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作 者:刘莹 张文馨 闫茗 羊银 吴翠玲[2] 李永发 张晓梅 LIU Ying;ZHANG Wenxin;YAN Ming;YANG Yin;WU Cuiling;LI Yongfa;ZHANG Xiaomei(Instrument Analysis Department,Tianjin Institute for Food Safety Inspection Technology,Tianjin 300310,China;Agilent Technologies(China)Co.,Ltd.,Beijing 100102,China;Beijing Shunyi District Metrology and Food and Drug Testing Center,Beijing 101300,China)
机构地区:[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
出 处:《食品研究与开发》2025年第8期198-204,共7页Food Research and Development
基 金:天津市食品安全检测技术研究院新羽科技计划项目(SJY2022S05)。
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×1.4μm)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250μL,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。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 or⁃thogonal 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×1.4μm).Then they were detected in multiple reflection monitoring mode and quantified by the internal stan⁃dard 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 250μL.Under these conditions,the recovery of 2⁃chloroethanol was 95.1%.The 2⁃chloroethanol showed a good linearity in the concentration range of 10.0-1000.0 ng/mL(R2≥0.9980),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 recov⁃ery 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.
关 键 词:QuEChERS法 气相色谱串联质谱法 酶解 食品增稠剂 环氧乙烷 2-氯乙醇
分 类 号:TS207.3[轻工技术与工程—食品科学]
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