Setor Técnico-Científico, Superintendência Regional do Departamento de Polícia Federal no Rio Grande do Sul, Porto Alegre, Brazil.
Anal Chim Acta. 2011 Jun 24;696(1-2):67-76. doi: 10.1016/j.aca.2011.04.014. Epub 2011 Apr 20.
A method for the simultaneous identification and quantification of amphetamine (AMP), methamphetamine (MET), fenproporex (FEN), diethylpropion (DIE) and methylphenidate (MPH) in oral fluid collected with Quantisal™ device has been developed and validated. Thereunto, in-matrix propylchloroformate derivatization followed by direct immersion solid-phase microextraction and gas chromatography-mass spectrometry were employed. Deuterium labeled AMP was used as internal standard for all the stimulants and analysis was performed using the selected ion monitoring mode. The detector response was linear for the studied drugs in the concentration range of 2-256 ng mL(-1) (neat oral fluid), except for FEN, whereas the linear range was 4-256 ng mL(-1). The detection limits were 0.5 ng mL(-1) (MET), 1 ng mL(-1) (MPH) and 2 ng mL(-1) (DIE, AMP, FEN), respectively. Accuracy of quality control samples remained within 98.2-111.9% of the target concentrations, while precision has not exceeded 15% of the relative standard deviation. Recoveries with Quantisal™ device ranged from 77.2% to 112.1%. Also, the goodness-of-fit concerning the ordinary least squares model in the statistical inference of data has been tested through residual plotting and ANOVA. The validated method can be easily automated and then used for screening and confirmation of amphetamine-type stimulants in drivers' oral fluid.
已开发并验证了一种使用 Quantisal™装置收集的口腔液中同时鉴定和定量检测苯丙胺（AMP）、甲基苯丙胺（MET）、芬普雷司（FEN）、二乙基丙 胺（DIE）和哌醋甲酯（MPH）的方法。为此，采用了基质中丙基氯甲酸酯衍生化，然后直接浸入固相微萃取和气相色谱-质谱法。所有兴奋剂均使用氘标记的 AMP 作为内标，并且使用选择离子监测模式进行分析。除 FEN 外，在研究药物的浓度范围为 2-256 ng mL(-1)（纯口腔液）时，检测器响应呈线性，而 FEN 的线性范围为 4-256 ng mL(-1)。检测限分别为 0.5 ng mL(-1)（MET）、1 ng mL(-1)（MPH）和 2 ng mL(-1)（DIE、AMP、FEN）。质量控制样品的准确度保持在目标浓度的 98.2-111.9%以内，而精密度未超过相对标准偏差的 15%。用 Quantisal™装置的回收率范围为 77.2%至 112.1%。此外，还通过残差绘图和方差分析测试了数据统计推断中普通最小二乘模型的拟合优度。该验证方法可轻松实现自动化，然后用于筛选和确认驾驶员口腔液中的苯丙胺类兴奋剂。
