摘要
目的:建立快速、准确的尿液中甲基苯丙胺(MA)及其代谢产物苯丙胺(AMP)的分子印迹固相萃取(MISPE)高效液相色谱测定方法。方法:尿液与10 mmol/L醋酸铵缓冲液(pH 8.0)混合后离心分离(8000 rpm),采用预先活化过的分子印迹固相萃取柱净化,以醋酸/乙腈溶液洗脱,在XBridge RP18色谱柱上,以甲醇-乙腈-水溶液(15∶30∶55,V/V/V)为流动相,采用210 nm波长进行检测。结果:MA和AMP的加标回收率在88.5%~97.0%范围,其相对标准偏差均小于5.0%,在0.05 mg/L~15.0 mg/L范围呈现良好的线性,其回归系数大于0.999,检出限(LODs)分别为0.005 mg/L和0.01 mg/L。结论:本方法回收率高,净化效果显著,稳定性好,杂质干扰少,可满足临床吸毒病人尿液中MA和AMP的检测要求。
Objective:To develop a method for the simultaneous determination of methamphetamine(MA) and amphetamine(AMP) in urine by high-performance liquid chromatography with molecularly imprinted solid-phase extraction(MISPE).Methods:After the urine samples were mixed with 10 mmol/L ammonium acetate buffer(pH8.0) and centrifuged at 8000 rpm,the clean up procedure was optimized on an activating molecularly imprinted solid-phase extraction cartridge and the elution was carried by acetate acid/ acetonitrile.The separation was performed on an XBridge RP18 column by a mobile phase consisting of methanol-acetonitrile-water(15:30:55,V/V/V).Detection was carried out by an ultraviolet detector at 210 nm.Results:Calibration curves of MA and AMP were linear within the range of 0.05 mg/L~15.0 mg/L with correlation coefficients of more than 0.999.The limits of detection(LODs) were 0.005 mg/L and 0.01 mg/L for MA and AMP,respectively.The extraction recoveries were between 88.5%~97.0%,and the RSDs were less than 5.0%.Conclusion:This developed method is simple,sensitive and accurate.It is suitable for the detection of MA and AMP residues in biological specimens for the clinical diagnosis of drug abuse patients.
出处
《中国卫生检验杂志》
北大核心
2012年第6期1217-1220,共4页
Chinese Journal of Health Laboratory Technology
基金
宁波市科技计划项目(2011C50048)
关键词
液相色谱法
甲基苯丙胺
苯丙胺
尿液
分子印迹固相萃取
High-performance liquid chromatography
Methamphetamine(MA)
Amphetamine(AMP)
Urine
Molecularly imprinted solid-phase extraction