分子印迹固相萃取法在血中苯丙胺类毒品分析中的应用

Application of molecularly imprinted solid-phase extraction for separating and assaying amphetamines in blood samples

目的建立分子印迹固相萃取(MISPE)、GC/MS分析方法,用于血液中苯丙胺类毒品检测。方法 10mmol/L醋酸铵缓冲液(pH8.0)4倍稀释空白添加血液,1mL甲醇,1mL10mmol/L醋酸铵缓冲液(pH8.0)活化苯丙胺类分子印迹固相萃取柱;2×1mL去离子水、1mL60%的乙腈去离子水、1mL1%醋酸乙腈洗涤杂质;2×1mL1%甲酸/甲醇洗脱,洗脱液挥干定容,经GC/NPD、GC/MS分析检测。结果各种苯丙胺类毒品回收率均在90%以上,在20～5 000ng/mL浓度范围内线性关系良好,r2为0.995 7～0.998 9,LOQ在16～30ng/mL之间,LOD在8～15ng/mL之间。结论本方法回收率高,净化效果显著,稳定性好,杂质干扰少,可用于血液中低浓度苯丙胺类毒品的分析检测。

Objecive A method for extraction of amphetamines in blood samples using molecularly imprinted solid phase extraction and gas chromatography-mass spectrometry（GC/MS）.Methods Human blood samples were spiked with amphetamine,methamphetamine,MDA and MDMA,and diluted with 4∶1（v/v）with 10mmol/L ammonium acetate buffer（pH8.0）;activating the MIP column with 1mL methanol and 1mL 10mmol/L ammonium acetate（pH8.0）;Washing the impurities using 2 1mL water,1mL 60/40 MeCN/water and 1mL 1% HAc in MeCN;Elute the amphetamine drugs with 2 1mL 1% formic acid in methanol,then evaporate under nitrogen to dryness and reconstitute with 100μL methanol prior to GC/MS analysis.Results The recoveries obtained with this method for amphetamine drugs are more than 90%.The linear range was 20～5000ng/mL with correlation coefficients between 0.995 7 and 0.998 9.The limits of detection were 20ng/mL for amphetamine（AM）,16ng/mL methamphetamine（MA）,30ng/mL methylenedioxyamphetamine（MDA）and methylened ioxy methamp hetamine（MDMA）,The limits of quantitative were 10ng/mL for AM,8ng/mL for methamphetamine（MAM）,15ng/mL for MDA and MDMA.Conclusion Recoveries are higher,impurities were less.The method could be applied for simultaneous determination of trace amphetamines in biological specimens.