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Using liquid chromatography tandem mass spectrometry to detect rhodamine123 in rat plasma

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Using liquid chromatography tandem mass spectrometry to dete...

liquid chromatography electrospray ionization tandem mass spectrometry(LC/ESI-MS/MS) method for quantitative estimation of moxifloxacin in human plasma

第十三次全国临床药理学学术大会

作者： Ya-Bin Sun~a,Zhong-Yuan Xu~a,Guo-Feng Li~b a GCP Office,Nanfang Hospital,Southern Medical University,Guangzhou 510515,China b Department of Pharmacy,Nanfang Hospital,Southern Medical University,Guangzhou 510515,China

A new,rapid and sensitive method was developed for the quantifying of rhodamine 123(R123) in rat plasma using liquid chromatography tandem mass spectrometry(LC-MS/MS).Rhodamine 6G(R6G) was used as the internal standard(IS).R123 and IS were extracted from aliquots of plasma with ethyl acetate and dichloromethane (4:1) as the solvent.Chromatographic separation was performed using a Zorbax Eclipse Plus C18 column.The mobile phase was composed of A:ammonium formate-formic acid buffer containing 5 mM ammonium formate and 0.1%formic acid and B:methanol(A:B,5:95,v/v).To quantify R123 and IS respectively,multiple reaction monitoring(MRM) transition of m/z 345.2→285.2 and m/z 443.3→415.2 were performed.The analysis lasted for 4 min,in the positive mode,the results of which were presented as a linear calibration curve over the concentration range of 1-200 ng/ml and sampling volume of 2μl.The lowest limit of quantification(LLOQ) reached 1 ng/ml.The intra and inter-day precision were 6.7%and 9.2%for the low quality control(QC) sample (2 ng/ml),respectively.Intra and inter-day precision of the medium QC sample(100 ng/ml) were both less than 3.4%.Intra and inter-day precision of high QC sample(150 ng/ml) were both less than 2.1%,while the intra and inter-day relative errors ranged between -7.4%and 9.1%for the above three QC concentration levels.The LC-MS/MS method proved to be simple,accurate,reliable and with a shorter running time and has been successfully applied to an absorption experiment in the rat.

关键词： Rhodamine 123 liquid chromatography tandem mass spectrometry Rhodamine 6G Rat plasma

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Journal of Chinese Pharmaceutical Sciences 2014年第3期23卷 159-164页

作者： Vipul.M.Vaghela Prajesh Prajapati Hetal K.Patel A.R.College of Pharmacy and G.H.Patel Institute of Pharmacy Institute of Research and Development Gujarat Forensic Sciences University Shree Swaminarayan Sanskar Pharmacy College

A rapid and sensitive liquid chromatography tandem mass spectrometry(LC-MS/MS) method has been developed and validated for the determination of moxifloxacin(MOXI) in human plasma. After a simple protein precipitation using acetonitrile, the post treatment samples were analysed on a C18 column interfaced with a Triple Quadropole tandem mass Spectrometer. Positive electrospray ionization was employed as the ionization source. The mobile phase consisted of 0.1% formic acid–acetonitrile(60:40, v/v). Ciprofloxacin(CIPRO) was used as an internal standard. The analyte and internal standard(CIPRO) were monitored in the multiple reaction monitoring mode(MRM). The mass transition ion-pair has been followed as m/z 402→358.2 for MOXI and 332→288.1 for CIPRO. The method was linear in the concentration range of 25–5000 ng/mL. The lower limit of quantification was 25 ng/mL. The intra- and inter-day precision(relative standard deviation) and accuracy(relative error) values were within 12.4%. Each plasma sample was analyzed within 3 min.

关键词： Moxifloxacin Ciprofloxacin Human plasma liquid chromatography tandem mass spectrometry Electrospray ionization

Simultaneous determination of clopidogrel,2-oxo-clopidogrel,and the thiol metabolite of clopidogrel in human plasma by LC-MS/MS

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The Journal of Biomedical Research 2022年第2期36卷 109-119页

作者： Lei Xu Ran Li Juan Li Zhou Dong Jiaxin Zong Chuchu Tan Zekang Ye Lu Shi Xiaoxuan Gong Chunjian Li Department of Cardiology the First Affiliated Hospital of Nanjing Medical UniversityNanjingJiangsu 210009China Department of Cardiology the Affiliated Sir Run Run Hospital of Nanjing Medical UniversityNanjing Jiangsu 210009China Cardiovascular Center the Second Affiliated Hospital of Nanjing Medical UniversityNanjingJiangsu 210003China

Clopidogrel is a pro-drug which needs two-step metabolism to produce the active thiol metabolite.This study aimed to explore an efficient method to simultaneously determine the plasma clopidogrel,2-oxo-clopidogrel(2-Oxo-CLP),and the clopidogrel active metabolite(CAM).A high-throughput liquid chromatography tandem mass spectrometry(LC-MS/MS)was therefore developed.The analytes were extracted from plasma by using methyl tert-butyl ether(MTBE).Chromatographic separation was performed on a C18 column under an isocratic elution,accompanied with acetonitrile and deionized water containing 0.1%formic acid.After optimizing the condition of LC-MS/MS,a stable linearity was observed in the standard curves over the concentration ranges of 0.05 to 50.0 ng/mL for clopidogrel,0.5 to 50.0 ng/mL for 2-Oxo-CLP,and 0.5 to 100 ng/mL for clopidogrel active metabolite derivative(CAMD).The retention time was 4.78 minutes,3.79 minutes,3.59 minutes,and 4.82 minutes for clopidogrel,2-Oxo-CLP,CAMD,and internal standard,respectively.Both the relative standard deviation and the relative error were within the requirement of operating criteria.No significant degradation of clopidogrel,2-Oxo-CLP,and CAMD occurred under different storage conditions.This method was successfully validated in 3 patients with coronary artery disease.The results showed that the current LC-MS/MS method was efficient for simultaneously detecting clopidogrel,2-Oxo-CLP,and CAM with fine linearity,accuracy,precision,and stability.

关键词： clopidogrel drug metabolites liquid chromatography tandem mass spectrometry coronary artery disease

Pharmacokinetics and Tolerability of Oral Dosage Forms of Huperzine A in Healthy Chinese Male Volunteers: a Randomized,Single Dose, Three-period, Six-sequence Crossover Study

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Journal of Huazhong University of Science and Technology(Medical Sciences) 2017年第5期37卷 795-802页

作者：伍三兰甘珺饶静贺思洁朱雯雯赵瑛吕永宁黄建耿刘亚妮 Department of Pharmacy Union Hospital Tongji Medical College Huazhong University of Science and Technology Clinical Research Organization for Pharmaceutical Products Union Hospital Tongji Medical College Huazhong University of Science and Technology Department of Pharmaceutics School of Pharmacy Tongji Medical College Huangzhong University of Science and Technology

Huperzine A is a potent, reversible, and blood-brain barrier permeable acetylcholinesterase inhibitor. The aim of this study was to compare the pharmacokinetics, tolerability, and bioavailability of two formulations with the established reference formulation of huperzine A in a fasting, healthy Chinese male population. This was a randomized, single-dose, 3-period, 6-sequence crossover study. The plasma concentrations of huperzine A were determined by liquid chromatography tandem mass spectrometry. Tolerability was assessed based on subject interview, vital sign monitoring, physical examination, and routine blood and urine tests. The mean（SD） pharmacokinetic parameters of the reference drug were Cmax, 1.550（0.528） ng/m L; t1/2, 12.092（1.898） h; AUC0-72 h, 17.550（3.794） ng·h/m L. Those of the test formulation A and test formulation B were Cmax, 1.412（0.467）, 1.521（0.608） ng/m L; t1/2, 12.073（2.068）, 12.271（1.678） h; AUC0-72 h, 15.286（3.434） ng·h/mL, 15.673（3.586） ng·h/m L. The 90% confidence intervals for the AUC0-72 h and Cmax were between 0.80 and 1.25. No adverse events were reported by the subjects or found with results of clinical laboratory test. The test and reference products met the regulatory criteria for bioequivalence in these fasting, healthy Chinese male volunteers. All three formulations appeared to be well tolerated.

关键词： huperzine A pharrnacokinetics bioequivalence tolerability liquid chromatography tandem mass spectrometry

Hydrophobic protein in colorectal cancer in relation to tumor stages and grades

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World Journal of Gastroenterology 2010年第22期16卷 2754-2763页

作者： Lay-Chin Yeoh Chee-Keat Loh Boon-Hui Gooi Manjit Singh Lay-Harn Gam School of Pharmaceutical Sciences Universiti Sains Malaysia Department of Surgery Penang General Hospital

AIM: To identify differentially expressed hydrophobic proteins in colorectal cancer. METHODS: Eighteen pairs of colorectal cancerous tissues in addition to tissues from normal mucosa were analysed. Hydrophobic proteins were extracted from the tissues, separated using 2-D gel electrophoresis and analysed using liquid chromatography tandem mass spectrometry (LC/MS/MS). Statistical analysis of the proteins was carried out in order to determine the significance of each protein to colorectal cancer (CRC) and also their relation to CRC stages, grades and patients’ gender. RESULTS: Thirteen differentially expressed proteins which were expressed abundantly in either cancerous or normal tissues were identified. A number of these proteins were found to relate strongly with a particular stage or grade of CRC. In addition, the association of these proteins with patient gender also appeared to be significant.CONCLUSION: Stomatin-like protein 2 was found to be a promising biomarker for CRC, especially in female patients. The differentially expressed proteins identified were associated with CRC and may act as drug target candidates.

关键词： Biomarker Colorectal cancer liquid chromatography tandem mass spectrometry Proteomic approach 2D-polyacrylamide gel electrophoresis

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液相色谱-质谱法测定人体血浆中阿那曲唑

液相色谱-质谱法测定人体血浆中阿那曲唑