优化液相色谱-串联质谱法测定食品中三氯蔗糖的含量

Optimization the method of determination of sucralose in food by liquid chromatography-tandem mass spectrometry

优化液相色谱-串联质谱法检测食品中三氯蔗糖含量。考察不同前处理方法 (未经过固相萃取柱净化直接上机、净化处理后上机),比较不同流动相梯度洗脱比例对回收率的影响,优化三氯蔗糖检测方法并进行方法学验证。试验结果表明,试样不经过固相萃取柱净化,仅通过调整流动相梯度洗脱比例、延迟出峰时间即能满足试验要求,该方法在质量浓度0.05~4.0μg/mL范围内线性良好,相关系数为0.999 2,白酒回收率为102.3%~105.8%,果冻回收率为100.0%~109.3%,挂面回收率为100.0%~109.6%,检出限、定量限均能够达到国家标准的要求。本方法简单、灵敏度和准确度均较高,适用于检验机构中三氯蔗糖含量的批量检测。

To establish a method for the determination of sucralose in food by liquid chromatography-tandem mass spectrometry(LCMS).Comparing the effects of unpurified by solid-phase extraction column and purified treatment,investigating the gradient elution ratio of different mobile phases on the recovery rate.To optimize the detection method of sucrose trichloride and conduct methodological verification.The unpurified samples could meet the experimental requirements by adjusting the gradient elution ratio of different mobile phases.The linear range were 0.05-4.0μg/mL,the correlation coefficient was 0.9992,the recoveries of sucralose in liquor were 102.3%~105.8%,the recoveries in jelly were 100.0%~109.3%,the recoveries in dried noodle were 100.0%~109.6%,and the limits of detection and quantification can meet the requirements of national standards.This method is simple,sensitive and accurate,which is suitable for routine test of sucralose in inspection institutions.