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通过高效液相色谱-串联质谱法测定口腔液样本中合成和天然大麻素(新型精神活性物质)的生物分析方法的验证

Validation of a Bioanalytical Method for the Determination of Synthetic and Natural Cannabinoids (New Psychoactive Substances) in Oral Fluid Samples by Means of HPLC-MS/MS.

作者信息

Calò Luca, Anzillotti Luca, Maccari Chiara, Cecchi Rossana, Andreoli Roberta

机构信息

Legal Medicine, Department of Medicine and Surgery, University of Parma, Parma, Italy.

Laboratory of Industrial Toxicology, Department of Medicine and Surgery, University of Parma, Parma, Italy.

出版信息

Front Chem. 2020 Jun 5;8:439. doi: 10.3389/fchem.2020.00439. eCollection 2020.

Abstract

New psychoactive substances (NPS) represent an important focus nowadays and are continually produced with minimal structural modifications in order to circumvent the law and increase the difficulty of identifying them. Moreover, since there are a high number of different compounds, it is arduous to develop analytical screening and/or confirmation methods that allow the identification and quantification of these compounds. The aim of this work is to develop and validate a bioanalytical method for detecting new synthetic drugs in biological samples, specifically oral fluid, using high-performance liquid chromatography coupled with mass spectrometry (HPLC-MS/MS) with minimal sample pretreatment. Oral fluid samples were simply centrifuged and denaturized with different rapid procedures before injection into the LC-MS/MS system. Calibration curves covered a linear concentration range from LOQ to 100 ng/mL. Validation parameters such as linearity, precision, accuracy, selectivity, matrix effect and thermal stability were evaluated and showed satisfactory results, in accordance with US Food & Drug Administration guidelines. The inter-day analytical bias and imprecision at two levels of quality control (QC) were within ±15% for most compounds. This method was able to identify and calculate the concentration of 10 NPS validated in this biological sample, even in the presence of matrix effect.

摘要

新型精神活性物质(NPS)是当下的一个重要关注点,它们不断被生产出来,结构改动极小,以规避法律并增加识别难度。此外,由于存在大量不同的化合物,开发能够对这些化合物进行识别和定量的分析筛查和/或确证方法十分艰巨。本研究的目的是开发并验证一种生物分析方法,用于检测生物样品(具体为口腔液)中的新型合成药物,采用高效液相色谱-质谱联用(HPLC-MS/MS)技术,且样品预处理最少。口腔液样品只需简单离心,并通过不同的快速程序进行变性处理,然后注入LC-MS/MS系统。校准曲线覆盖了从定量下限(LOQ)到100 ng/mL的线性浓度范围。按照美国食品药品监督管理局的指导方针,对线性、精密度、准确度、选择性、基质效应和热稳定性等验证参数进行了评估,结果令人满意。大多数化合物在两个质量控制(QC)水平下的日间分析偏差和不精密度在±15%以内。即使存在基质效应,该方法也能够识别并计算出在该生物样品中验证的10种新型精神活性物质的浓度。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/bbfe/7325870/d6c7a1abb540/fchem-08-00439-g0001.jpg

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