首页> 外文期刊>Journal of mass spectrometry: JMS >Use of LC-HRMS in full scan-XIC mode for multi-analyte urine drug testing - a step towards a 'black-box' solution?
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Use of LC-HRMS in full scan-XIC mode for multi-analyte urine drug testing - a step towards a 'black-box' solution?

机译:使用LC-HRMS在全扫描XIC模式下进行多分析物尿药物测试 - 迈向“黑匣子”解决方案的一步吗?

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The influx of new psychoactive substances (NPS) has created a need for improved methods for drug testing in toxicology laboratories. The aim of this work was to design, validate and apply a multi-analyte liquid chromatography-high-resolution mass spectrometry (LC-HRMS) method for screening of 148 target analytes belonging to the NPS class, plant alkaloids and new psychoactive therapeutic drugs. The analytical method used a fivefold dilution of urine with nine deuterated internal standards and injection of 2 mu l. The LC system involved a 2.0 mu m 100 x 2.0 mm YMC-UltraHT Hydrosphere-C18 column and gradient elution with a flow rate of 0.5 ml/min and a total analysis time of 6.0 min. Solvent A consisted of 10 mmol/l ammonium formate and 0.005% formic acid, pH 4.8, and Solvent B was methanol with 10 mmol/l ammonium formate and 0.005% formic acid. The HRMS (Q Exactive, Thermo Scientific) used a heated electrospray interface and was operated in positive mode with 70 000 resolution. The scan range was 100-650 Da, and data for extracted ion chromatograms used +/- 10 ppm tolerance. Product ion monitoring was applied for confirmation analysis and for some selected analytes also for screening. Method validation demonstrated limited influence from urine matrix, linear response within the measuring range (typically 0.1-1.0 mu g/ml) and acceptable imprecision in quantification (CV < 15%). A few analytes were found to be unstable in urine upon storage. The method was successfully applied for routine drug testing of 17 936 unknown samples, of which 2715 (15%) contained 52 of the 148 analytes. It is concluded that the method design based on simple dilution of urine and using LC-HRMS in extracted ion chromatogram mode may offer an analytical system for urine drug testing that fulfils the requirement of a 'black box' solution and can replace immunochemical screening applied on autoanalyzers. Copyright (C) 2017 John Wiley & Sons, Ltd.
机译:新的精神活性物质(NPS)的涌入创造了有必要改进的毒理学实验室药物检测方法。这项工作的目的是设计,验证和应用多分析物液相色谱 - 高分辨率质谱(LC-HRMS)方法,用于筛选属于NPS类,植物生物碱和新的精神活性治疗药物的148个靶分析物。分析方法使用尿液稀释的尿液稀释,九个氘代内标和注射2μl。 LC系统涉及2.0μm100x 2.0mm的YMC-Ultraht Hydle-C18柱和梯度洗脱,流速为0.5ml / min,总分析时间为6.0分钟。溶剂A由10mmol / L甲酸铵和0.005%甲酸,pH4.8和溶剂B组成,甲醇B是甲醇,甲酸乙酯和0.005%甲酸。 HRMS(Q辐射,热科学)使用加热的电喷雾界面,并以70 000分辨率为正模式运行。扫描范围为100-650Da,并且用于提取的离子色谱图的数据使用+/- 10 ppm公差。产品离子监测用于确认分析和一些选定的分析物也用于筛选。方法验证表现出尿基质的有限影响,测量范围内的线性响应(通常为0.1-1.0μmg/ ml),并且量化的可接受不可接受(CV <15%)。发现一些分析物在储存时尿液不稳定。该方法已成功应用于17 936个未知样品的常规药物检测,其中2715(15%)含有148分析物中的52个。得出结论是,基于简单稀释的尿液和使用LC-HRMS在提取的离子色谱图中的方法设计可以提供尿液试验的分析系统,该系统满足了“黑盒子”解决方案的要求,可以替代应用免疫化学筛选自动分析仪。版权所有(c)2017 John Wiley&Sons,Ltd。

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