气相色谱-三重四极杆质谱法同时测定方便面中环氧乙烷及其代谢物2-氯乙醇

Simultaneous determination of ethylene oxide and its metabolite 2-chloroethanol in instant noodles by gas chromatography-triple quadrupole mass spectrometry

中文关键词:  环氧乙烷  2-氯乙醇  方便面  气相色谱-三重四极杆质谱法

英文关键词:ethylene oxide  2-chloroethanol  instant noodles  gas chromatography-triple quadrupole mass spectrometry

中文摘要:

      目的 建立气相色谱-三重四极杆质谱法同时测定方便面中环氧乙烷及代谢物2-氯乙醇的分析方法。方法 样品经粉碎后用乙腈提取, 提取液经分散固相萃取净化, 采用气相色谱-三重四极杆质谱法测定, 基质标准工作曲线外标法定量。结果 该方法中环氧乙烷及2-氯乙醇在0.005~1.000 μg/mL浓度范围内的线性关系较好, 环氧乙烷的相关系数(r2)为0.9997, 2-氯乙醇的r2为0.9999, 同时在0.15、1.50和5.00 mg/kg水平下进行加标回收实验, 环氧乙烷的回收率为83.3%~100.4%, 相对标准偏差(relative standard deviations, RSDs)为0.3%~2.3%, 2-氯乙醇的回收率为99.9%~112.2%, RSDs为0.1%~5.0%。环氧乙烷的定量限为0.3 mg/kg, 检出限为0.06 mg/kg; 2-氯乙醇的定量限为0.1 mg/kg, 检出限为0.02 mg/kg。采用建立的方法对流通领域阳性样品分析, 发现脱水蔬菜中2-氯乙醇检出含量较高, 面饼中2-氯乙醇检出含量较低, 调味粉和调味酱未检出2-氯乙醇, 研究的样品中均未检出环氧乙烷。结论 本方法适用于食品基质, 尤其是方便面中环氧乙烷及代谢物2-氯乙醇的同时检测, 具有较好的检测准确性和灵敏度。

英文摘要:

      Objective To establish a method for the simultaneous determination of ethylene oxide and its metabolite 2-chloroethanol in instant noodles by gas chromatography-triple quadrupole mass spectrometry. Methods The samples were crushed and extracted with acetonitrile, and the extracts were purified by dispersive solid-phase extraction, determined by gas chromatography-triple quadrupole mass spectrometry, and quantified by external standard method of matrix standard working curve. Results In this method, the linear relationships of ethylene oxide and 2-chloroethanol were good in the concentration range of 0.005?1.000 μg/mL. the correlation coefficient (r2) of ethylene oxide was 0.9997, and the r2 of 2-chloroethanol was 0.9999. Meanwhile, the recovery experiments were carried out at the levels of 0.15, 1.50 and 5.00 mg/kg, founding the recoveries were 83.3%?100.4% with relative standard deviations (RSDs) of 0.3%?2.3% for ethylene oxide, the recoveries were 99.9%?112.2% with RSDs of 0.1%?5.0% for 2-chloroethanol. The results of the experiment indicated that the limit of quantification of ethylene oxide was 0.3 mg/kg and the limit of detection was 0.06 mg/kg; the limit of quantification of 2-chloroethanol was 0.1 mg/kg and the limit of detection was 0.02 mg/kg. Using the established method to analyze the positive samples in the circulation field, it was found that the detected content of 2-chloroethanol in dehydrated vegetables was high, the detected content of 2-chloroethanol in flour cake was low, 2-chloroethanol was not detected in seasoning powder and sauce, and ethylene oxide was not detected in the studied samples. Conclusion The investigation carried out the method is suitable for the simultaneous detection of ethylene oxide and its metabolite 2-chloroethanol in food matrices, particularly in instant noodles, that has good detection accuracy and sensitivity.