Centre for Radiation, Chemicals and Environmental Hazards (CRCE), Public Health England, Chilton OX11 0RQ, UK.
Centre for Radiation, Chemicals and Environmental Hazards (CRCE), Public Health England, Chilton OX11 0RQ, UK.
J Chromatogr B Analyt Technol Biomed Life Sci. 2019 Mar 1;1109:84-89. doi: 10.1016/j.jchromb.2019.01.030. Epub 2019 Jan 31.
Methyl salicylate has a long history of use as a chemical warfare agent simulant for volatile lipophilic compounds such as sulphur mustard. An improved isotope dilution GC-MS/MS method was developed, optimised and validated for the analysis of methyl salicylate in human skin and hair samples, for use in emergency decontamination volunteer studies. Following derivatisation, quantification was measured on a triple quadrupole mass spectrometer, set to EI mode and conducting multiple reaction monitoring of target ions. The mass transitions were 209 → 179 and 213 → 161 for quantitation of methyl salicylate and methyl salicylate D4, respectively whereas qualifier ion transitions used to verify identity were 209 → 169 and 213 → 89. The method achieved excellent coefficient of determination (R > 0.9968 to 0.9999) over the range of 0.5-5000 ng/ml and the LOD and LOQ were 0.05 ng/ml and 0.5 ng/ml. The method was further validated for accuracy (intra-day and inter-day average 100.28% to 102.03% and 99.48% to 102.33%, respectively) and precision (intra-day RSD 1.43% to 2.35%, inter-day RSD 1.91% to 2.97%) at three concentrations (25, 250 and 2500 ng/ml). The validated method was successfully used to identify methyl salicylate in samples of human skin generated during volunteer studies of emergency decontamination systems and in hair of staff conducting these studies.
水杨酸甲酯作为一种挥发性亲脂性化合物（如硫芥）的化学战剂模拟物，其使用历史悠久。本研究建立并验证了一种用于分析人体皮肤和头发样品中水杨酸甲酯的同位素稀释 GC-MS/MS 方法，用于紧急去污志愿者研究。衍生化后，在三重四极杆质谱仪上进行定量测量，采用 EI 模式并对目标离子进行多重反应监测。定量分析的质荷比跃迁分别为 209→179 和 213→161，用于定量分析水杨酸甲酯和水杨酸甲酯 D4；用于确证身份的定性离子跃迁分别为 209→169 和 213→89。该方法在 0.5-5000ng/ml 范围内获得了优异的决定系数（R>0.9968 至 0.9999），检出限和定量限分别为 0.05ng/ml 和 0.5ng/ml。该方法进一步验证了准确度（日内和日间平均回收率分别为 100.28%至 102.03%和 99.48%至 102.33%）和精密度（日内 RSD 为 1.43%至 2.35%，日间 RSD 为 1.91%至 2.97%），在三个浓度（25、250 和 2500ng/ml）下进行。该验证方法成功用于识别志愿者紧急去污系统研究中产生的人体皮肤样本和进行这些研究的工作人员头发中的水杨酸甲酯。
