Chromatographic Retention Index for the Identification of Illicit Substances

G.H. Giudice, A.H.L. Machado, J.J. Zacca, M.P. Souza, L.N.B. Caldas, E.D. Botelho, J.C.L. Ambrósio
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引用次数: 0

Abstract

Introduction

New Psychoactive Substances have a high introduction rate into the market and represent a huge challenge from a regulatory and forensic point of view. Thus, the need for a method capable of identifying NPS, without the availability of certified analytical standards, arises.

Methods

The methodology of the work relies on the development of a GC/MS method; its validation; and the calculation of the Kovats’ Retention Index. This index was selected because it was reported as a tool for high-precision identification. A total of twenty-two substances were used: AM-2201, MAM-2201, JWH-081, JWH-210, N-ethylpentylone, 5-MAPB, 2-FA, 25C-NBOMe, o-CPP, p-CPP, U-47700, 5-MeO-MiPT, 5-IAI, Salvia divinorium, methiopropamine, THC, heroin, amphetamine, methamphetamine, MDMA, cocaine, and ephedrine.

Results

The method presented one Selectivity limitation (coelution of methiopropamine and methamphetamine). Resolution values were higher than 1.25, indicating signal separation. Separation Factor, Number of Theoretical Plates, and Tailing provided satisfactory results. Evaluation of Intermediate Precision indicated Relative Standard Deviations (RSD) that varied from 0.02 to 0.29%, lower than the literature. Robustness evaluation using a Fractional Factorial Design identified that changing the column polarity was the most influential factor, while column brand, gas flow, split rate, injector temperature, and ramp temperature did not interfere significantly. Retention Index was calculated without overlap and the Global Confidence Interval varied from 0,5 to 20,6 Retention Index Unity and the RSD varied from 0,02 to 0,29%, inferior to the range found in the literature.

Conclusions

The results of the development and validation indicate the adequacy of the method that uses Kovats’ Retention Index to identify NPS. The collection of Index calculated can be updated and made available to forensic institutes to be used as a tool in NPS identification.
鉴别违禁物质的色谱保留指数
新精神活性物质进入市场的比率很高,从监管和法医的角度来看,这是一个巨大的挑战。因此,在没有经过认证的分析标准的情况下,需要一种能够识别NPS的方法。方法本研究的方法学建立在气相色谱/质谱法的基础上;它的验证;以及科瓦茨留任指数的计算。选择该指标是因为有报道称它是一种高精度鉴定工具。共使用了22种物质:AM-2201、MAM-2201、JWH-081、JWH-210、n -乙基戊酮、5-MAPB、2-FA、25c - nbp、o-CPP、p-CPP、U-47700、5-MeO-MiPT、5-IAI、丹参、甲氧丙胺、四氢大麻酚、海洛因、安非他明、甲基苯丙胺、MDMA、可卡因和麻黄碱。结果该方法存在一个选择性限制(甲氧丙胺与甲基苯丙胺共洗脱)。分辨率值大于1.25,表明信号分离。分选系数、理论板数、尾矿均取得了满意的结果。中间精密度评价显示相对标准偏差(RSD)在0.02 ~ 0.29%之间,低于文献。采用分数析因设计的稳健性评估发现,改变色谱柱极性是最重要的影响因素,而色谱柱品牌、气体流量、分裂速率、进样器温度和斜坡温度没有显著干扰。Retention Index计算无重叠,Global Confidence Interval范围为0.05 ~ 20.6 Retention Index Unity, RSD范围为0.02 ~ 0.29%,低于文献中所见范围。结论开发和验证结果表明,采用Kovats保留指数鉴别NPS的方法是适当的。所计算的指数集合可以更新并提供给法医研究所,作为鉴定国家养老金计划的工具。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
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来源期刊
Emerging trends in drugs, addictions, and health
Emerging trends in drugs, addictions, and health Pharmacology, Psychiatry and Mental Health, Forensic Medicine, Drug Discovery, Pharmacology, Toxicology and Pharmaceutics (General)
CiteScore
2.40
自引率
0.00%
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