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目的建立全血和尿液中4-甲氧基甲基安非他明(PMMA)的液相色谱-质谱(LC-MS/MS)联用检测方法。方法血液、尿液添加样本经MCX柱固相萃取(SPE)后,采用电喷雾正离子模式离子化、多反应监测模式检测PMMA,外标法定量,并对PMMA和甲基安非他明(MA)进行比较,对方法学指标进行考察。结果采用SPE-LC-MS/MS法,血液和尿液中PMMA含量在0.1~100μg/L范围内呈良好的线性关系,相关系数R2为0.998 8(血液,n=6)和0.999 5(尿液,n=6);标准回收率分别为71%~80%(血液)和76%~89%(尿液),日内与日间精密度均小于6%。PMMA的方法检测限(LOD)0.03μg/L,定量下限(LOQ)为0.1μg/L。结论采用本文SPE-LC-MS/MS方法,可对血液和尿液中PMMA准确定性,且检出限低,回收率高,选择性强,可适用于相关毒品检验。
Objective To establish a liquid chromatography-mass spectrometry (LC-MS / MS) method for the detection of 4-methoxymethyl amphetamine (PMMA) in whole blood and urine. Methods Blood and urine samples were analyzed by MCX column solid phase extraction (SPE) and electrospray positive ion mode ionization. Multiple reaction monitoring (PMMA) and external standard method were used to quantify PMMA and methamphetamine MA) were compared to study the methodological indicators. Results The SPE-LC-MS / MS method showed a good linear relationship between the concentration of PMMA in blood and urine in the range of 0.1-100 μg / L with the correlation coefficients R2 of 0.998 8 (blood, n = 6) and 0.999 5 Liquid, n = 6). The standard recoveries were 71% -80% (blood) and 76% -89% (urine), respectively. The intra- and inter-day precision was less than 6%. The method detection limit (LOD) of 0.03μg / L and the limit of quantitation (LOQ) of PMMA were 0.1μg / L. Conclusion The method of SPE-LC-MS / MS in this paper can accurately determine PMMA in blood and urine with low detection limit, high recovery rate and high selectivity, which can be applied to related drug tests.