液相色谱串联质谱法测定人血浆中的长春新碱.docVIP

史上最快最全的网络文档批量下载批量上传，尽在：/item.htm?id=9176907081 史上最快最全的网络文档批量下载批量上传，尽在：/item.htm?id=9176907081 液相色谱串联质谱法测定人血浆中的长春新碱 左艳华1, 沙春洁2, 周凤梅2,盖芸芸2, 刘万卉1,2*(1 烟台大学药学院 烟台 264005 ; 2 山东绿叶制药有限公司, 烟台 264003) 摘要目的建立快速、灵敏测定血浆中分析方法2﹕1﹕0.1 (m粒径, 50×4.6 mm I.D.）,流动相为：甲醇︰水（80﹕20,含10 mmol·L-1 醋酸铵, 用甲酸调 pH至3.0）。电离方式为电喷雾正离子,扫描方式为多反应监测(MRM),用于定量分析的离子对分别是长春新碱：m/z 825.8→765.4,长春瑞宾：m/z 779.9→122.6。结果 测定血浆中长春新碱的线性范围为1.05～840 ng·mL-1（r=0.9982）, 最低定量限为1.05 ng·mL-1, 日内和日间精密度均在15%以内。结论 该法快速, 灵敏, 专属。Determination of Vincristine in Human Plasma by Liquid Chromatography and Electrospray Tandem Mass Spectrometry ZUO Yan-hua1, SHA Chun-jie2, ZHOU Feng-mei2, GAI Yun-yun2, LIU Wan-hui1,2*（chool of Pharmacy, Yantai University, Yantai, 264005, China ; 2 Shandong Luye Pharmaceutical Co. Ltd. Yantai , 264003, China） AOBJECTIVE To establish a rapid and sensitive method for quantification of vincristine in human plasma for clinical trials. METHODS Vincristine and internal standard (vinorelbine) were extracted from plasma using a solvent mixture of n-hexane﹕dichloromethane﹕isopropanol 2﹕1﹕0.1). Liquid chromatography and electrospray tandem mass spectrometric (LC-MS/MS) was used for the determination of incristine and vinorelbine. Chromatographic separation was achieved on an Agilent Eclispe XDB C18（1.8 (m , 50×4.6 mm I.D.）using the eluent 作者简介：左艳华（1983- ）, 女, 山东青岛人, 硕士研究生, 研究方向：天然产物的ADME研究 *通讯作者： Tel:0535-6717618-8030E-mail：wanhui@ of methanol﹕H2O (﹕10 mmol· L-1 ammonium acetate, adjust pH to 3.0 with formic acid) as mobile phase. This method involved the use of the ions mass spectrum of vincristine and IS at m/z 825.8→765.4 and m/z 779.9→122.6 with the selected reaction monitoring (MRM) mode. RESULTS The calibration curve was linear over the range of 1.05～80 ng·mL-1 with a correlation coefficient of 0.9982. The mean extraction recoveries of vincristine determined over the concentrations of 3.1, 82.0 and 640 ng·mL-1 were 82.7%, 81.3% and 79.8%, respectively, and the extraction recovery of vinorelbine was 82