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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。
Objective To establish a method of molecularly imprinted solid phase extraction (MISPE) and GC / MS for the detection of amphetamines in blood. Methods The blood was diluted 4 times with 10mmol / L ammonium acetate buffer (pH8.0), and 1mL methanol and 1mL 10mmol / L ammonium acetate buffer (pH8.0) were used to activate amphetamines molecularly imprinted solid phase extraction column. 2 × 1mL deionized Water, 1mL60% acetonitrile deionized water, 1mL1% acetonitrile to wash the impurities; 2 × 1mL1% formic acid / methanol, the eluent evaporated to dryness and determined by GC / NPD and GC / MS. Results The recoveries of various amphetamines were above 90%. The linear range was from 20 000 to 5 000 ng / mL with r2 ranging from 0.995 7 to 0.998 9, LOQ ranging from 16 to 30 ng / mL, 15ng / mL. Conclusion The method has high recovery rate, significant purification effect, good stability and less impurity interference, and can be used for the analysis and detection of low concentration amphetamine drugs in the blood.