LC-MS-MS法测定人血浆中阿托伐他汀浓度
投稿时间:2010-05-18  修订日期:2010-09-09  点此下载全文
引用本文:姜楠,杨永革,许雪廷,赵钢涛.LC-MS-MS法测定人血浆中阿托伐他汀浓度[J].药学实践杂志,2011,29(1):15~16,70
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作者单位
姜楠 北京军区总医院药理科,北京100700 
杨永革 北京军区总医院药理科,北京100700 
许雪廷 北京军区总医院药理科,北京100700 
赵钢涛 北京军区总医院药理科,北京100700 
中文摘要:目的 建立液质联用色谱法(LC-MS-MS)测定人血浆中阿托伐他汀(atorvastatin )浓度。 方法 采用萃取法处理血浆样品进行LC-MS-MS分析。分析柱为美国Thermo公司Thermo BioBasic-C8柱(2.1 mm×100 mm,5 μm) ;流动相为乙腈(含0.1%甲酸):水(含0.1%甲酸)=70:30;流速0.3 ml/min;质谱条件:电喷雾离子化电离源ESI负离子检测,喷雾电压(SP)3 500 KV,鞘气(SGP)流速10 Arb,辅助气(AGP)流速15 Arb,毛细管温度(TEM)314 ℃;选择反应监测(SRM)分别测定阿托伐他汀和甲苯磺丁脲 558→278 m/z(30 EV)和269→106 m/z(22 EV) 。 结果 阿托伐他汀在0.1~20 μg/L检测浓度范围内呈良好线性关系(r>0.99),最低定量限(LLOQ)为0.1 μg/L,绝对回收率在70%以上,高中低3种浓度的日内和日间RSD≤15%。 结论 该方法操作简便、灵敏、准确,适用于临床阿托伐他汀的血药浓度监测及I期临床试验。
中文关键词:阿托伐他汀钙  血药浓度  液质联用色谱法
 
Determination of Atorvastatin in human plasma by LC-MS-MS
Abstract:Objective To establish a method for determining Atorvastatin in human plasma by LC-MS-MS. Methods Atorvastatin was extracted for determination by LC-MS-MS. Analytical column was Thermo BioBasic-C8(2.1 mm×100 mm,5 μm). The mobile phase was acetonitrile(0.1%acid):water(0.1%acid)=70:30. Mass spectrum conditions was ESI performing in the SRM mode using target ions m/z 558→278(30EV)(Atorvastatin ), m/z 269→106(22 EV)(tolbutamide), SP 3 500 KV, SGP 10 Arb, AGP 15 Arb, TEM 314 ℃. Results The calibration curve was linear over the range of 0.1~20 μg/L. The LLOQ of Atorvastatin in plasma was 0.1 μg/L. The extracted recovery was>70%. The intra-and inter-day RSD were<15%. Conclusion The method is sensitive, simple and accurate to determinate Atorvastatin plasma concentration and suitable to study phase I clinical test of Atorvastatin.
keywords:Atorvastatin  plasma concentration  LC-MS-MS
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