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A sensitive and validated LC-MS/MS method for high-throughput determination of pomalidomide in human plasma and pharmacokinetic studies

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Chinese Chemical Letters 2022年第2期33卷 916-919页

作者： Chang Shu Teng-Fei Li Duo Li Zhong-Qiu Li Xing-Hua Xia State Key Laboratory of Analytical Chemistry for Life Science School of Chemistry and Chemical EngineeringNanjing UniversityNanjing 210023China Department of Pharmaceutical Analysis School of PharmacyChina Pharmaceutical UniversityNanjing 210009China School of Pharmacy Department of Clinical PharmacologySir Run HospitalNanjing Medical UniversityNanjing 211166China

Pomalidomide is an immunomodulatory agent (IMiD) that has been approved by the US Food and Drug Administration (FDA) for clinical treatment of patients with multiple myeloma.In this work,we developed a sensitive and validated LC-MS/MS method for high-throughput determination of pomalidomide over the range of 1.006-100.6 ng/mL(R^(2)=0.9991) in human plasma and pharmacokinetic studies.A liquid-liquid extraction method using ethyl acetate was applied to extract pomalidomide and afatinib (as an internal standard,IS) from human plasma.Chromatographic separation was performed on a Hedera ODS column (150 mm×2.1 mm,5μm) with security guard C18 column (4 mm×2.0 mm) at 40℃.Methanol and 10 mmol/L aqueous solution of ammonium acetate containing 0.1%formic acid were used as a gradient elution mobile phase,and the flow rate was 0.4 mL/min.A triple quadruple tandem mass spectrometer using multiplex reaction monitoring mode (MRM) with electrospray ionization (ESI) positive ionization was employed.The precursor to product ion transitions for the quantitative analysis of pomalidomide and the IS were m/z 274.2→163.1 and m/z 486.1→371.1,respectively.This established method has been validated according to regulatory guideline,and the results were all within the acceptance criteria.The validated LC-MS/MS method was successfully applied to analyze samples obtained from clinical pharmacokinetics study after oral administration of pomalidomide (4 mg) capsules in human.

关键词： Pomalidomide Liquid-liquid extraction LC–MS/MS method Pharmacokinetic human plasma

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Quantitation of tadalafil in human plasma using a sensitive and rapid LC-MS/MS method for a bioequivalence study

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Journal of Pharmaceutical Analysis 2018年第4期8卷 271-276页

作者： Abhaysingh Bhadoriya Bhavesh Dasandi Dharmesh Parmar Priyanka A. Shah Pranav S. Shrivastav Bioanalytical Department Synchron Research Services Pvt. Ltd. Department of Chemistry School of Sciences Gujarat University

A highly sensitive liquid chromatography-tandem mass spectrometry（LC-MS/MS） method was developed for the determination of tadalafil（TAD） in human plasma. TAD and its deuterated internal standard（IS）, tadalafil-d3, were extracted from 200 mL plasma using Phenomenex Strata-X-C 33 m extraction cartridges. Chromatographic analysis was carried out on Synergi Hydro-RP C18（100 mm × 4.6 mm, 4 mm）column with a mobile phase consisting of methanol and 10 m M ammonium formate, p H 4.0（90：10, v/v）,delivered at a flow rate of 0.9 m L/min. Quantitation of the protonated analyte was done on a triple quadrupole mass spectrometer using multiple reaction monitoring via electrospray ionization. The precursor to product ions transitions monitored for TAD and TAD-d3 were m/z 390.3-268.2 and m/z393.1-271.2, respectively. The calibration curve was linear over the concentration range of 0.50–500 ng/m L with correlation coefficient, r2 Z 0.9994. Acceptable intra-batch and inter-batch precision（r3.7%） and accuracy（97.8% to 104.1%） were obtained at five concentration levels. The recovery of TAD from spiked plasma was highly precise and quantitative（98.95% to 100.61%）. Further, the effect of endogenous matrix components was minimal. TAD was found to be stable under different storage conditions in human plasma and also in whole blood samples. The validated method was successfully used to determine TAD plasma concentration in a bioequivalence study with 20 mg TAD tablets in 24 healthy volunteers. Method performance was evaluated by reanalyzing 115 study samples.

关键词： Tadalafil Tadalafil-d3 LC-MS/MS Sensitive Bioequivalence study human plasma

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Sensitive and rapid determination of amantadine without derivatization in human plasma by LC–MS/MS for a bioequivalence study

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Journal of Pharmaceutical Analysis 2018年第3期8卷 202-207页

作者： Abhaysingh Bhadoriya Shivprakash Rathnam Bhavesh DasANDi Dharmesh Parmar Mallika Sanyal Pranav S.Shrivastav Bioanalytical Department Synchron Research Services Pvt.Ltd Department of Chemistry St.Xavier's College Department of Chemistry School of Sciences Gujarat University

A highly sensitive, rapid and rugged liquid chromatography-tandem mass spectrometw （LC-ESI-MS/MS） method was developed for reliable estimation of amantadine （AMD）, an antiviral drug in human plasma. The analyte and internal standard （IS）, amantadine-d6 （AMD-d6）, were extracted from 200μL plasma by solid phase extraction on Phenomenex Strata-X-C 33 ~t cartridges. Chromatography was performed on Synergi^TM Hydro-RP C18 （150 mm×4.6 mm, 4 μm） analytical column using a mixture of acetonitrile and 10 mM ammonium formate, pH 3.0 （80：20, v/v） as the mobile phase. Detection and quantitation was done by multiple reaction monitoring in the positive ionization mode for AMD （m/z 152.1→ 135.1 ） and IS （m/z 158.0 → 141.1） on a triple quadrupole mass spectrometer. The assay was linear in the concentration range of 0.50-500 ng/mL with correlation coefficient （r^2）〉 0.9969. The limit of detection of the method was 0.18 ng/mL The intra-batch and inter-batch precisions were 〈 5.42% and the accuracy varied from 98.47% to 105.72%. The extraction recovery of amantadine was precise and quantitative in the range of 97.89%-100.28%. IS-normalized matrix factors for amantadine varied from 0.981 to 1.012. The stability of AMD in whole blood and plasma was evaluated under different conditions. The developed method was successfully applied for a bioequivalence study with 100 mg of AMD in 32 healthy volunteers. The reproducibility of the assay was determined by reanalysis of 134 subject samples.

关键词： Amantadine Amantadine-d6 LC-ESI-MS/MS Sensitive Bioequivalence study human plasma

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Determination of asenapine in presence of its inactive metabolites in human plasma by LC-MS/MS

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Journal of Pharmaceutical Analysis 2018年第5期8卷 341-347页

作者： Nirav R Patel Mallika Sanyal Naveen Sharma Dinesh S.Patel Pranav S.Shrivastav Bhavin N.Patel Bioanalytical Laboratory Uiantha Research India Ltd.BodakdevAhmedabad 380054GujaratIndia Kadi Sarva Viswavidyalaya Sector-15Ghandhinagar 382715GujaratIndia Department of Chemistry St.Xavier's CollegeNavrangpuraAhmedabad 380009GujaratIndia Department of Chemistry School of SciencesGujarat UniversityNavrangpuraAhmedabad 380009GujaratIndia

A highly selective and sensitive liquid chromatography-tandem mass spectrometry （LC-MS/MS） assay has been described for the determination of asenapine （ASE） in presence of its inactive metabolites N-desmethyl asenapine （DMA） and asenapine-N-glucuronide （ASG）. ASE, and ASE 13C-d3, used as internal standard （IS）, were extracted from 300 μL human plasma by a simple and precise liquid-liquid extraction procedure using methyl tert-butyl ether. Baseline separation of ASE from its inactive metabolites was achieved on Chromolith Performance RPse （100 mm ×4.6 mm） column using acetonitrile- 5.0 mM ammonium acetate-10% formic acid （90：10：0.1, v/v/v） within 4.5 min. Quantitation of ASE was done on a triple quadrupole mass spectrometer equipped with electrospray ionization in the positive mode. The protonated precursor to product ion transitions monitored for ASE and ASE 13C-d3 were m/z 286.1 → 166.0 and m/z 290.0 → 166.1, respectively. The limit of detection （LOD） and limit of quantitation （LOQ） of the method were 0.0025 ng/mL and 0.050 ng/mL respectively in a linear concentration range of 0.050-20.0 ng/mL for ASE. The intra-batch and inter-batch precision （% CV） and mean relative recovery across quality control levels were 〈 5.8% and 87.3%, respectively. Matrix effect, evaluated as IS-normalized matrix factor, ranged from 1.03 to 1.05. The stability of ASE under different storage conditions was ascertained in presence of the metabolites. The developed method is much simpler, matrix free, rapid and economical compared to the existing methods. The method was suc- cessfully used for a bioequivalence study of asenapine in healthy Indian subjects for the first time.

关键词： Asenapine Asenapine 13C-d3 Metabolites LC-MS/MS Bioequivalence study human plasma

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Simultaneous determination of acetaminophen and oxycodone in human plasma by LC–MS/MS and its application to a pharmacokinetic study

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Journal of Pharmaceutical Analysis 2018年第3期8卷 160-167页

作者： Wei Lu Shunbo Zhao Meng Gong Luning Sun Li Ding Department of Pharmaceutical Analysis China Pharmaceutical University 24 Tongjiaxiang Nanjing 210009 PR China Nanjing Clinical Tech Laboratories Inc. 18 Zhilan Road Jiangning District Nanjing 211000 PR China Research Division of Clinical Pharmacology the First Affiliated Hospital Nanjing Medical University Nanjing 210029 PR China

A simple and rapid liquid chromatography-tandem mass spectrometry （LC-MS/MS） method was de- veloped and validated for simultaneous determination of acetaminophen and oxycodone in human plasma. Acetaminophen-d4 and oxycodone-d3 were used as internal standards. The challenge en- countered in the method development that the high plasma concentration level of acetaminophen made the MS response saturated while the desired lower limit of quantification （LLOQ,） for oxycodone was hard to reach was well solved. The analytes were extracted by protein precipitation using acetonitrile. The matrix effect of the analytes was avoided by chromatographic separation using a hydrophilic C18 column coupled with gradient elution. Multiple reaction monitoring in positive ion mode was performed on tandem mass spectrometer employing electrospray ion source. The calibration curves were linear over the concentration ranges of 40.0-8000 ng/mL and 0.200-40.0 ng/mL for acetaminophen and oxycodone, respectively. This method, which could contribute to high throughput analysis and better clinical drug monitoring, was successfully applied to a pharmacokinetic study in healthy Chinese volunteers.

关键词： Acetaminophen Oxycodone LC-MS/MS human plasma Pharmacokinetics

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Simultaneous determination of 3-chlorotyrosine and 3-nitrotyrosine in human plasma by direct analysis in real time–tandem mass spectrometry

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Acta Pharmaceutica Sinica B 2015年第5期5卷 482-486页

作者： Yuqiao Song Jie Liao Cheng Zha Bin Wang Charles C.Liu Medical Experiment and Analysis Center of PLA General Hospital ASPEC Technologies Limited Beijing

A novel method for the simultaneous determination of 3-nitrotyrosine(NT) and 3-chlorotyrosine(CT) in human plasma has been developed based on direct analysis in real time–tandem mass spectrometry(DART–MS/MS). Analysis was performed in the positive ionization mode using multiple reaction monitoring(MRM) of the ion transitions at m/z 216.2/170.1 for CT, m/z 227.2/181.1 for NT and m/z 230.2/184.2 for the internal standard, d^3-NT. The assay was linear in the ranges 0.5–100 μg/m L for CT and 4–100 μg/m L for NT with corresponding limits of detection of 0.2 and 2 μg/m L. Intra- and inter-day precisions and accuracies were respectively <15% and ±15%. Matrix effects were also evaluated. The method is potentially useful for high throughput analysis although sensitivity needs to be improved before it can be applied in clinical research.

关键词： 3-Nitrotyrosine 3-Chlorotyrosine Determintion DART–MS/MS human plasma

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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

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Determination of torasemide in human plasma and its bioequivalence study by high-performance liquid chromatography with electrospray ionization tandem mass spectrometry

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Journal of Pharmaceutical Analysis 2016年第2期6卷 95-102页

作者： Lin Zhang Rulin Wang Yuan Tian Zunjian Zhang Key Laboratory of Drug Quality Control and Pharmacovigilance(Ministry of Education) China Pharmaceutical University State Key Laboratory of Natural Medicine China Pharmaceutical University

A sensitive and selective method using high-performance liquid chromatography coupled with elec- trospray ionization tandem mass spectrometry （HPLC-ESI-MS） to determine the concentration of tor- asemide in human plasma samples was developed and validated. Tolbutamide was chosen as the internal standard （IS）. The chromatography was performed on a GI Sciences Inertsil ODS-3 column （100 mm× 2.1 mm i.d., 5.0 μm） within 5 min, using methanol with 10 mM ammonium formate （60：40, v/ v） as mobile phase at a flow rate of 0.2 mL/min. The targeted compound was detected in negative io- nization at m/z 347.00 for torasemide and 269.00 for IS. The linearity range of this method was found to be within the concentration range of 1-2500 ng/mL （r=0.9984） for torasemide in human plasma. The accuracy of this measurement was between 94.05% and 103.86%. The extracted recovery efficiency was from 84.20% to 86.47% at three concentration levels. This method was also successfully applied in pharmacokinetics and bioequivalence studies in Chinese volunteers.

关键词： Torasemide HPLC-ESI-MS human plasma Bioequivalence Pharmacokinetics

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Development of a Liquid Chromatography-tandem Mass Spectrometry Method for Determination of Butoconazole Nitrate in human plasma and Its Application to a Pharmacokinetic Study

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Journal of Huazhong University of Science and Technology(Medical Sciences) 2014年第3期34卷 431-436页

作者：贾萌萌周莹何晓梦吴义来李虎群谌辉黎维勇 Institute of Clinical Pharmacy Union Hospital Tongji Medical College Huazhong University of Science and Technology

Summary： A liquid chromatography-tandem mass spectrometry （LC-MS/MS） method was developed and validated for the determination of butoconazole in human plasma. human plasma samples of 0.2 μL were pretreated by a single step protein precipitation procedure and analyzed using a high performance liquid chromatography （HPLC） electrospray tandem mass spectrometer system. The compounds were eluted isocratically on an Inertsil ODS-SP column （100 min×2.1 mm, 3 μm）, ionized using a positive ion atmospheric pressure electrospray ionization source and analyzed using multiple reaction monitoring （MRM） mode. The ion transitions monitored were m/z 412.8→q65.1 for butoconazole and m/z 453.4→230.3 for the internal standard. The chromatographic run time was 3.5 min per injection, with retention time of 2.47 rain and 2.15 min for butoconazole and repaglinide, respectively. The method was validated to be linear over the range of 20 to 8000 pg/mL （r〉0.999） by using a weighted （1/x2） quadratic regression. The mean recovery rate was more than 86.7%, and the intra- and inter-day precision of the quality control samples （QCs） was less than 8.3% and the accuracy ranged from 96.0% to 110.2%, which indicated that the quantitative method was reliable and accurate. The method is simple, rapid, and has been applied successfully to a pharmacokinetics study of butoconazole nitrate suppositories in healthy Chinese females.

关键词： liquid chromatography-tandem mass spectrometry human plasma pharmacokinetics bu- toconazole nitrate

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A Simple and Sensitive Liquid Chromatographic Technique for the Determination of Cefotetan Disodium in human plasma and Its Application in a Pharmacokinetic Study

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Journal of Huazhong University of Science and Technology(Medical Sciences) 2012年第5期32卷 779-784页

作者：刘亚妮黄建耿刘金梅马林吕永宁师少军 Clinical Trial Organization for Pharmaceutical Products Union HospitalTongji Medical CollegeHuazhong University of Science and Technology Department of Pharmaceutics School of PharmacyTongji Medical CollegeHuazhong University of Science and Technology

A simple and sensitive liquid chromatographic method was developed for quantification of cefotetan disodium (CTT),a semi-synthetic cephamycin antibiotic,in human plasma.CTT and the internal standard chloramphenicol were extracted from plasma by a simple one-step protein precipitation with 35% (v/v) perchloric acid.Separation was carried out on a reverse-phase C18 column with a mobile phase of acetonitile-water containing 0.5% (v/v) phosphoric acids (20:80,v/v) at a flow rate of 1.0 mL/min.The column effluent was monitored by UV detection at 300 nm.The column temperature was maintained at 40°C.This method demonstrated good linearity in the range of 0.525-300.0 μg/mL,with correlation coefficients greater than 0.99.The limit of quantification (LOQ) was 0.525 μg/mL in human plasma.Intra-and inter-day precisions were less than 6.63% in terms of relative standard deviation (RSD).The accuracy,when expressed by the bias,ranged from 0.57% to 4.04%.The mean extraction recovery of CTT was higher than 40.94%.The method was found to be precise,accurate,and specific for CTT quantitative analysis,and was successfully applied for a pharmacokinetic study of CTT after a single intravenous dose of 1.0 g of CTT in healthy Chinese subjects.

关键词： cefotetan disodium liquid chromatography human plasma pharmacokinetics

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