Gray Teresa R, Shakleya Diaa M, Huestis Marilyn A
Chemistry and Drug Metabolism, Intramural Research Program, National Institute on Drug Abuse, National Institutes of Health, 251 Bayview Blvd., Baltimore, MD 21224, USA.
Anal Bioanal Chem. 2009 Apr;393(8):1977-90. doi: 10.1007/s00216-009-2680-5. Epub 2009 Feb 26.
A method for the simultaneous quantification of 20 cocaine, amphetamine, opiate, and nicotine analytes in meconium, the first neonatal feces, by liquid chromatography tandem mass spectrometry was developed and validated. Specimen preparation included methanol homogenization and solid phase extraction. Two injections were required to achieve sufficient sensitivity and linear dynamic range. Linearity ranged from 0.5-25 up to 500 ng/g (250 ng/g p-hydroxymethamphetamine), and correlation coefficients were >0.996. Imprecision was <10.0% CV, analytical recovery 85.5-123.1%, and extraction efficiencies >46.7% at three concentrations across the linear range. Despite significant matrix effects of -305.7-40.7%, effects were similar for native and deuterated analytes. No carryover, endogenous or exogenous interferences were observed, with analyte stability at room temperature, 4 degrees C, and -20 degrees C and on the autosampler >70%, except for 6-acetylmorphine, hydrocodone, oxycodone, and morphine. Method applicability was demonstrated by analyzing meconium from drug-exposed neonates.
开发并验证了一种通过液相色谱串联质谱法同时定量分析胎粪(新生儿首次排出的粪便)中20种可卡因、苯丙胺、阿片类药物和尼古丁分析物的方法。样本制备包括甲醇匀浆和固相萃取。需要进样两次以实现足够的灵敏度和线性动态范围。线性范围为0.5 - 25至500 ng/g(对羟基甲基苯丙胺为250 ng/g),相关系数>0.996。在整个线性范围内的三个浓度下,精密度<10.0% CV,分析回收率为85.5 - 123.1%,萃取效率>46.7%。尽管存在 - 305.7 - 40.7%的显著基质效应,但天然和氘代分析物的效应相似。未观察到残留、内源性或外源性干扰,除6 - 乙酰吗啡、氢可酮、羟考酮和吗啡外,分析物在室温、4℃和 - 20℃以及自动进样器上的稳定性>70%。通过分析暴露于药物的新生儿的胎粪证明了该方法的适用性。