 2015. Published by Elsevier B.V.

  15. Simultaneous Determination of 14 Phenolic Compounds in Grape Canes by HPLC-DAD-UV Using Wavelength Switching Detection

    Directory of Open Access Journals (Sweden)

    Ang Zhang

    2013-11-01

    Full Text Available The paper described a novel chromatographic method for the simultaneous determination of phenolic compounds such as gallic, protocatechuic, vanillic, caffeic, syringic, p-coumaric and salicylic acid, (+-catechin, (‒-epicatechin, rutin, morin, quercetin, coumarin and trans-resveratrol at their maximum absorbance wavelengths (MAW employing reverse-phase high performance liquid chromatography combined with DAD and UV detection via detection wavelength switching. The method was based on MAW acquisition by DAD and quantification by UV. The separation process was performed on a Shim-Pack VP-ODS C18 column (250 mm × 4.6 mm, 5 μm held at 30 °C, utilizing 3.0% acetic acid and acetonitrile as mobile phase at a flow rate of 0.8 mL/min in the gradient elution mode. The method was fully validated in terms of linearity (r2 > 0.9990, 10‒350 mg/L, precision (both intra-day and inter-day RSD < 4.22%, accuracy (97.31%‒104.66%, specificity, robustness (0.59% < RSD < 2.86%, limit of detection and quantification. The switching method significantly improved the sensitivities of most phenolics studied in comparison with the standard constant wavelength detection (280 nm. The proposed method has been successfully applied to the determination of 14 phenolic compounds in 89 varieties of one-year-old Chinese grape one-year-canes. Grape canes contain many phenolics, especially trans-resveratrol, (‒-epicatechin, and (+-catechin.

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

    Science.gov (United States)

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

    2017-01-05

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

  17. Simultaneous Determination of Source Wavelet and Velocity Profile Using Impulsive Point-Source Reflections from a Layered Fluid

    National Research Council Canada - National Science Library

    Bube, K; Lailly, P; Sacks, P; Santosa, F; Symes, W. W

    1987-01-01

    .... We show that a quasi-impulsive, isotropic point source may be recovered simultaneously with the velocity profile from reflection data over a layered fluid, in linear (perturbation) approximation...

  18. Simultaneous determination of exponential background and Gaussian peak functions in gamma ray scintillation spectrometers by maximum likelihood technique

    International Nuclear Information System (INIS)

    Eisler, P.; Youl, S.; Lwin, T.; Nelson, G.

    1983-01-01

    Simultaneous fitting of peaks and background functions from gamma-ray spectrometry using multichannel pulse height analysis is considered. The specific case of Gaussian peak and exponential background is treated in detail with respect to simultaneous estimation of both functions by using a technique which incorporates maximum likelihood method as well as a graphical method. Theoretical expressions for the standard errors of the estimates are also obtained. The technique is demonstrated for two experimental data sets. (orig.)

  19. Standardization of HPTLC method for the estimation of oxytocin in edibles.

    Science.gov (United States)

    Rani, Roopa; Medhe, Sharad; Raj, Kumar Rohit; Srivastava, Manmohan

    2013-12-01

    Adulteration in food stuff has been regarded as a major social evil and is a mind-boggling problem in society. In this study, a rapid, reliable and cost effective High Performance thin layer Chromatography (HPTLC) has been established for the estimation of oxytocin (adulterant) in vegetables, fruits and milk samples. Oxytocin is one of the most frequently used adulterant added in vegetables and fruits for increasing the growth rate and also to enhance milk production from lactating animals. The standardization of the method was based on simulation parameters of mobile phase, stationary phase and saturation time. The mobile phase used was MeOH: Ammonia (pH 6.8), optimized stationary phase was silica gel and saturation time of 5 min. The method was validated by testing its linearity, accuracy, precision, repeatability and limits of detection and quantification. Thus, the proposed method is simple, rapid and specific and was successfully employed for quality and quantity monitoring of oxytocin content in edible products.

  20. Simultaneous determination and stability studies of linezolid, meropenem and vancomycin in bacterial growth medium by high-performance liquid chromatography.

    Science.gov (United States)

    Wicha, Sebastian G; Kloft, Charlotte

    2016-08-15

    For pharmacokinetic/pharmacodynamic (PK/PD) assessment of antibiotics combinations in in vitro infection models, accurate and precise quantification of drug concentrations in bacterial growth medium is crucial for derivation of valid PK/PD relationships. We aimed to (i) develop a high-performance liquid chromatography (HPLC) assay to simultaneously quantify linezolid (LZD), vancomycin (VAN) and meropenem (MER), as typical components of broad-spectrum antibiotic combination therapy, in bacterial growth medium cation-adjusted Mueller-Hinton broth (CaMHB) and (ii) determine the stability profiles of LZD, VAN and MER under conditions in in vitro infection models. To separate sample matrix components, the final method comprised the pretreatment of 100μL sample with 400μL methanol, the evaporation of supernatant and its reconstitution in water. A low sample volume of 2μL processed sample was injected onto an Accucore C-18 column (2.6μm, 100×2.1mm) coupled to a Dionex Ultimate 3000 HPLC+ system. UV detection at 251, 240 and 302nm allowed quantification limits of 0.5, 2 and 0.5μg/mL for LZD, VAN and MER, respectively. The assay was successfully validated according to the relevant EMA guideline. The rapid method (14min) was successfully applied to quantify significant degradation of LZD, VAN and MER in in vitro infection models: LZD was stable, VAN degraded to 90.6% and MER to 62.9% within 24h compared to t=0 in CaMHB at 37°C, which should be considered when deriving PK/PD relationships in in vitro infection models. Inclusion of further antibiotics into the flexible gradient-based HPLC assay seems promising. Copyright © 2016 Elsevier B.V. All rights reserved.