Chen Xiaohong, Zhang Yu, Shi Yuejin, Cai Meiqiang, Jin Micong
Key Laboratory of Health Risk Appraisal for Trace Toxic Chemicals of Zhejiang Province, Ningbo Municipal Center for Disease Control and Prevention, Ningbo 315010, China.
School of Environmental Science and Engineering, Zhejiang Gongshang University, Hangzhou 310018, China.
Wei Sheng Yan Jiu. 2021 May;50(3):488-494. doi: 10.19813/j.cnki.weishengyanjiu.2021.03.024.
To establish a rapid and accurate method for the determination of trace acetaldehyde, acrolein, methacrylaldehyde, crotonaldehyde in the air by ultra-fast liquid chromatography-tandem mass spectrometry(UFLC-MS/MS).
The air sample was concentrated and derivatived by 3-methyl-2(3 H)-benzothiazolonhydrazone(MBTH), and the effect of derivative conditions including the concentration of MBTH, the pH, the derivative time and temperature was investigated. The stability of derivatives, the cracking mechanism of mass spectrometry, the matrix effect of the method and air sampling efficiency were studied. The chromatographic separation was carried out on a Shim-pack XR-ODS II column(100 mm×2. 0 mm, 2. 2 μm) by using water/methanol solution as the mobile phase with the gradient elution. Detection was performed in positive multi-reaction monitoring(MRM) mode for quantification by using external standard method.
The four analytes showed good linear relationship within the range of 1. 00-100 μg/L(calculated by aldehyde) with a correlation coefficient r≥0. 9990. The limits of quantitation(LOQs) of the method(concentrated with 10 L air) were 0. 5 μg/m~3 in air, for acetaldehyde, acrolein, methacrylaldehyde, crotonaldehyde. The recoveries of the method were 90. 6%-97. 8% at the three spiked levels, and the relative standard deviations(RSDs) were between 1. 9%-6. 4%(n=6), the average sampling efficiency was between 91. 0%-97. 1%.
The developed method is simple, less interference and specificity, and is suitable for the simultaneous rapid determination of trace acetaldehyde, acrolein, methacrylaldehyde, crotonaldehyde in air of work place.
建立一种超快速液相色谱 - 串联质谱法（UFLC-MS/MS）快速准确测定空气中痕量乙醛、丙烯醛、甲基丙烯醛、巴豆醛的方法。
空气样品经3 - 甲基 - 2（3H）- 苯并噻唑酮腙（MBTH）浓缩和衍生化，考察MBTH浓度、pH值、衍生时间和温度等衍生条件的影响。研究衍生物的稳定性、质谱裂解机理、方法的基质效应和空气采样效率。采用水/甲醇溶液为流动相，在Shim-pack XR-ODS II柱（100 mm×2. 0 mm，2. 2 μm）上进行梯度洗脱色谱分离。采用正离子多反应监测（MRM）模式，外标法定量检测。
4种分析物在1. 00 - 100 μg/L（以醛计）范围内线性关系良好，相关系数r≥0. 9990。该方法（采集10 L空气浓缩后）对空气中乙醛、丙烯醛、甲基丙烯醛、巴豆醛的定量限均为0. 5 μg/m³。在3个加标水平下，方法回收率为90. 6% - 97. 8%，相对标准偏差（RSDs）为1. 9% - 6. 4%（n = 6），平均采样效率为91. 0% - 97. 1%。
所建立的方法简便、干扰少、特异性强，适用于工作场所空气中痕量乙醛、丙烯醛、甲基丙烯醛、巴豆醛的同时快速测定。
