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首页> 外文期刊>Journal of Analytical Toxicology >Quantitative and isomeric determination of amphetamine and methamphetamine from urine using a nonprotic elution solvent and R(-)-alpha-methoxy-alpha-trifluoromethylphenylacetic acid chloride derivatization.
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Quantitative and isomeric determination of amphetamine and methamphetamine from urine using a nonprotic elution solvent and R(-)-alpha-methoxy-alpha-trifluoromethylphenylacetic acid chloride derivatization.

机译:使用非质子洗脱溶剂和R(-)-α-甲氧基-α-三氟甲基苯基乙酸氯衍生化测定尿液中的苯丙胺和甲基苯丙胺的定量和异构体。

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摘要

Forensic Urine Drug Testing Laboratories often requires two confirmatory methods for a methamphetamine positive screen. First, methamphetamine is identified and quantitated using gas chromatography-mass spectrometry. If the total methamphetamine concentration is above the administrative cutoff level, the isomeric composition must be determined. This eliminates a possible contribution by over-the-counter cold medications that contain l-methamphetamine (Vick's inhalers). Products that contain only the l-isomer of methamphetamine must be distinguishable from prescription or illicitly manufactured methamphetamine, which consists mainly of the d-isomer. Optically impure derivatizing reagents will produce an impure mixture from a pure isomeric compound. Therefore, methods utilizing impure reagents can prove problematic when interpreting results. Use of an optically pure chiral derivatizing reagent, such as R(-)-alpha-methoxy-alpha-trifluoromethylphenylacetic acid chloride, allows for the creation and measurement of chromatographically separable isomeric compounds. The novel method described here utilizes a polymer-based solid-phase column adapted to a positive pressure manifold extraction system and a one-step derivatization process that occurs directly in the elution solvent. This methodology eliminates an elution solvent dry-down step that may adversely affect recovery of volatile amphetamine compounds. Although the method was designed for the quantitative analysis of the isomers of amphetamine and methamphetamine, it can be adapted for use with a wide range of phenethylamines including methylenedioxyamphetamine, N-methylenedioxymethamphetamine, and possibly N-methylenedioxyethylamphetamine. The linear range for quantitation was 25-10,000 ng/mL for d,l-methamphetamine and d,l-amphetamine, and correlation coefficients were 0.997 or better. The coefficient of variation for all four analytes did not exceed 2.8%. Concentrations analyzed ranged from 500 to 4000 ng/mL (n=40). The method allows for a simple and accurate quantitation and isomeric determination of amphetamine and methamphetamine using a process that eliminates extraction and derivatization complications common in current methods.
机译:法医尿液药物检测实验室通常需要两种确认方法来进行甲基苯丙胺阳性筛查。首先,使用气相色谱-质谱法对甲基苯丙胺进行鉴定和定量。如果甲基苯丙胺的总浓度高于管理的临界水平,则必须确定异构体组成。这样就消除了含有l-甲基苯丙胺(维克吸入器)的非处方感冒药可能带来的影响。仅包含甲基苯丙胺的l-异构体的产品必须与处方药或非法制造的甲基苯丙胺(主要由d-异构体组成)区分开。光学不纯的衍生试剂将由纯的异构体化合物产生不纯的混合物。因此,在解释结果时,使用不纯试剂的方法可能会出现问题。使用光学纯的手性衍生试剂,例如R(-)-α-甲氧基-α-三氟甲基苯基乙酸氯,可以创建和测量色谱上可分离的异构化合物。本文所述的新方法利用了适用于正压歧管萃取系统的基于聚合物的固相色谱柱,以及直接在洗脱溶剂中进行的一步衍生化过程。这种方法消除了洗脱溶剂干燥步骤,该步骤可能会对挥发性苯丙胺化合物的回收产生不利影响。尽管该方法设计用于定量分析苯丙胺和甲基苯丙胺的异构体,但它可适用于多种苯乙胺,包括亚甲基二氧苯丙胺,N-亚甲基二氧甲基苯丙胺,以及可能的N-亚甲基二氧乙基苯丙胺。 d,l-甲基苯丙胺和d,l-苯异丙胺的定量线性范围为25-10,000 ng / mL,相关系数为0.997或更高。所有四种分析物的变异系数均不超过2.8%。分析浓度范围为500至4000 ng / mL(n = 40)。该方法使用一种消除了当前方法中常见的提取和衍生化复杂性的方法,可以对苯丙胺和甲基苯丙胺进行简单,准确的定量和异构体测定。

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