文章摘要
李泰平.LC-MS法测定大鼠血浆中EXH-1626的浓度[J].南京医科大学学报,2014,(1):
LC-MS法测定大鼠血浆中EXH-1626的浓度
Determination of the Concentration of EXH-1626 in Rat Plasma by LC-MS
投稿时间:2013-07-15  修订日期:2013-12-16
DOI:10.7655/NYDXBNS201401029
中文关键词: EXH-1626  LC-MS法  血药浓度
英文关键词: EXH-1626, LC/MS, drug plasma concentration
基金项目:
作者单位E-mail
李泰平 南京医科大学附属友谊整形外科医院 litaiping@126.com 
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中文摘要:
      摘 要 目的:建立测定大鼠血浆中EXH-1626浓度的LC-MS方法。 方法:大鼠血浆样品中加入内标卡马西平,经蛋白沉淀剂(甲醇:5%硫酸锌溶液= 70:30,V/V)沉淀血浆蛋白后取上清液5 μL进行LC-MS测定。色谱条件:色谱柱为汉邦ODS C18柱(5 µm,150 mm×4.6 mm),流动相为乙腈-10 mmol/L醋酸铵水溶液(用乙酸调pH至3)70:30,流速为0.6 mL/min,柱温30℃;质谱条件:采用电喷雾离子化(ESI)方式,以选择性离子监测(SIM)方式检测,EXH-1626和内标选择检测离子的质荷比分别为m/z 453.3([M+H]+)和m/z 274.3([M+H]+)。 结果:大鼠血浆中EXH-1626在线性范围5~10 000 ng/mL内线性关系良好(r = 0.9997),最低定量限(LOQ)为5 ng/mL,由低到高(10、100、1 000和10 000 ng/mL)4个浓度的日内和日间精密度RSD均小于10 %,绝对回收率均大于70 %,相对回收率在90 %~110 %之间。结论:该方法快速、准确,灵敏度高,操作简便,适用于EXH-1626血药浓度测定及其非临床药代动力学研究。
英文摘要:
      Abstract Objective To develop a LC-MS method for the determination of EXH-1626 in rat plasma. Methods Using Carbamazepine as internal standard (IS), plasma samples were deposited by blood precipitation reagent(methanol:5 %zinc sulfate =70:30,V/V)before sampling and determined by injecting 5 μL to LC-MS system. The analytes was separated on a Han Bang ODS C18(5 µm, 150 mm×4.6 mm) analytical column with acetonitrile and 10 mmol/L ammonium acetate(using acetic acid makes pH to 3) (70:30) as the mobile phase. Analysis was performed at a flow rate of 0.6 mL/min and the column temperature was 30℃. MS determination was in electrospray ionization(ESI) mode and the selected ion monitoring(SIM) mode, EXH-1626 was monitored at m/z 453.3 and internal standard at m/z 274.3. Results The linearity of EXH-1626 concentration curve was in a range of 5~1.0×104 ng/mL,r = 0.9997,and the lowest limit of quantification(LOQ) was 5 ng/mL. The RSDs of inter-day and intra-day were all less than 10 %, absolute recoveries were greater than 70 %, and relative recoveries were in between 90 %~110 %. Conclusion:The method is proved to be fast, precise, sensitive, convenient, and suitable for determination of the concentration and non clinical pharmacokinetic study of EXH-1626.
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