UHPLC-MS/MS正电离喷雾模式测定腌渍蔬菜中的三氯蔗糖
Determination of Sucralose in Pickled Vegetables by UHPLC-MS/MS with Electrospray Ionization Positive Mode
陈子凡 1董莹 2郑少锋 2陈碧聪 1张南峰2
作者信息
- 1. 河源市食品检验所 河源 517000
- 2. 黄埔海关技术中心 东莞 523000;广东省口岸安全智能化检测重点实验室 广州 510510
- 折叠
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 0.22 μm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R2＞0.998,加标回收率为 84.3%～99.1%,精确度为 5.3%,检出限为 0.1 μg/kg,定量限为 0.2 μg/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.
Abstract
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 0.22 μm Perform machine testing after filtering the membrane.Liquid chromatography uses C18 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 R2＞0.998.The added standard recovery rate was 84.3%to 99.1%,the relative standard deviation 5.3%,and the detection limit 0.1 μg/kg,with a quantification limit of 0.2 μg/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.
关键词
三氯蔗糖/超高效液相色谱/三重四极杆质谱/电离喷雾正模式/腌渍蔬菜Key words
sucralose/high-performance liquid chromatography(HPLC)/triple quadrupole mass spectrometry/electrospray ionization positive mode/pickled vegetables引用本文复制引用
出版年
2024
NETL
NSTL
万方数据