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Simultaneous quantification of 106 drugs or their metabolites in nail samples by UPLC-MS/MS with high-throughput sample preparation: Application to 294 real cases

The nail is an alternative matrix to complement hair analysis in proving drug intake over several months in forensic toxicology investigations. However, because of the high hardness and toughness of nails, the existing pretreatment procedures for nails have the disadvantages of either a high degree...

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Published in:Analytica chimica acta 2022-09, Vol.1226, p.340170-340170, Article 340170
Main Authors: Liu, Peipei, Liu, Wenjuan, Qiao, Hongwei, Jiang, Shan, Wang, Youmei, Chen, Jie, Su, Mengxiang, Di, Bin
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Liu, Wenjuan
Qiao, Hongwei
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Chen, Jie
Su, Mengxiang
Di, Bin
description The nail is an alternative matrix to complement hair analysis in proving drug intake over several months in forensic toxicology investigations. However, because of the high hardness and toughness of nails, the existing pretreatment procedures for nails have the disadvantages of either a high degree of time consumption (from hours to days), or low extraction recoveries. This study aims to propose a high-throughput nail sample preparation method and provide a quantitative analytical method for 106 drugs and their metabolites present in nail. We developed cryogenic grinding, coupled with high-speed grinding in the extraction solvent method, which could improve the extraction recovery by thoroughly destroying the nail keratin for approximately 18 min. Subsequently, an ultra-high-performance liquid chromatography-tandem mass spectrometry method was developed for the identification and quantification of 34 synthetic cannabinoids, 26 fentanyls, 18 synthetic cathinones, 10 phenylethylamines, eight opioids, three phencyclidine, two tryptamines, two piperazine, cocaine, benzoylecgonine, and tetrahydrocannabinol (THC). Nail samples were collected from people with a history of drug abuse from five different regions of China. The analysis of 294 authentic samples resulted in 213 detected samples, and showed a broad concentration range including 5.04–67.26 pg/mg for nine synthetic cannabinoids, 109.29–250.29 pg/mg for a synthetic cathinone, 5.06–434291 pg/mg for four phenylethylamines, 5.06–464278 pg/mg for three phencyclidine, 5.50–192195 pg/mg for six opioids, 19.44–36.11 pg/mg for cocaine, and 50.53 pg/mg for THC in nail. Furthermore, up to 10 different compounds were detected in a single nail sample. This nail analysis method serves as a useful tool for the large-scale surveillance of illicit drugs abuse. [Display omitted] •Quantitative method validation for 106 drugs in human nail with a three-step extraction.•Cryogenic grinding coupled with room temperature zircon beads grinding was an efficient drug extraction method from nail.•Concentration ranges of authentic nail samples and prevalence of drugs from 294 Chinese drug addicts.
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However, because of the high hardness and toughness of nails, the existing pretreatment procedures for nails have the disadvantages of either a high degree of time consumption (from hours to days), or low extraction recoveries. This study aims to propose a high-throughput nail sample preparation method and provide a quantitative analytical method for 106 drugs and their metabolites present in nail. We developed cryogenic grinding, coupled with high-speed grinding in the extraction solvent method, which could improve the extraction recovery by thoroughly destroying the nail keratin for approximately 18 min. Subsequently, an ultra-high-performance liquid chromatography-tandem mass spectrometry method was developed for the identification and quantification of 34 synthetic cannabinoids, 26 fentanyls, 18 synthetic cathinones, 10 phenylethylamines, eight opioids, three phencyclidine, two tryptamines, two piperazine, cocaine, benzoylecgonine, and tetrahydrocannabinol (THC). Nail samples were collected from people with a history of drug abuse from five different regions of China. The analysis of 294 authentic samples resulted in 213 detected samples, and showed a broad concentration range including 5.04–67.26 pg/mg for nine synthetic cannabinoids, 109.29–250.29 pg/mg for a synthetic cathinone, 5.06–434291 pg/mg for four phenylethylamines, 5.06–464278 pg/mg for three phencyclidine, 5.50–192195 pg/mg for six opioids, 19.44–36.11 pg/mg for cocaine, and 50.53 pg/mg for THC in nail. Furthermore, up to 10 different compounds were detected in a single nail sample. This nail analysis method serves as a useful tool for the large-scale surveillance of illicit drugs abuse. 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However, because of the high hardness and toughness of nails, the existing pretreatment procedures for nails have the disadvantages of either a high degree of time consumption (from hours to days), or low extraction recoveries. This study aims to propose a high-throughput nail sample preparation method and provide a quantitative analytical method for 106 drugs and their metabolites present in nail. We developed cryogenic grinding, coupled with high-speed grinding in the extraction solvent method, which could improve the extraction recovery by thoroughly destroying the nail keratin for approximately 18 min. Subsequently, an ultra-high-performance liquid chromatography-tandem mass spectrometry method was developed for the identification and quantification of 34 synthetic cannabinoids, 26 fentanyls, 18 synthetic cathinones, 10 phenylethylamines, eight opioids, three phencyclidine, two tryptamines, two piperazine, cocaine, benzoylecgonine, and tetrahydrocannabinol (THC). Nail samples were collected from people with a history of drug abuse from five different regions of China. The analysis of 294 authentic samples resulted in 213 detected samples, and showed a broad concentration range including 5.04–67.26 pg/mg for nine synthetic cannabinoids, 109.29–250.29 pg/mg for a synthetic cathinone, 5.06–434291 pg/mg for four phenylethylamines, 5.06–464278 pg/mg for three phencyclidine, 5.50–192195 pg/mg for six opioids, 19.44–36.11 pg/mg for cocaine, and 50.53 pg/mg for THC in nail. Furthermore, up to 10 different compounds were detected in a single nail sample. This nail analysis method serves as a useful tool for the large-scale surveillance of illicit drugs abuse. 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However, because of the high hardness and toughness of nails, the existing pretreatment procedures for nails have the disadvantages of either a high degree of time consumption (from hours to days), or low extraction recoveries. This study aims to propose a high-throughput nail sample preparation method and provide a quantitative analytical method for 106 drugs and their metabolites present in nail. We developed cryogenic grinding, coupled with high-speed grinding in the extraction solvent method, which could improve the extraction recovery by thoroughly destroying the nail keratin for approximately 18 min. Subsequently, an ultra-high-performance liquid chromatography-tandem mass spectrometry method was developed for the identification and quantification of 34 synthetic cannabinoids, 26 fentanyls, 18 synthetic cathinones, 10 phenylethylamines, eight opioids, three phencyclidine, two tryptamines, two piperazine, cocaine, benzoylecgonine, and tetrahydrocannabinol (THC). Nail samples were collected from people with a history of drug abuse from five different regions of China. The analysis of 294 authentic samples resulted in 213 detected samples, and showed a broad concentration range including 5.04–67.26 pg/mg for nine synthetic cannabinoids, 109.29–250.29 pg/mg for a synthetic cathinone, 5.06–434291 pg/mg for four phenylethylamines, 5.06–464278 pg/mg for three phencyclidine, 5.50–192195 pg/mg for six opioids, 19.44–36.11 pg/mg for cocaine, and 50.53 pg/mg for THC in nail. Furthermore, up to 10 different compounds were detected in a single nail sample. This nail analysis method serves as a useful tool for the large-scale surveillance of illicit drugs abuse. 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subjects Forensic toxicology
Illicit drugs
Nail analysis
New psychoactive substances
Ultra-high performance liquid chromatography-tandem mass spectrometry
title Simultaneous quantification of 106 drugs or their metabolites in nail samples by UPLC-MS/MS with high-throughput sample preparation: Application to 294 real cases
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