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高效液相色谱二极管阵列检测器测定尿液中氯氮平

Analysis of trace clozapine in urine by high-performance liquid chromatography coupled with diode array detector
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摘要 目的:建立一种准确、灵敏的尿液样品中氯氮平的高效液相色谱二极管阵列检测方法。方法:尿液样品直接经固相萃取小柱净化、富集后,采用Extend C18柱(250 mm×4.6 mm i.d.,5μm),以0.02 mol/L乙酸铵+甲醇(15+85,v/v)为流动相,紫外228 nm检测,采用地西泮为内标进行定量。结果:尿液样品中氯氮平在0.01~1.0 mg/L范围内呈良好线性关系,日内精密度RSD%〈6.5,日间精密度RSD%〈9.5,方法回收率在96.0%~98.0%之间,定量检出限为0.01 mg/L。结论:本方法简便、灵敏、重现性好,能满足氯氮平服药病人以及中毒病人的临床诊断检测要求。 Objective:To establish a method for determination of clozapine in urine by high-performance liquid chromatography coupled with diode array detector(DAD).Methods:After the urine sample was cleaned and enriched by solid-phase extraction(SPE) cartridges,the sample was separated on an Extend C18 column(250 mm×4.6 mm i.d.,5 μm)by using the mobile phase consisting of 0.02 mol/L ammonium acetate+methanol(15+85,v/v).Detection was carried out by DAD at 228 nm.Quantitative analysis was based on an internal standard method with diazapam.Results:The calibration curve was linear within the range of 0.01~1.0 mg/L,and the limit of quantification was found to be 0.01 mg/L.The extraction recovery was 96.0%~98.0%,the Intra-day RSD was less than 6.5% and the Inter-day RSD was less than 9.5%.Conclusion:This method is simple,sensitive,accurate and of good specificity for the satisfactory determination of trace clozapine residue in poisoned patients.
作者 朱波 金米聪
出处 《中国卫生检验杂志》 CAS 2009年第12期2844-2846,共3页 Chinese Journal of Health Laboratory Technology
基金 宁波市医学科技计划项目资助(2006051)
关键词 高效液相色谱法 二极管阵列 尿液 氯氮平 HPLC DAD Urine Clozapine
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