LC-atmospheric pressure chemical ionization-MS/MS analysis of multiple illicit drugs, methadone, and their metabolites in oral fluid following protein precipitation
LC-atmospheric pressure chemical ionization-MS/MS analysis of multiple illicit drugs, methadone, and their metabolites in oral fluid following protein precipitation
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DOI：
10.1021/ac026111t
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发表时间：
2003-02-15
影响因子：
7.4
通讯作者：
Huestis, MA
中科院分区：
文献类型：
--
作者：
Dams, R;Murphy, CM;Huestis, MA
建立了一种同时测定口服液中多种非法药物美沙酮及其代谢物的LC-APCI-MS/MS定量方法。样品前处理仅限于乙腈蛋白沉淀。LC分离在25.5分钟内进行，总分析时间为35分钟。鉴别和定量基于选定的反应监测。通过线性回归分析进行校准，使用氘代内标物和加权因子1/x。检测限和定量下限（LOQ）分别确定为0.25 - 5 ng/ mL和0.5-10 ng/mL。在LOQ至最大值500 ng/mL的动态范围内，获得线性，平均相关系数（R-2）> 0.99。该方法证明了所有化合物的准确度、批内和批间精密度、回收率和稳定性良好。在整个色谱运行过程中未观察到口服液基质效应。蛋白质沉淀法是一种快速、简便的样品前处理方法，而LC-APCI-MS/MS被证明是一种灵敏、耐用的口腔液中多种非法和法律的药物定量方法。该方法被证明是合适的评价口腔液作为尿液的替代基质，用于监测非法药物的使用，并确定口服液美沙酮浓度在怀孕的阿片类药物和/或可卡因成瘾。
A quantitative LC-APCI-MS/MS method for simultaneous determination of multiple illicit drugs, methadone, and their metabolites in oral fluid was developed and validated. Sample pretreatment was limited to acetonitrile protein precipitation. LC separation was performed in 25.5 min, with a total analysis time of 35 min. Identification and quantitation were based on selected reaction monitoring. Calibration by linear regression analysis utilized deuterated internal standards and a weighing factor 1/x. limits of detection and lower limits of quantitation (LOQ) were established between 0.25 and 5 ng/ mL and 0.5-10 ng/mL, respectively. linearity was obtained with an average correlation coefficient (R-2) of > 0.99, over a dynamic range from the LOQ up to maximum 500 ng/mL. The method demonstrated good accuracy, intra- and interbatch precision, recovery, and stability for all compounds. No oral fluid matrix effect was observed throughout the chromatographic run. Protein precipitation provided a fast and simple sample pretreatment, while LC-APCI-MS/MS proved to be a sensitive and rugged quantitative method for multiple illicit and legal drugs in oral fluid. The method proved to be suitable for the evaluation of oral fluid as an alternative matrix to urine for monitoring illicit drug use and for determining oral fluid methadone concentrations in pregnant opiate and/or cocaine addicts.