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Journal of Pharmaceutical Analysis 2022年第6期12卷 852-859页

作者： Takashi Mochizuki Kaito Shibata Takafumi Naito Kumiko Shimoyama Noriyoshi Ogawa Masato Maekawa Junichi Kawakami Department of Hospital Pharmacy Hamamatsu University School of MedicineHamamatsu431-3192Japan Department of Pharmacy Shinshu University HospitalMatsumotoNagano390-8621Japan Third Division Department of Internal MedicineHamamatsu University School of MedicineHamamatsu431-3192Japan Department of Laboratory Medicine Hamamatsu University School of MedicineHamamatsu431-3192Japan

The quantitation of serum tocilizumab using liquid chromatography tandem-mass spectrometry(lc-ms/ms)method has not been widely applied in clinical settings because of its time-consuming and costly sample *** present study aimed to develop a validated lc-ms/ms method for detecting serum tocilizumab by utilizing immobilized trypsin without an immunoglobulin G purification step and evaluate its applicability in the treatment of rheumatoid arthritis(RA)patients administered intravenously or subcutaneously with *** tocilizumab-derived signature peptide was deciphered using a nano-lc system coupled to a hybrid quadrupole-orbitrap mass *** serum tocilizumab was rapidly digested by immobilized trypsin for 30 *** chromatographic peak of the signature peptide and that of the internal standard were separated from the serum digests for a total run time of 15 *** calibration curve of serum tocilizumab concentration was linear with a range of 2-200 μg/*** intra-and inter-day accuracy and relative standard deviation(RSD)were 90.7%-109.4%andlc-ms/ms method with minimal sample pretreatments for monitoring serum tocilizumab concentrations in RA patients was developed.

关键词： Tocilizumab lc-ms/ms Immobilized trypsin IgG purification Proteomics Rheumatoid arthritis

Simultaneous quantification of chlorogenic acid and taurocholic acid in human plasma by lc-ms/ms and its application to a pharmacokinetic study after oral administration of Shuanghua Baihe tablets

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Chinese Journal of Natural Medicines 2016年第4期14卷 313-320页

作者： GU Pan LIU Rui-Juan CHENG Min-Lu WU Yao ZHENG Lu LIU Yu-Jie MA Peng-Cheng DING Li Department of Pharmaceutical Analysis China Pharmaceutical UniversityNanjing 210009China Nanjing Clinical Tech laboratories Inc. Nanjing 211000China Yangtze River Pharmaceutical Group Taizhou 225321China Institute of Dermatology Chinese Academy of Medical Sciences and Peking Union Medical CollegeNanjing 210042China

An lc-ms/ms method was developed and validated for the simultaneous quantification of chlorogenic acid(CGA) and taurocholic acid(TCA) in human plasma using hydrochlorothiazide as the internal standard. The chromatographic separation was achieved on a Hedera ODS-2 column with a gradient elution using 10 mmol·L^(-1) of ammonium acetate buffer solution containing 0.5% of formic acid- acetonitrile as mobile phase at a flow rate of 300 μL·min-1. The detection was performed on a triple quadrupole tandem mass spectrometer by multiple reaction monitoring in negative ESI mode. The method was fully validated over the concentration ranges of 0.1–10 ng·m L^(-1) for CGA and 2–150 ng·m L^(-1) for TCA. It was successfully applied to a pharmacokinetic study of CGA and TCA in healthy Chinese volunteers after oral administration of Shuanghua Baihe tablets(SBTs). In the single-dose study, the maximum plasma concentration(C_(max)), time to reach C_(max)(T_(max)) and elimination half-life(t_(1/2)) of CGA were(0.763 8 ± 0.542 0) ng·m L^(-1),(1.0 ± 0.5) h, and(1.3 ± 0.6) h, respectively. In the multiple-dose study, the C_(max), T_(max) and t_(1/2) of CGA were(0.663 7 ± 0.583 3) ng·m L^(-1),(1.1 ± 0.5) h, and(1.4 ± 0.7) h, respectively. For TCA, no significant characteristic increasing plasma TCA concentration-time curve was found in the volunteers after oral administration of SBTs, indicating its complicated process in vivo as an endogenous ingredient.

关键词： Chlorogenic acid Taurocholic acid Shuanghua Baihe tablets Pharmacokinetics lc-ms/ms

Pharmacokinetic analysis and tissue distribution of Vam3 in the rat by a validated lc-ms/ms method

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Acta Pharmaceutica Sinica B 2015年第3期5卷 254-263页

作者： Ruixia Zhang Ping Mao Tingting Zhang Chen Ma Bo Jin Tong Li Institute of Materia Medica Chinese Academy of Medical Sciences and Peking Union Medical College

Vam3 is a potential pharmacologically active ingiedient isolated from Vitis amurensis Rupr. A rapid, simple and sensitive method to determine Vam3 levels in rat plasma and tissue was developed based on EC-ms/ms. Vam3 and an internal standard (IS) were chromatographed on a C18 short column with acetonitrile-0.1% formic acid in water by gradient elution. ms detection was performed by electrospray ionization in negative ion multiple reaction monitoring modes,This method monitored the transitions m/z 451.0 -> 345.0 and m/z 301.0 -> 164.0 for Vam3 and IS, respectively. The calibration curve was linear over a concentration range of 1,64-1000 ng/mE, The inter-day and intra-day variabilities in precision was less than 12.8%, while the inter -day and intim-day accuracies ranged from 10.60% to 9.084 in plasma and tissue homogenates. This method was applied to investigate the pharmacokinetics and tissue distribution of Vain3 in rats. The results indicated that Vain3 had poor absorption into systemic circulation and extensive tissue distribution after oral administration, and the absolute bioavailability was low (0.79%). Vam3 had a relatively long terminal elimination half-life in lung, and the highest concentration was found in small intestinal tissue. The developed method and the pharmacokinetic data can provide a basis for further studies on the bioactivity of Vam3. (C) 2015 Chinese Pharmaceutical Association and Institute of Materia Medica, Chinese Academy of Medical Sciences. Production and hosting by Elsevier B.V.

关键词： Vam3 Pharmacokinetics Tissue distribution Absolve bioavialability lc-ms/ms

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

Click chemistry-based enrichment strategy for tracing cellular fatty acid metabolism by lc-ms/ms

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Journal of Pharmaceutical Analysis 2023年第10期13卷 1221-1231页

作者： Ru-Jie Yang Jian Zou Jia-Yue Liu Jiang-Kun Dai Jian-Bo Wan State Key Laboratory of Quality Research in Chinese Medicine Institute of Chinese Medical SciencesUniversity of MacaoMacao SAR999078China

Fatty acids(FAs),which were initially recognized as energy sources and essential building blocks of biomembranes,serve as the precursors of important signaling *** FA metabolism is essential to understanding the biochemical activity and role of FAs in physiological and pathological *** by the advances in click chemistry for protein enrichment,we herein established a click chemistry-based enrichment(CCBE)strategy for tracing the cellular metabolism of eicosapentaenoic acid(EPA,20:5 n-3)in neural *** alkyne-labeled EPA(EPAA)used as a surrogate was incubated with N2a,mouse neuroblastoma cells,and alkyne-labeled metabolites(ALms)were selectively captured by an azide-modified resin via a Cu(I)-catalyzed azide-alkyne cycloaddition reaction for *** removing unlabeled metabolites,ALms containing a triazole moiety were cleaved from solid-phase resins and subjected to liquid chromatography mass spectrometry(lc-ms)*** proposed CCBE strategy is highly selective for capturing and enriching alkyne-labeled metabolites from the complicated *** addition,this method can overcome current detection limits by enhancing ms sensitivity of targets,improving the chromatographic separation of sn-position glycerophospholipid regioisomers,facilitating structural characterization of ALms by a specific ms/ms fragmentation signature,and providing versatile fluorescence detection of ALms for cellular *** CCBE strategy might be expanded to trace the metabolism of other FAs,small molecules,or drugs.

关键词： Click chemistry-based enrichment EPA metabolism Terminal alkyne-labeled EPA Azide-modified resin lc-ms/ms

Fragmentation stability and retention time-shift obtained by lc-ms/ms to distinguish sialylated N-glycan linkage isomers in therapeutic glycoproteins

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Journal of Pharmaceutical Analysis 2023年第3期13卷 305-314页

作者： Chi Soo Park Minju Kang Ahyeon Kim Chulmin Moon Mirae Kim Jieun Kim Subin Yang Leeseul Jang Ji Yeon Jang Ha Hyung Kim Department of Global Innovative Drugs Graduate School of Chung-Ang UniversitySeoul06974Republic of Korea

Sialylated N-glycan isomers withα2-3 orα2-6 linkage(s)have distinctive roles in glycoproteins,but are difficult to ***-type(WT)and glycoengineered(mutant)therapeutic glycoproteins,cytotoxic T lymphocyte-associated antigen-4-immunoglobulin(CTLA4-Ig),were produced in Chinese hamster ovary cell lines;however,their linkage isomers have not been *** this study,N-glycans of CTLA4-Igs were released,labeled with procainamide,and analyzed by liquid chromatography-tandem mass spectrometry(ms/ms)to identify and quantify sialylated N-glycan linkage *** linkage isomers were distinguished by comparison of 1)intensity of the N-acetylglucosamine ion to the sialic acid ion(Ln/Nn)using different fragmentation stability in ms/ms spectra and 2)retention time-shift for a selective m/z value in the extracted ion *** isomer was distinctively identified,and each quantity(>0.1%)was obtained relative to the total N-glycans(100%)for all observed ionization *** sialylated N-glycan isomers with onlyα2-3 linkage(s)in WT were identified,and each isomer's sum of quantities was 50.4%.Furthermore,39 sialylated N-glycan isomers(58.8%)in mono-(3 N-glycans;0.9%),bi-(18;48.3%),tri-(14;8.9%),and tetra-(4;0.7%)antennary structures of mutant were obtained,which comprised mono-(15 N-glycans;25.4%),di-(15;28.4%),tri-(8;4.8%),and tetra-(1;0.2%)sialylation,respectively,with onlyα2-3(10 N-glycans;4.8%),bothα2-3 andα2-6(14;18.4%),and onlyα2-6(15;35.6%)linkage(s).These results are consistent with those forα2-3 neuraminidase-treated *** study generated a novel plot of Ln/Nn versus retention time to distinguish sialylated N-glycan linkage isomers in glycoprotein.

关键词： Therapeutic glycoprotein Sialylation Linkage isomer lc-ms/ms

Simultaneous Quantification of κ-Carrageenan Oligosaccharides of DP 3, 5 and 7 by lc-ms/ms: Application to an in vitro Absorption Study

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Journal of Ocean University of China 2020年第5期19卷 1177-1182页

作者： YANG Yali ZHANG Pengpeng LIU Guilin YANG Shuang WANG Yuanhong JIANG Tingfu LV Zhihua YU Mingming School of Medicine and Pharmacy Ocean University of ChinaQingdao 266003China Laboratory for Marine Drugs and Bioproducts of Qingdao National Laboratory for Marine Science and Technology Qingdao 266003China Key Laboratory of Glycoscience&Glycotechnology of Shandong Province Qingdao 266003China Key Laboratory of Marine Drugs Ministry of Education of ChinaQingdao 266003China

Carrageenans are widely utilized in many commercial applications such as the food and pharmaceutical industry, due to their excellent functional properties. In this study, a sensitive lc-ms/ms method was developed to determine κ-3, κ-5, and κ-7 carrageenan oligosaccharides simultaneously. Optimum MRM transitions for κ-3, κ-5, and κ-7 carrageenan oligosaccharides were(645.079→565.111, [M-H]-),(515.137→474.946, [M-2H]^2-), and(471.484→445, [M-3H]^3-), respectively. Chromatographic separation was performed on an Amide column coupled with a guard column operated at 60℃ under stepwise gradient elution. The linearity of the lc-ms/ms method for κ-3, κ-5, and κ-7 carrageenan oligosaccharides, evaluated over the concentration range of 0.10- 20.0 μmol L^-1, was excellent. The precisions of the method for κ-3, κ-5, and κ-7 carrageenan oligosaccharides were from 0.91% to 9.66%, and the inter-day precisions were from 0.92% to 10.5%. Validation of the lc-ms/ms method indicated that the method was precise and in line with the CFDA guidance. This method has been successfully applied to an in vitro absorption study.

关键词： κ-carrageenan oligosaccharide Caco-2 cell lc-ms/ms degree of polymerization

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

Simultaneous determination of LY3214996,abemaciclib,and M2 and M20 metabolites in human plasma,cerebrospinal fluid,and brain tumor by lc-ms/ms

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Journal of Pharmaceutical Analysis 2022年第4期12卷 601-609页

作者： Tigran Margaryan Mackenna Elliott Nader Sanai Artak Tovmasyan Ivy Brain Tumor Center Barrow Neurological InstitutePhoenixAZ85013USA

A sensitive and rapid liquid chromatography tandem mass spectrometry(lc-ms/ms)method was established for the quantification of total and unbound concentrations of LY3214996,an extracellular signal-regulated kinase inhibitor;abemaciclib,a cyclin-dependent kinase 4/6 inhibitor;and abemaciclib active metabolites,M2 and M20,in human plasma,brain tumor,and cerebrospinal fluid *** method was validated over a concentration range of 0.2e500 nM within a total run time of 3.8 min using isocratic elution on a Kinetex^(TM) F_(5) *** was performed on a Sciex QTRAP 6500t mass spectrometer employing multiple reaction monitoring mode under positive electrospray *** intra-and inter-batch accuracy as well as the precision of the method for all matrices was within ±20% and ≤20% at the lower limit of quantification,and within ±15% and ≤15% for other quality control levels for all *** unbound fractions of drugs and metabolites in spiked and patient samples were determined using an optimized equilibrium *** validated method was successfully applied in a phase 0/2 clinical trial to assess the central nervous system penetration of LY3214996 and abemaciclib.

关键词： lc-ms/ms LY3214996 Abemaciclib Brain tumor penetration Equilibrium dialysis

Development and validation of a high throughput lc–ms/ms method for simultaneous quantitation of pioglitazone and telmisartan in rat plasma and its application to a pharmacokinetic study

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Journal of Pharmaceutical Analysis 2017年第6期7卷 381-387页

作者： Pinaki Sengupta Bappaditya Chatterjee Uttam Kumar Mandal Bapi Gorain Tapan Kumar Pal Department of Pharmaceutical Technology Kulliyyah of PharmacyInternational Islamic University MalaysiaMalaysia Lincoln University College Malaysia Bioequivalence Study Centre Jadavpur UniversityKolkataIndia

Management of cardiovascular risk factors in diabetes demands special attention due to their co-existence. Pioglitazone （PIO） and telmisartan （TLM） combination can be beneficial in effective control of cardiovascular complication in diabetes. In this research, we developed and validated a high throughput lc-ms/ms method for simultaneous quantitation of PIO and TLM in rat plasma. This developed method is more sensitive and can quantitate the analytes in relatively shorter period of time compared to the previously reported methods for their individual quantification. Moreover, till date, there is no bioanalytical method available to simultaneously quantitate PIO and TLM in a single run. The method was validated according to the USFDA guidelines for bioanalytical method validation. A linear response of the analytes was observed over the range of 0.005-10 pg/mL with satisfactory precision and accuracy. Accuracy at four quality control levels was within 94.27%-106.10%. The inlxa- and inter-day precision ranged from 2.32% to 10.14% and 5.02% to 8.12%, respectively. The method was reproducible and sensitive enough to quantitate PIO and TLM in rat plasma samples of a preclinical pharmacokinetic study. Due to the potential of PIO-TLM combination to be therapeutically explored, this method is expected to have significant usefulness in future.

关键词： lc-ms/ms Rat plasma Pharmacokinetic applicability Telmisartan Pioglitazone Pharmacokinetic application