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Journal of Pharmaceutical Analysis 2017年第3期7卷 163-169页

作者： jaivik v.shah Priyanka A.shah Priya v.shah Mallika Sanyal Pranav S.Shrivastav Department of Chemistry School of Sciences Gujarat University Department of Pharmacy M.S.University Department of Chemistry St.Xavier's College

A sensitive and rapid liquid chromatography-tandem mass spectrometry(LC–MS/MS) method has been developed for the simultaneous determination of lisinopril(LIS) and hydrochlorothiazide(HCTZ) in human plasma using their labeled internal standards(ISs). Sample pre-treatment involved solid phase extraction on Waters Oasis HLB cartridges using 100 μL of plasma, followed by liquid chromatography on Hypersil Gold C_(18)(50 mm×3.0 mm, 5 μm) column. The analytes were eluted within 2.0 min using acetonitrile-5.0 m M ammonium formate, p H 4.5(85:15, v/v) as the mobile phase. The analytes and ISs were analyzed in the negative ionization mode and quantified using multiple reaction monitoring. The method showed excellent linearity over the concentration range of 0.50–250.0 ng/m L for both the analytes. The intra-batch and inter-batch precision(% Cv) was ≤5.26% and their extraction recoveries were in the range of 96.6%–103.1%. Matrix effect evaluated in terms of IS-normalized matrix factors ranged from 0.97 to 1.03 for both the analytes. The validated method was successfully applied to determine the plasma concentration of the drugs using 10 mg lisinopril and 12.5 mg hydrochlorothiazide fixed dose formulation in 18 healthy Indian volunteers.

关键词： Lisinopril Hydrochlorothiazide LC–MS/MS Solid phase extraction Human plasma

Simultaneous quantification of amiloride and hydrochlorothiazide in human plasma by liquid chromatography–tandem mass spectrometry

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Journal of Pharmaceutical Analysis 2017年第5期7卷 288-296页

作者： jaivik v.shah Priyanka A.shah Mallika Sanyal Pranav S.Shrivastav Department of Chemistry School of Sciences Gujarat University Department of Chemistry St.Xavier's College

A selective, sensitive and precise assay based on solid phase extraction and liquid chromatography–tandem mass spectrometry(LC–MS/MS) was developed for the simultaneous determination of amiloride(AMI) and hydrochlorothiazide(HCTZ) in human plasma. Sample clean-up with 250 μL of plasma was done on Phenomenex Strata^(?)-X extraction cartridges using their labeled internal standards(AMI-15 N3 and HCTZ-13 C,d2). Chromatography was performed on Hypersil Gold C18(50 mm×3.0 mm, 5 μm) column using acetonitrile with 4.0 m M ammonium formate(p H 4.0, adjusted with 0.1% formic acid)(80:20, v/v) as the mobile phase. Detection was carried out on a triple quadrupole API 5500 mass spectrometer utilizing an electrospray ionization interface and operating in the positive ionization mode for AMI and negative ionization mode for HCTZ. Multiple reaction monitoring was used following the transitions at m/z 230.6/116.0, m/z233.6/116.0, m/z 296.0/204.9 and m/z 299.0/205.9 for AMI, AMI-15 N3, HCTZ and HCTZ-13 C,d2,respectively. Calibration curves were linear(r2≥0.9997) over the concentration range of 0.050–50.0 and0.50–500 ng/m L for AMI and HCTZ, respectively, with acceptable accuracy and precision. The signal-to-noise ratio at the limit of quantitation was ≥14 for both the analytes. The mean recovery of AMI and HCTZ from plasma was 89.0% and 98.7%, respectively. The IS-normalized matrix factors determined for matrix effect ranged from 0.971 to 1.024 for both the analytes. The validated LC–MS/MS method was successfully applied to a bioequivalence study using 5 mg AMI and 50 mg HCTZ fixed dose tablet formulation in 18 healthy Indian volunteers with good reproducibility.

关键词： Amiloride Hydrochlorothiazide LC–MS/MS Solid phase extraction Human plasma

Application of an LC–MS/MS method for the analysis of amlodipine,valsartan and hydrochlorothiazide in polypill for a bioequivalence study

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Journal of Pharmaceutical Analysis 2017年第5期7卷 309-316页

作者： jaivik v.shah Jignesh M.Parekh Priyanka A.shah Priya v.shah Mallika Sanyal Pranav S.Shrivastav Department of Chemistry School of Sciences Gujarat University Department of Chemistry St.Xavier's College Department of Pharmacy M.S.University

A sensitive and selective method has been proposed for the simultaneous determination of amlodipine(AML),valsartan(vAL) and hydrochlorothiazide(HCTZ) in human plasma by liquid chromatography–tandem mass spectrometry(LC–MS/MS). The analytes and their deuterated analogs were quantitatively extracted from100 μL human plasma by solid phase extraction on Oasis HLB cartridges. The chromatographic separation of the analytes was achieved on a Chromolith RP18 e(100 mm × 4.6 mm) analytical column within 2.5 min. The resolution factor between AML and vAL, AML and HCTZ, and vAL and HCTZ was 2.9, 1.5 and 1.4, respectively,under isocratic conditions. The method was validated over a dynamic concentration range of 0.02–20.0 ng/m L for AML, 5.00–10,000 ng/m L for vAL and 0.20–200 ng/m L for HCTZ. Ion-suppression/enhancement effects were investigated by post-column infusion technique. The mean IS-normalized matrix factors for AML, vAL and HCTZ were 0.992, 0.994 and 0.998, respectively. The intra-batch and inter-batch precision(% Cv) across quality control levels was ≤ 5.56% and the recovery was in the range of 93.4%–99.6% for all the analytes. The method was successfully applied to a bioequivalence study of 5 mg AML + 160 mg vAL + 12.5 mg HCTZ tablet formulation(test and reference) in 18 healthy Indian males under fasting. The mean log-transformed ratios of C max, AUC0–120 h and AUC0-inf and their 90% CIs were within 90.2%–102.1%. The assay reproducibility was demonstrated by reanalysis of 90 incurred samples.

关键词： Amlodipine valsartan Hydrochlorothiazide LC–MS/MS Polypill Bioequivalence

SPE-UPLC-MS/MS assay for determination of letrozole in human plasma and its application to bioequivalence study in healthy postmenopausal Indian women

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Journal of Pharmaceutical Analysis 2016年第4期6卷 276-281页

作者： Pravin G.vanol Puran Singhal Priyanka A.shah jaivik v.shah Pranav S.Shrivastav Mallika Sanyal Chemistry Department St.Xavier's College Bioanalytical Department Alkem Laboratories Ltd. Department of Chemistry School of SciencesGujarat University

A rapid and sensitive ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） method is described for determination of letrozole in human *** solid phase extraction（SPE） of letrozole and letrozole-d4 on Orochem DvB-LP cartridges,chromatography was performed on Acquity UPLC BEH C_（18）（50 mm × 2.1 mm.1.7 μm） column using methanol-0.1%formic acid in water（85：15,v/v） as the mobile *** was carried out on a triple quadrupole mass spectrometer with an electrospray source,operated under positive ionization *** of letrozole and letrozole-d4 was done using multiple reaction monitoring（MRM） following the transitions at m/z286.2→217.0 and m/z 290.2→221.0,*** calibration plots were linear through the concentration range of 0.10-100 ng/mL（r^2 ≥ 0.9990） using 100 μL human *** extraction recovery of letrozole ranged from 94.3%to 96.2%and the intra-batch and inter-batch precision was ≤ 5.2%.The method was successfully applied to a bioequivalence study of letrozole after oral administration of2.5 mg tablet formulation to 16 healthy postmenopausal Indian *** assay reproducibility was also established through incurred sample reanalysis（ISR） of 74 subject samples.

关键词： Letrozole Letrozole-D4 UPLC-MS/MS Solid phase extraction Bioequivalence study

Determination of lercanidipine in human plasma by an improved UPLC–MS/MS method for a bioequivalence study

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Journal of Pharmaceutical Analysis 2016年第2期6卷 87-94页

作者： Darshan v.Chaudhary Daxesh P.Patel Priyanka A.shah jaivik v.shah Mallika Sanyal Pranav S.Shrivastav Department of Chemistry School of Sciences Gujarat University Navrangpura Ahmedabad Gujarat 380009 India Laboratory of Metabolism Center for Cancer Research National Cancer Institute National Institutes of Health Building 37 Room 3106 Bethesda MD 20892 USA Department of Chemistry St. Xavier's College Navrangpura Ahmedabad Gujarat 380009 India

An improved and reliable ultra-performance liquid chromatography/tandem mass spectrometry （UPLC- MS/MS） method has been developed and validated for the determination of lercanidipine in human plasma. Plasma samples with lercanidipine-d3 as an internal standard （IS） were prepared by solid phase extraction on Phenomenex Strata-X cartridges using 100 μL of human plasma. Chromatographic analysis was performed on UPLC BEH C18 （50 mm × 2.1 mm, 1.7 μm） column under isocratic conditions. Linear calibration curves were obtained over a wide dynamic concentration range of 0.010-20.0 ng/mL. Matrix effect was assessed by post-column infusion, post-extraction spiking and standard-line slope methods. The mean extraction recovery was 〉 94% for the analyte and IS. Inter-batch and intra-hatch precision （% Cv） across five quality controls was 〈 5.8%. Bioequivalence study was performed with 36 healthy sub- jects after oral administration of 10 mg of lercanidipine and the assay reproducibility was evaluated by reanalysis of 133 incurred samples.

关键词： Lercanidipine UPLC-MS/MS Bioequivalence Solid phase extraction Human plasma