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一种液相色谱-串联质谱法测定呼出气中 28 种非挥发性滥用药物。

A liquid chromatography and tandem mass spectrometry method to determine 28 non-volatile drugs of abuse in exhaled breath.

机构信息

Department of Clinical Pharmacology, Karolinska University Hospital Laboratory and Department of Laboratory Medicine, Karolinska Institutet, Stockholm, Sweden.

Department of Clinical Pharmacology, Karolinska University Hospital Laboratory and Department of Laboratory Medicine, Karolinska Institutet, Stockholm, Sweden.

出版信息

J Pharm Biomed Anal. 2018 Jan 30;148:251-258. doi: 10.1016/j.jpba.2017.10.003. Epub 2017 Oct 9.

Abstract

Exhaled breath carries aerosol micro-particles containing nonvolatile organic substances. Recently, the analysis of drugs of abuse (DOA) have become of interest in exhaled breath particles (EBP). In this study, a liquid chromatography - tandem mass spectrometry (LC-MS/MS) method was developed and validated to analyze 28 DOA in 30L of EBP collected on a permeable polymer filter. After extraction, the chromatographic separation was achieved on a UPLC BEH phenyl column using a mobile phase consisting of methanol and water both containing 4mmol/L ammonium formate and 0.05% ammonia. The column temperature was set at 50°C and mobile phase flow rate 0.5mL/min in gradient mode with a total run time of 5min. The mass spectrometer was operated in positive electrospray ionization and selected reaction monitoring mode. Acquired limits of quantification were in the range of 1-66pg/filter for all substances except DM-tramadol. Excellent linearity over the concentration range from LLOQs - 15ng/filter with r2 values >0.99 and satisfactory recoveries (70-116% at 100pg/filter) were achieved. During method application a total 26 samples were analyzed of which 24 were found to be positive for 13 analytes. The highest amount was found for methadone (56ng/filter) and the lowest amount was found for the methadone metabolite EDDP (2pg/filter) in two different samples.

摘要

呼出气携带含有非挥发性有机物质的气溶胶微粒。最近,滥用药物(DOA)的分析已成为呼出气颗粒(EBP)中的研究热点。在这项研究中,开发并验证了一种液相色谱-串联质谱(LC-MS/MS)方法,用于分析 30L 可渗透聚合物滤器收集的 EBP 中 28 种 DOA。经过提取后,在 UPLC BEH 苯基柱上使用包含甲醇和水的流动相进行色谱分离,流动相中含有 4mmol/L 甲酸铵和 0.05%氨。柱温设定为 50°C,流动相流速为 0.5mL/min,采用梯度模式,总运行时间为 5min。质谱仪以正电喷雾电离和选择反应监测模式运行。除 DM-曲马多外,所有物质的定量下限均在 1-66pg/滤器范围内。在 LLOQs-15ng/滤器的浓度范围内,获得了极好的线性关系(r2 值>0.99),回收率令人满意(100pg/滤器时为 70-116%)。在方法应用过程中,共分析了 26 个样本,其中 24 个样本对 13 种分析物呈阳性。在两个不同的样本中,发现美沙酮的含量最高(56ng/滤器),而美沙酮代谢物 EDDP 的含量最低(2pg/滤器)。

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