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超高效液相色谱-串联质谱法测定死后血液和尿液中的新型精神活性物质和其他药物:方法验证和法医样本分析。

Determination of new psychoactive substances and other drugs in postmortem blood and urine by UHPLC-MS/MS: method validation and analysis of forensic samples.

机构信息

Forensic Analysis Laboratory, Criminalistics Institute, The Civil Police of the Federal District, Brasília, DF, 70610-907, Brazil.

Laboratory of Toxicology, Department of Pharmacy, University of Brasília, Campus Darcy Ribeiro, Brasília, DF, 70910-900, Brazil.

出版信息

Forensic Toxicol. 2022 Jan;40(1):88-101. doi: 10.1007/s11419-021-00600-y. Epub 2021 Oct 5.

Abstract

PURPOSE

This study aimed to validate a modified QuEChERS method followed by ultra-high performance liquid chromatography-tandem mass spectrometry to determine 79 new psychoactive substances (NPS) and other drugs in blood and urine.

METHODS

Prescription drugs (n = 23), synthetic cathinones (n = 13), phenethylamines (n = 11); synthetic cannabinoids (n = 8), amphetamines (n = 7) and other psychoactive substances (n = 17) were included in the method. 500 µL of biological fluid was extracted with 2 mL of water/ACN (1:1), 500 mg of anhydrous MgSO/NaOAc (4:1) added, followed by a supernatant cleanup with 25 mg of primary secondary amine and 75 mg of anhydrous MgSO. Quantification was done using matrix-matched calibration curves and deuterated internal standards.

RESULTS

The method was satisfactorily validated for blood and urine at limit of quantifications ranging from 0.4 to 16 ng/mL, and applied to the analysis of 54 blood (38 postmortem and 16 antemortem) and 16 antemortem urine samples from 68 forensic cases. All urine samples and 59.3% of the blood samples were positive for at least one analyte. Twenty-two analytes were detected in at least one biological sample, including the synthetic cathinones ethylone (222 ng/mL, antemortem blood), eutylone (246 and 446 ng/mL, urine), and N-ethylpentylone (597 and 7.3 ng/mL, postmortem and antemortem blood, respectively).

CONCLUSIONS

The validated method was shown to be suitable for the analysis of blood and urine forensic samples and an important tool to collect information on emerging drug threats and understanding the impact of NPS and other drugs in poisoning cases.

摘要

目的

本研究旨在验证一种改良的 QuEChERS 方法,结合超高效液相色谱-串联质谱法,用于检测血液和尿液中的 79 种新型精神活性物质(NPS)和其他药物。

方法

纳入方法的药物包括处方药物(n=23)、合成卡西酮(n=13)、苯乙胺(n=11);合成大麻素(n=8)、苯丙胺(n=7)和其他精神活性物质(n=17)。用 2 mL 水/乙腈(1:1)提取 500 µL 生物流体,加入 500 mg 无水硫酸镁/醋酸钠(4:1),然后用 25 mg 一级二级胺和 75 mg 无水硫酸镁进行上清液净化。使用基质匹配校准曲线和氘代内标进行定量。

结果

该方法在定量限为 0.4 至 16 ng/mL 的血液和尿液中得到了令人满意的验证,并应用于 68 例法医案例中 54 份血液(38 份死后和 16 份生前)和 16 份生前尿液样本的分析。所有尿液样本和 59.3%的血液样本均至少有一种分析物呈阳性。在至少一种生物样本中检测到 22 种分析物,包括合成卡西酮乙基酮(222 ng/mL,生前血液)、依他酮(246 和 446 ng/mL,尿液)和 N-乙基戊基酮(597 和 7.3 ng/mL,死后和生前血液)。

结论

该验证方法适用于血液和尿液法医样本的分析,是收集新兴药物威胁信息和了解 NPS 及其他药物在中毒案件中影响的重要工具。

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