气相色谱质谱联用法测定现制饮料中甜蜜素  

Determination of sodium cyclamate in freshly made beverages using gas chromatography⁃mass spectrometry

作　　者：曹慧[1] 沈超南 陈鹏 赵婷婷 雍宗锋 CAO Hui;SHEN Chao⁃nan;CHEN Peng;ZHAO Ting⁃ting;YONG Zong⁃feng(Suqian Municipal Center for Disease Control and Prevention,Jiangsu Suqian 223800,China)

机构地区：[1]宿迁市疾病预防控制中心,江苏宿迁223800

出　　处：《江苏预防医学》2024年第5期565-567,595,共4页Jiangsu Journal of Preventive Medicine

基　　金：江苏省预防医学课题(Y2018069)

摘　　要：目的建立气相色谱质谱联用法(GC-MS)测定现制饮料中甜蜜素。方法优化衍生化条件和仪器条件,以标准系列工作溶液中甜蜜素的浓度为横坐标,以衍生物环己醇亚硝酸酯和环己醇2峰面积之和为纵坐标,绘制标准曲线;计算检出限、回收率和精密度;测试24 h内稳定性。并采集市售现制饮料进行检测。结果优化后的衍生化条件和仪器条件为:取样品约2 g,加水稀释至10 mL,加入5 mL正己烷、2.5 mL硫酸溶液和2.5 mL亚硝酸钠溶液,于冰浴中放置30 min衍生化,用质谱选择离子扫描模式(SIM)进行定性定量分析。甜蜜素在质量浓度2~200μg/mL范围内线性良好(r^(2)>0.999),加标回收率为89.1%~116%,相对标准偏差(RSDs)<5.0%,方法检出限为0.001 g/kg。24 h内检测结果RSD为3.6%。20份市售现制饮料甜蜜素检出率为15.00%,均未超标。结论建立的方法灵敏度高、准确度高、稳定性好,可以满足日常检测要求。Objective To establish a gas chromatography⁃mass spectrometry(GC⁃MS)for determination of sodium cyclamate in freshly made beverages.Methods Derivatization and apparatus conditions were optimized.The cyclohexylsulfamic acid concentration in the standard working solution served as a horizontal coordinate,and the sum of the peak area of cyclohexylsulfamic acid derivatives cyclohexanol nitrite ester and 2⁃cyclohexanol served as a vertical coordinate to create a standard curve.The detection limit,recovery and precision were calculated,and the stability within 24 hours was tested.In addition,the sodium cyclamate was determined in market⁃sold freshly made beverages.Results The derivatization and apparatus conditions were optimized as follows:approximately 2 g samples were diluted with water into 10 mL,added with 5 mL N⁃hexane,2.5 mL sulfuric acid solution and 2.5 mL sodium nitrite solution,and derivatized on ice bath for 30 min.MS was performed with a selected ion monitoring mode for qualitative and quantitative analyses.Sodium cyclamate had a good linear relationship at a mass concentration of 2 to 200μg/mL,r^(2)>0.999,spiked recovery rates of 89.1%to 116%,relative standard deviations(RSDs)of<5.0%,and a detection limit of 0.001 g/kg,respectively.The RSD of detection results was 3.6%within 24 hours.In addition,the detection of sodium cyclamate was 15.00%in 20 market⁃sold freshly made beverages,which all did not exceed the standard.Conclusions The established GC⁃MS is high in sensitivity,accuracy and stability,which may meet the demands of daily determinations.

关 键 词：甜蜜素 现制饮料 气相色谱质谱联用 选择离子扫描 

分 类 号：R113[医药卫生—公共卫生与预防医学]