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

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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Determination of trace amounts of morphine in human plasma by anodic adsorptive stripping differential pulse voltammetry

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Chinese Chemical Letters 2008年第4期19卷 465-468页

作者： Ali Niazi Ateesa Yazdanipour Department of Chemistry Faculty of SciencesAzad University of ArakArakIran

New adsorptive anodic differential pulse stripping voltammetry method for the direct determination of morphine at trace levels in human plasma of addicts is *** procedure involves an adsorptive accumulation of morphine on a HMDE,followed by oxidation of adsorbed morphine by voltammetry scan using differential pulse *** optimum conditions for the analysis of morphine are pH 10.5,Eacc of -100 mV（***/AgCl）,and tacc of 120 *** peak current is proportional to the concentration of morphine,and a Linear calibration graph is obtained at 0.01-3.10μg mL^-1.A relative standard deviation of 1.06%（n=5）was obtained,and the limit of detection was 3 ng mL^-*** capabiLity of the method for the analysis of real samples was evaluated by the determination of morphine in spiked human plasma and addicts human plasma with satisfactory results.

关键词： Morphine Adsorptive differential pulse voltammetry 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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Rapid and Sensitive LC-MS/MS Method for Quantification of Fexofenadine in human plasma——Application to a Bioequivalence Study in Chinese Volunteers

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Chemical Research in Chinese Universities 2007年第5期23卷 514-517页

作者： TENG Guo-sheng TENG Le-sheng WU Yi TANG Yun-biao LIU Lan-ying GU Jing-kai　 Research Center for Drug Metabolism College of Life Science School of Pharmaceutical Science Jilin University Changchun 130021 P. R. China Department of Pharmacy General Hospital of Shenyang Military Command Shenyang 110016 P. R. China

A rapid and sensitive liquid chromatography-tandem mass spectrometry method（LC-MS/MS）was developed and validated for the quantification of fexofenadine in human plasma,to conduct comparative bioavailability *** plasma was extracted with a mixture of dichloromethane-diethyl ether（volume ratio 2∶3）in a basic environment and the extract was separated on a C18 column with a mobile phase consisting of acetonitrile-methanol-10 mmol/L ammonium acetate（volume ratio 45∶45∶10）.The analytes were detected via electrospray ionization（ESI）tandem mass spectrometry in the multiple-reaction-monitoring（MRM）*** linearity was within a range of 1-1000 ng/*** intra-and inter-day precision were〈4.1% and〈4.8%,respectively,and the accuracy was in the range of 95.0%-105%.The method was applied to the quantification of fexofenadine human plasma from 20 healthy male Chinese volunteers,according to a single dose,randomized,two-way crossover design with a two-week washout *** mean values of major pharmacokinetic parameters of ρmax,AUC0-48,AUC0-∞,tmax,and t1/2 were determined from the plasma *** analysis of variance（ANOVA）did not show any significant difference between the two products of fexofenadine and 90% confidence intervals fell within the acceptable range for bioequivalence.

关键词： Fexofenadine Bioequivalence LC-MS/MS human plasma

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Rapid Determination of Ranitidine in human plasma by Liquid Chromatography-Tandem Mass Spectrometry and Its Application to a Clinical Pharmacokinetic Study

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Chemical Research in Chinese Universities 2010年第6期26卷 910-914页

作者： ZHANG Chao WANG Lu GUAN Xin J. Paul Fawcett ZHAO Li-mei SUN Yan-tong GU Jing-kai Research Center for Drug Metabolism College of Life Science Jilin University Changchun 130021 P R. China Liaoning Province Academy of Analytic Science Shenyang 110015 P. R. China School of Pharmacy University of Otago PO Box 56 Dunedin New Zealand Second Clinical Hospital Affiliated to the Chinese Medical University Shenyang 110004 P. R. China

A rapid and sensitive assay based on high performance liquid chromatography-tandem mass spectrometry（LC-MS/MS） was developed for the determination of ranitidine（RAN） in human plasma with codeine as internal standard（IS）.After protein precipitation with acetonitrile,the analyte and IS were separated on a Zorbax SB-Aq C18 column（150 mm×4.6 mm i.d.,5 μm） eluted with a mobile phase consisting of methanol/acetonitrile/10 mmol/L ammonium acetate containing 1% formic acid（pH=2.4）（volume ratio 12.5：12.5：75） at a flow rate of 1.0 mL/*** was performed by electrospray ionization in the positive ion mode followed by the multiple reaction monito-ring（MRM） of the transitions of RAN at m/z 315.1→176.3 and of IS at m/z 300.1→*** method was linear over a concentration range of 1―1000 ng/mL（r=0.9991） with a lower limit of quantitation（LLOQ） of 1 ng/mL and a limit of detection（LOD） of 0.3 ng/*** as relative error was from-0.01% to-1.7% and intra-day and inter-day precisions as relative standard deviation were ≤8.9% and ≤5.5%,*** method was successfully applied to a pharmacokinetic study of ranitidine,getting a single oral dose（160 mg） to healthy volunteers.

关键词： Ranitidine Pharmacokinetics human plasma Protein precipitation LC-MS/MS

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Development of a Rapid and Simultaneous Detection Method for Buprenorphine, Norbuprenorphine and Naloxone in human plasma Using Ultra-high Performance Liquid Chromatography- tandem Mass Spectrometer with Solid-phase Extraction

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Chinese Journal of Chemistry 2011年第9期29卷 1922-1926页

作者： Guo, Qiaozhen Du, Zhenxia Faculty of Science Beijing University of Chemical Technology Beijing 100029 China

A simultaneous method was successfully established and validated for the separation and determination of bu- prenorphine （BP）, its primary metabolite, nor-buprenorphine （NBP） and a proposed co-formulate, naloxone （NLX） in human plasma. The method used buprenorphine-d4 （BP-D4）, nor-buprenorphine-d3 （NBP-D3）, naltrexone （NTX） as internal standards （ISs）. 100 μL of plasma sample fortified with the ISs was cleaned up by solid-phase extraction （SPE）, and was then separated on a Waters AcquityTM BEH C18 column with gradient elution using methanol and water （containing 0.2% formic） at a flow rate of 0.25 mL·min^-1. The mass spectrometer was used for detection and was operated in the positive electrospray ionization with multiple reaction monitoring （MRM） mode. The three compounds were effectively separated in 5 min. The linear ranges of the compounds were 0.1--25, 0.25--25 and 0.05--25 ng·mL^-1 for BP, NBP and NLX, respectively, with r≥0.9935. The method had high sensitivity （the lim- its of detection were 0.02, 0.1 and 0.01 ***-1 for BP, NBP and NLX, respectively） and high recoveries （≥97.6%）. The result was shown to be linear and satisfactorily met current acceptance criteria for validation of bio- analytical method： intra and inter assay precisions within the required limits of ≤25% RSD. The LOQs fulfilled the LOQ requirements： precision≤25% RSD, and was fully validated according to the State Food and Drug Administration （SFDA） regulations. The results demonstrated that ultra-high performance liquid chromatography- tandem mass spectrometer （UPLC-MS/MS） with SPE was a powerful detection tool and contributed to pharmaceutical analysis in biological matrices.

关键词： ultra-high performance liquid chromatography-tandem mass spectrometer buprenorphine naloxone,norbuprenorphine human plasma

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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 *** 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 *** 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 *** 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,*** established method has been validated according to regulatory guideline,and the results were all within the acceptance *** 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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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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