本文已被:浏览 51次 下载 33次
投稿时间:2024-03-29
投稿时间:2024-03-29
中文摘要: 食品中的环氧乙烷在酸性条件下会转化为2-氯乙醇。采用QuEChERS 技术结合气相色谱串联质谱技术,建立一种能够快速、简便地单独检测食品增稠剂中2-氯乙醇残留量的分析方法。样品通过正交试验优化酶解工艺,经乙酸乙酯提取,QuEChERS 净化,利用DB-624 毛细管色谱柱(30 m×0.25 mm×1.4 μm)进行分离,采用多反应监测模式检测,内标法定量。结果表明,食品增稠剂中环氧乙烷的最佳提取工艺条件为酶解时间20 min、酶解温度35 ℃、纤维素酶添加量250 μL,该工艺条件下2-氯乙醇回收率为95.1%。2-氯乙醇浓度为10.0~1 000.0 ng/mL 时线性良好(R2≥0.998 0),检出限和定量限(limit of quantitation,LOQ)分别为0.025 mg/kg 和0.05 mg/kg。食品增稠剂中2-氯乙醇的平均回收率为70.6%~100.7%,平均相对标准偏差为5.7%~11.9%。该方法灵敏、准确,可用于食品增稠剂中环氧乙烷及其代谢物2-氯乙醇残留量的快速测定。
Abstract:Ethylene oxide in food is converted to 2-chloroethanol under acidic conditions. A quick and simple analytical method for the determination of 2-chloroethanol residues in food thickeners was developed by QuEChERS extraction method combined with gas chromatography-mass spectrometry (GC-MS/MS). The orthogonal test was carried out to optimize the enzymolysis process of the samples. The samples were extracted with ethyl acetate,purified by QuEChERS,and separated on a DB-624 capillary column (30 m×0.25 mm×1.4 μm). Then they were detected in multiple reflection monitoring mode and quantified by the internal standard method. According to the results,the optimal process conditions for the extraction of 2-chloroethanol from food thickeners were as follows: enzymolysis time of 20 min,enzymolysis temperature of 35 ℃,cellulase dosage of 250 μL. Under these conditions,the recovery of 2-chloroethanol was 95.1%. The 2-chloroethanol showed a good linearity in the concentration range of 10.0-1 000.0 ng/mL (R2≥ 0.998 0),with the limit of detection(LOD) and the limit of quantification( LOQ) of 0.025 mg/kg and 0.05 mg/kg respectively. The average recovery of 2-chloroethanol in food thickeners was 70.6%-100.7% with average relative standard deviations of 5.7%-11.9%. This sensitive and accurate method could be used for quick determination of ethylene oxide and its metabolite 2-chloroethanol residues in food thickeners.
keywords: QuEChERS gas chromatography-mass spectrometry enzymolysis food thickener ethylene oxide 2-chloroethanol
文章编号:202508025 中图分类号: 文献标志码:
基金项目:天津市食品安全检测技术研究院新羽科技计划项目(SJY2022S05)
作者 | 单位 |
刘莹1,张文馨1,闫茗1,羊银1,吴翠玲2,李永发1 *,张晓梅3 | 1.天津市食品安全检测技术研究院 仪器分析部,天津 300310;2.安捷伦科技(中国)有限公司,北京 100102;3.北京市顺义区计量和食品药品检测中心,北京 101300 |
Author Name | Affiliation |
LIU Ying1,ZHANG Wenxin1,YAN Ming1,YANG Yin1,WU Cuiling2,LI Yongfa1 *,ZHANG Xiaomei3 |
引用文本: