目的:建立QuEChERS(Quick,Easy,Cheap,Effective,Rugged and Safe)-气相色谱-串联质谱法,用于测定食品中环氧乙烷和2-氯乙醇的残留.方法:样品经冷冻粉碎后用预冷的乙腈提取,提取液经分散固相萃取净化.选择DB-624毛细管色谱柱,分流进样,采用多反应监测(Multiple reaction monitoring,MRM)模式检测,外标法定量.结果:环氧乙烷和2-氯乙醇在5.00～200.0 ng/mL线性关系良好(相关系数r＞0.999),定量限为0.010 mg/kg,检出限为0.005 mg/kg.在方便面、冰淇淋、花生、香辛料、沙拉酱、饮料基质中进行加标回收试验,添加水平为0.010、0.020 mg/kg和0.100 mg/kg时,环氧乙烷的回收率范围为74.9％～99.5％,相对标准偏差(Relative standard deviations,RSDs)为0.98％～4.78％;2-氯乙醇的回收率范围为82.1％～117.0％,RSDs为1.32％～4.34％.采用该方法对实际样品进行分析,环氧乙烷均未检出,有3款香草味冰淇淋中检出2-氯乙醇,含量为0.023～0.038 mg/kg.结论:该方法操作简单、灵敏度高、重现性好,适用于多种食品基质中环氧乙烷和2-氯乙醇的同时检测.
Simultaneous Determination of Ethylene Oxide and 2-Chloroethanol Residues in Food by QuEChERS-Gas Chromatography-Tandem Mass Spectrometry
Objective:To establish a QuEChERS(Quick,Easy,Cheap,Effective,Rugged and Safe)-gas chromatography-tandem mass spectrometry method for the simultaneous determination of ethylene oxide and 2-chloroethanol residues in food.Methods:The samples were extracted with pre-cooled acetonitrile after freezing and crushing,the extract was purified by dispersive solid-phase extraction.Utilizing a DB-624 capillary column with for split injection.The multiple reaction monitoring(MRM)mode was used for detection and external standard method for quantification.Results:The linear relationship between ethylene oxide and 2-chloroethanol was good at 5.00-200.0 ng/mL(correlation coefficient r＞0.999),the limit of quantitation was 0.010 mg/kg,and the limit of detection was 0.005 mg/kg.The recovery tests were carried out in instant noodles,ice cream,peanut,spices,salad dressing and beverage matrix,when the supplemental levels were 0.010,0.020,0.100 mg/kg,the recoveries of ethylene oxide ranged from 74.9％ to 99.5％,the relative standard deviations(RSDs)ranged from 0.98％ to 4.78％,and the recoveries of 2-chloroethanol ranged from 82.1％ to 117.0％,with RSDs ranging from 1.32％ to 4.34％.This method was used to analyze the actual samples,ethylene oxide was not detected,2-chloroethanol was detected in 3 vanilla ice creams,with the content of 0.023-0.038 mg/kg.Conclusion:The method has the advantages of simple operation,high sensitivity and good reproducibility,and is suitable for the simultaneous detection of ethylene oxide and 2-chloroethanol in multiple food matrices.
QuEChERSgas chromatography-tandem mass spectrometryethylene oxide2-chloroethanol
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