摘要
目的:建立高效液相色谱-质谱联用法测定恒河猴血浆中纳曲酮及其代谢物纳曲醇的浓度。方法:液相色谱:色谱柱为Nucleocil ODS(5μm,50 mm×2.0 mm),流动相为乙腈-甲醇-水-冰醋酸(20:20:60:1),流速为0.2 mL·min-1;质谱:离子源为Turbo Ionspray源,采用多反应监测(MRM)方式进行检测,m/z342.3→324.3(纳曲酮)、m/z 344.3→326.6(纳曲醇,代谢产物)、m/z 328.4→310.4(纳洛酮,内标)。样品经有机相提取纯化后进样。结果:纳曲酮和纳曲醇的线性范围分别为0.098-150 ng·mL-1和0.781-25 ng·mL-1,萃取回收率均大于75%,日内误差(RSD)均小于9.3%,日间误差(RSD)均小于12%。结论:本方法准确、快速、灵敏、专属性好,适用于动物试验及临床上测定血浆中纳曲酮及其代谢物纳曲醇的浓度和药代动力学研究。
Objective:To establish an HPLC/MS/MS method for the determination of naltrexone and its metabolite naltrexol in rhesus monkey plasma. Methods: LC: Nucleocil ODS column ( 5 μm, 50 mm×2. 0 mm) , the mobile phase consisting of acetonitrile - methanol - water - acetic acid(20: 20: 60: 1) , a flow rate of 0. 2 mL· min-1, injection volume 20μL; MS; Use Turbo Ionspray, and the multiple reaction monitoring ( MRM ) mode, m/z 342. 3→326. 3 (naltrexone, NTX ) , m/z 344. 3→326. 3 ( naltrexol, NOL, metabolite ) and m/z 328. 4→310. 4 ( naloxone, NLX, internal standard). Samples were extracted with benzene - ethanol (9: 1) . The residues was dissolved in 100 μL of water - acetic acid( 100:1 )and injected. Results:The linear range of NTX was 0. 098 - 150 ng ·mL-1. The linear range of NOL was 0. 781 - 25 ng· mL-1. The extraction recovery rates were more than 75% , intra - day RSD was less than 9. 3% ,and inter - day RSD was less than 12% . Conclusion:The established method is accurate,rapid, sensitive and specific. Such method is suitable for application in the determination of NTX and its metabolite NOL and investigation of NTX pharmacokinetics.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2004年第6期573-576,共4页
Chinese Journal of Pharmaceutical Analysis
基金
国家高技术研究发展计划(863)
项目编号:2003AA22347B
