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作 者:郭秒[1,2] 郭继芬[2] 虞林[2] 王以美[2] 贾栗[2] 彭双清[2] 袁波[1]
机构地区:[1]沈阳药科大学药学院,沈阳110016 [2]军事医学科学院疾病预防控制所,北京100071
出 处:《国际药学研究杂志》2017年第3期273-277,共5页Journal of International Pharmaceutical Research
基 金:国家自然科学基金青年基金资助项目(81001468)
摘 要:目的建立测定大鼠血浆中芍药内酯苷的液相色谱-串联质谱(LC-MS/MS)法。方法血浆样品经乙酸乙酯-异丙醇(95∶5,V/V)提取后,以Poroshell 120 EC-C18柱(50 mm×2.1 mm,2.7μm)为分析柱,乙腈-水为流动相梯度洗脱,采用ESI源在多反应监测(MRM)方式下进行正离子检测。用于定量分析的离子反应为m/z 498.5→m/z 197.1(芍药内酯苷)和m/z 251.3→m/z 108.2(拉科酰胺,内标)。结果芍药内酯苷血浆浓度测定方法的线性范围为20~2000 ng/ml,日内、日间精密度RSD%均<15%,准确度(RE)在±8.06%之间。结论该法适用于芍药内酯苷在大鼠体内的毒代动力学研究。Objective To develop and validate a LC-MS/MS method for the determination of albiflorin in rat plasma. Meth?ods Plasma samples were extracted by liquid-liquid extraction with a mixture of ethyl acetate-isopropanol(95:5,V/V)to prepare samples for analysis. Chromatographic separation was performed on a Poroshell 120 EC-C18 column(50 mm × 2.1 mm I.D. 2.7μm). The mobile phase consisted of acetonitrile-water followed gradient elution. Detection of albiflorin and the internal standard(IS)lacos?amide was achieved by ESI MS/MS in the positive ion mode using m/z 498.5→m/z 197.1 and m/z 251.3→m/z 108.2 transitions,respec?tively. Results The method was linear in the range of 20 to 2000 ng/ml when 50μl plasma was analyzed. The lower limit of quantifi?cation was 20 ng/ml. The inter-and intra-day precision values were both below 15%,and the accuracy(relative error)was within ± 8.06%in all quality control samples. Conclusion The method provides a sensitive and rapid means for the determination of albiflorin in rat plasma,and completely meets the requirements for toxicokinetic study.
关 键 词:芍药内酯苷 液相色谱-串联质谱法 毒代动力学
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