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LC/ESI-MS/MS method for quantification of 28 synthetic cannabinoids in neat oral fluid and its application to preliminary studies on their detection windows

机译:LC / ESI-MS / MS方法测定纯净口腔液中28种合成大麻素的含量及其在检测窗口初步研究中的应用

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Serum and urine samples are commonly used for the analysis of synthetic cannabinoids in biofluids; however, their utilization as analytical matrices for drug abstinence control features some substantial drawbacks. While for blood collection invasive sampling is inevitable, the urinary analysis of synthetic cannabinoids is limited by the lack of available reference standards of the respective major metabolites. Moreover, the long detectability of synthetic cannabinoids in both matrices hampers the identification of a recent synthetic cannabinoid use. This article describes the development, validation and application of an LC/ESI-MS/MS method for the quantification of 28 synthetic cannabinoids in neat oral fluid (OF) samples. OF samples were prepared by protein precipitation using ice-cold acetonitrile. Chromatographic separation was achieved by gradient elution on a Luna Phenyl Hexyl column (50×2 mm, 5 μm), while detection was carried out on a QTrap 4000 instrument in positive ionization mode. The limits of detection ranged from 0.02 to 0.40 ng/mL, whereas the lower limits of quantification ranged from 0.2 to 4.0 ng/mL. The method was applied to authentic samples collected during two preliminary studies in order to obtain insights into the general detectability and detection windows of synthetic cannabinoids in this matrix. The results indicate that synthetic cannabinoids are transferred from the blood stream into OF and vice versa only at a very low rate. Therefore, positive OF samples are due to contamination of the oral cavity during smoking. As these drug-contaminations could be detected up to approximately 2 days, neat oral fluid appears to be well suited for detection of a recent synthetic cannabinoid use.
机译:血清和尿液样品通常用于分析生物流体中的合成大麻素。然而,它们用作禁欲分析的分析基质具有一些实质性的缺点。虽然对于采血是不可避免的,但侵入性采样是不可避免的,但合成大麻素的尿液分析受到各主要代谢物缺乏可用参考标准的限制。此外,合成大麻素在两种基质中的长期可检测性妨碍了最近合成大麻素用途的鉴定。本文介绍了LC / ESI-MS / MS方法的开发,验证和应用,该方法用于定量纯净口腔液(OF)样品中的28种合成大麻素。用冰冷的乙腈通过蛋白沉淀制备OF样品。色谱分离是通过在Luna苯基己基色谱柱(50×2 mm,5μm)上进行梯度洗脱而实现的,而检测是在QTrap 4000仪器上以正电离模式进行的。检出限范围为0.02至0.40 ng / mL,而定量下限范围为0.2至4.0 ng / mL。该方法应用于两次初步研究中收集的真实样品,以了解该基质中合成大麻素的一般可检测性和检测窗口。结果表明,合成大麻素仅以非常低的速率从血流转移到OF中,反之亦然。因此,阳性OF样品归因于吸烟期间口腔的污染。由于可以在大约2天的时间内检测到这些药物污染,因此纯净的口腔液似乎非常适合于检测最近使用的合成大麻素。

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