LC-AJS ESI-MS/MS测定蒸馏酒中三氯蔗糖的方法研究  

Determination of Sucralose in Distilled Liquor by LC-AJS ESI-MS/MS

作　　者：孙琳 周玉 唐艳荣 孙莉 SUN Lin;ZHOU Yu;TANG Yanrong;SUN Li(Yellow Crane Tower Distillery(Xianning)Co.Ltd.,Xianning,Hubei 437000;Yellow Crane Tower Distillery Co.Ltd.,Wuhan,Hubei 430050,China)

机构地区：[1]黄鹤楼酒业(咸宁)有限公司,湖北咸宁437000 [2]黄鹤楼酒业有限公司,湖北武汉430050

出　　处：《酿酒科技》2025年第3期138-141,共4页Liquor-Making Science & Technology

摘　　要：建立使用液相色谱-质谱联用仪测定蒸馏酒中三氯蔗糖含量的分析方法,对国标方法标准品的稀释过程和质谱条件进行优化。分析柱为Agilent ZORBAX RX-C_(18)(4.6×100 mm,2.7μm),流动相为水和甲醇,流速为0.5 m L/min,标准曲线从中间液采用逐级稀释的方法进行配制,外标法进行定量分析。该方法在0.0~10 mg/L范围内线性关系良好(相关系数r=0.9999),仪器检出限是0.05 mg/L,定量限是0.1 mg/L;样品中分别添加低、中、高三个水平浓度的三氯蔗糖时,回收率在85%~105%范围内,相对偏差均小于10%。本方法主要在GB 5009.298—2023《食品中三氯蔗糖的测定》基础上改变标准品配制方式和对液相质谱质谱条件进行优化,使标准曲线的线性关系更好、响应更好,提高蒸馏酒中的三氯蔗糖检测的准确度。从方法验证学多方面进行分析比较,均满足方法使用要求,故本方法可用于蒸馏酒中三氯蔗糖含量的分析。A method for the determination of sucralose in distilled liquor was developed by using liquid chromatography-mass spectrometry.The dilution process and mass spectrometry conditions provided in the national standard were optimized.The analytical column was Agilent ZORBAX RX-C_(18)(4.6×100 mm,2.7μm).The mobile phase was water and methanol,and the flow rate was 0.5 mL/min.The standard curve was configured from the intermediate solution by gradient dilution,and quantitative analysis was performed by external standard method.The linear relationship was good in the range of 0.05 mg/L to 10 mg/L(r=0.9999).The detection limit was 0.05 mg/L and the quantitative limit was 0.1 mg/L.The recoveries ranged from 85%to 105%with relative deviations less than 10%when low,medium and high concentrations of sucralose were added to the samples respectively.This method is based on the method provided in national standard GB 5009.298-2023,and optimizes the configuration method of standard samples and conditions of LC-MS/MS,so as to improve the detection accuracy of sucralose in distilled liquor.Methodology verification proves that this method can be used for the analysis of sucralose content in distilled liquor.

关 键 词：液相色谱-质谱联用仪 蒸馏酒 标准曲线 方法优化 方法学研究 

分 类 号：TS262.3[轻工技术与工程—发酵工程] TS261.7[轻工技术与工程—食品科学与工程]