摘要
目的建立工作场所空气中醋酸乙烯酯的气相色谱-质谱(gas chromatography-mass spectrometry,GC-MS)检测方法。方法采用5%(V/V)对苯二酚-乙醇溶液浸渍的活性炭管采集空气样本,优化解吸、色谱和质谱条件,用二硫化碳解吸,DB-FFAP(60 m×0.32 mm×1.0μm)毛细管色谱柱分离,气相色谱-质谱法检测空气中的醋酸乙烯酯。结果建立的方法在质量浓度(0.008~186.240)mg/L范围内线性关系良好,r=0.9995,检出限为0.002 mg/L,定量限为0.008 mg/L,批内精密度分别为2.0%、2.5%、1.6%,批间精密度分别为1.4%、3.2%、1.8%。解吸效率分别为93.8%、97.2%、96.7%。低、中、高3个浓度水平回收率分别为98.5%、98.6%、103.3%。与国标GBZ/T 160.64—2004中醋酸乙烯酯热解吸-直接进样-气相色谱法对比,检出限和定量限均更低,定量检测范围更大,解吸效率更高。结论建立的工作场所空气中醋酸乙烯酯的液相解吸-气相色谱-质谱检测方法,检出限低,解吸率、精密度、灵敏度、回收率均较高,适合日常高通量检测需求。
Objective To establish a gas chromatography-mass spectrometry(GC-MS)for determination of vinyl acetate in workplace air.Methods Air samples were collected using activated charcoal tubes immersed with 5%(V/V)phenol/ethanol solution.The desorption,chromatography and mass spectrometry conditions were optimized,and air samples were desorbed with carbon disulfide,and separated with DB-FFAP columns(60 m×0.32 mm×1.0μm).The vinyl acetate was determined in air samples using GC-MS.Results The established GC-MS assay showed a good linear relationship at mass concentrations of 0.008 to 186.240 mg/L(r=0.9995),with a detection limit of 0.002 mg/L,a limit of quantitation of 0.008 mg/L,intrabatch precision of 2.0%,2.5% and 1.6%,interbatch precision of 1.4%,3.2% and 1.8%,and desorption efficiency of 93.8%,97.2% and 96.7%,respectively.The recovery rates were 98.5%,98.6% and 103.3% for low-,moderate-and high-concentrations of air samples,respectively.Compared with the vinyl acetate thermal desorption-direct injection-gas chromatography described in the Methods for determination of unsaturated aliphatic esters in the air of workplace(GBZ/T 160.64—2004),the established GC-MS showed a lower detection limit and limit of quantitation,wider range of quantitative detection and higher desorption efficiency.Conclusion The established liquid-phase desorption-GC-MS has a low limit of detection,and high desorption efficiency,precision,sensitivity and recovery rate for determination of vinyl acetate in workplace air,which is suitable for daily high-throughput detection.
作者
张琳昀
李泽冉
朱峰
ZHANG Lin-yun;LI Ze-ran;ZHU Feng(Jiangsu Provincial Center for Disease Control and Prevention,Jiangsu Nanjing 210009,China)
出处
《江苏预防医学》
CAS
2023年第2期133-135,共3页
Jiangsu Journal of Preventive Medicine
关键词
醋酸乙烯酯
二硫化碳
气相色谱质谱法
工作场所空气
Vinyl acetate
Carbon disulfide
Gas chromatography-mass spectrometry
Workplace air
