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作 者:陈子凡 董莹 郑少锋 陈碧聪 张南峰 CHEN Zi-Fan;DONG Ying;ZHENG Shao-Feng;CHEN Bi-Cong;ZHANG Nan-Feng(Heyuan Food Inspection Institute,Heyuan 517000;Huangpu Customs District,Dongguan 523000;Guangdong Provincial Key Laboratory of Intelligent Port Security Inspection,Guangzhou 510510)
机构地区:[1]河源市食品检验所,河源517000 [2]黄埔海关技术中心,东莞523000 [3]广东省口岸安全智能化检测重点实验室,广州510510
出 处:《中国口岸科学技术》2024年第3期84-90,共7页China Port Science and Technology
摘 要:本文建立一种测定腌渍蔬菜中三氯蔗糖的超高效液相色谱串联质谱仪-正电离喷雾模式(ESI+)的方法。腌渍蔬菜样品用乙腈作为提取液,加入QuECHERS试剂振摇,离心后取上层澄清液,过0.22μm滤膜后上机检测。液相色谱采用C18色谱柱,以超纯水和甲醇为流动相梯度洗脱分离目标物。质谱选择419 m/z作为前体离子,239 m/z作为定量离子,221 m/z、203 m/z作为定性离子,采用外标法进行定量。结果表明三氯蔗糖的标准曲线在0.5~100 ng/mL之间呈线性关系,相关系数R^(2)>0.998,加标回收率为84.3%~99.1%,精确度为5.3%,检出限为0.1μg/kg,定量限为0.2μg/kg。结果表明,该方法具有快速高效、检测下限低、灵敏度高、重复性好的特点,可作为腌渍蔬菜中三氯蔗糖含量测定方法。An ultra-performance liquid chromatography-tandem mass spectrometry electrospray ionization positive mode(ESI+)method was developed for the determination of sucralose in pickled vegetables.The pickled vegetable sample was extracted with acetonitrile and shaken with QuECHERS reagent.The upper clear solution was taken via centrifugation,and passed through 0.22μm Perform machine testing after filtering the membrane.Liquid chromatography uses C_(18)column,with ultrapure water and methanol as the mobile phase for gradient elution and separation of the target substance.The mass spectrometry selected 419 m/z as the parent ion,239 m/z as the quantitative ion,and 221 m/z and 203 m/z as the qualitative ions.The external standard method was used for quantification.The results show that the standard curve of sucralose exhibits a linear relationship between 0.5 and 100 ng/mL with a correlation coefficient R^(2)>0.998.The added standard recovery rate was 84.3%to 99.1%,the relative standard deviation 5.3%,and the detection limit 0.1μg/kg,with a quantification limit of 0.2μg/kg.With low detection limit,high sensitivity,and good repeatability,this method is rapid and efficient in determining the content of sucralose in pickled vegetables.
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