摘要
目的:建立人血浆中地西泮、硝西泮、奥沙西泮、艾司唑仑和阿普唑仑的反向高效液相色谱测定法(RP-HPLC)。方法:以血浆为基质,配制含有5种镇静催眠药的混合标准品,取1mL样品加入50mg/L卡马西平10μL为内标,乙酸乙酯萃取后用100μL流动相溶解,进样20μL,通过高效液相色谱仪检测人血浆基质中5种镇静催眠药浓度。色谱条件:色谱柱为C18柱(4.6mm×250mm),柱温30℃,流动相为甲醇:水(65:35),流速1.0mL/min,紫外检测波长为230nm。结果:地西泮、硝西泮、奥沙西泮、艾司唑仑和阿普唑仑在5～1200μg/L范围内线性关系良好(r≥0.9966,P<0.05),加样回收率在95.5%～105.6%,萃取回收率均在75%以上,日内及日间变异相对标准偏差(RSD)均小于10%(n=5)。结论:RP-HPLC方法简便、准确、灵敏,适用于人血浆中地西泮、硝西泮、奥沙西泮、艾司唑仑和阿普唑仑的血药浓度的同时检测。
Objective To determine diazepam prazolam simultaneously in human plasma by reversed , nitrazepam, oxazepam, estazolam, and alphase high-performance liquid chromatography （RP-HPLC）. Methods Ten microliter carbamazepine （50 mg/L）as the internal standard was added into 1 mL sample, which contained the 5 mixed sedative hypnotics as standard substance and human plasma as ground substance. They were extracted with acetoacetate from plasma samples, and then were dissolved by 100 μL mobile phase. The blood drug levels were analyzed by high performance liquid chromatograph with 20 μL sample injection on a chromatographic column C 18 （ 4.6 mm × 250 mm）at 30 ℃. The mobile phase consisted of methanol and water （65：35） , and the flow rate was 1.0 mL/min. The ultraviolet detection wavelength was 230 nm. Results The linearity range of the 5 drugs was 5 - 1 200 μg/L（r≥0. 9966, P 〈0. 05）. The recovery rate was 95.5% 105.6% . The extraction recovery rate was more than 75 % . The relative standard deviation （ RSD ） of intra-day and inter-day was less than 10% （n = 5）. Conclusion RP-HPLC method is conven-lent, accurate and sensitive for simultaneous determination of the concentration of diazepam, nitrazepare, oxazepam, estazolam, and alprazolam in human plasma.
出处
《中南大学学报（医学版）》
CAS
CSCD
北大核心
2009年第7期689-692,F0003,共5页
Journal of Central South University ：Medical Science
关键词
镇静催眠药
反向高效液相色谱法
血药浓度
sedative hypnotics
reversed phase high-performance liquid chromatography
blood drug level
