固相萃取-高效液相色谱串联质谱法测定食品中的三氯蔗糖  

Determination of sucralose in food by solid phase extraction and highperformance liquid chromatography-tandem mass spectrometry

作　　者：曾初欢 梁进祥 陈润禧 陈子键[2] 徐振林[2] ZENG Chuhuan;LIANG Jinxiang;CHEN Runxi;CHEN Zijian;XU Zhenlin(Guangdong Food Industry Association,Guangzhou 510080;College of Food Science,South China Agricultural University,Guangzhou 510642;Dongguan Daojiao Food Industry Association,Donguan 523000)

机构地区：[1]广东省食品行业协会,广州510080 [2]华南农业大学食品学院,广州510642 [3]东莞市道滘食品行业协会,东莞523000

出　　处：《中国食品添加剂》2023年第8期27-33,共7页China Food Additives

基　　金：国家自然科学基金(32060578);广东省基础与应用基础研究基金(2021B1515120042)。

摘　　要：利用固相萃取-高效液相色谱-串联质谱(SPE-HPLC-MS/MS)建立了食品中三氯蔗糖的分析检测方法。样品用水提取后经沉淀、超声、离心除杂后,过Oasis HLB柱净化,最后用水定容、过膜,经BEH C18柱(100 mm×2.1 mm,1.7μm)分离,以水和甲醇为流动相进行梯度洗脱,电喷雾负离子(ESI-)下采用多反应监测(MRM)模式检测。结果表明,三氯蔗糖在5种不同基质样品的绝对基质效应为21.2%~158.2%,在10~500 ng/m L浓度范围内线性关系良好,相关系数(r2)在0.997以上;白酒的检出限为0.02mg/kg,其他样品检出限为0.10 mg/kg;在低、中、高3个水平的平均加标回收率为83.2%~110.3%,相对标准偏差(RSDs)为2.00%~5.70%(n=6)。本方法简单、高效、灵敏度高、精密度好,能满足日常监督抽检中多种食品基质的三氯蔗糖测定。A solid-phase extraction high-performance liquid chromatography-tandem mass spectrometry(SPEHPLC-MS/MS)method was set up to determine the content of sucralose in foods.After water extraction,the sample was precipitated,sonicated,and centrifuged to remove impurities.It was purified on an Oasis HLB column,and finally diluted with water,filtered through a membrane,and passed through a BEH C18 column(100 mm×2.1 mm,1.7μm).Gradient elution was carried out with water and methanol as mobile phase.The test was conducted with multiple reaction monitoring(MRM)mode under negative electrospray ionization(ESI)condition.It was found that the absolute matrixes effect(AME)of sucralose were 21.2%〜158.2%,and the linearity of sucralose were good in the range of 10〜500 ng/mL,with the correlation coefficients(r2)were all above 0.997 in 5 distinct samples.The limit of detection of spirits and other samples were 0.02 mg/kg and 0.10 mg/kg,respectively.The average recoveries of all the samples were 83.2%〜110.3%with the relative standard deviations(RSDs)ranged from 2.00%to 5.70%(n=6)at three spiked levels.The developed method was specific,efficient,sensitive and accurate,which could meet the requirement of the supervision and inspection of sucralose in multiple food matrixes.

关 键 词：固相萃取 高效液相色谱-串联质谱 三氯蔗糖 基质效应 甜味剂 

分 类 号：TS202.3[轻工技术与工程—食品科学] TS207.3[轻工技术与工程—食品科学与工程]