气相色谱法快速测定饮料中甜蜜素  

Rapid determination of cyclamate in beverage by gas chromatography

作　　者：王金鑫 仇倩颖 杨清华[1] 施逸岚[1] WANG Jinxin;QIU Qianying;YANG Qinghua;SHI Yilan(Nantong Center for Disease Control and Prevention,Nantong 226007,China)

机构地区：[1]江苏省南通市疾病预防控制中心,江苏南通226007

出　　处：《化学分析计量》2022年第9期22-25,共4页Chemical Analysis And Meterage

基　　金：南通市卫健委青年课题B(QB2021023)。

摘　　要：建立以正己烷为提取试剂,超声波辅助提取,HP-5毛细色谱柱分离的饮料中甜蜜素含量的气相色谱测定方法。色谱柱初始温度为50 ℃,保持3 min,以10 ℃/min的速率升至100 ℃,保持0.5 min,以20 ℃/min的速率升至200 ℃,保持3 min;检测器温度为265 ℃;氢气流量为35 mL/min;空气流量为350 mL/min。通过优化的实验方法与国标法对比分析并绘制色谱图。甜蜜素衍生物出峰时间相对缩短,甜蜜素的质量浓度在0~1.6 mg/mL范围内与色谱峰面积具有良好的线性关系,相关系数为0.999 2,检出限为0.01 g/kg。样品测定结果的相对标准偏差小于0.7%(n=6),加标回收率为88.5%~103.3%。该检测方法操作便捷,检测高效,结果重现性好,为饮料中甜蜜素含量测定提供参考依据。A gas chromatography was established for the determination of cyclamate in beverage by HP-5 capillary chromatography with n-hexane as extraction reagent and ultrasonic assisted extraction.The initial temperature of the chromatographic column was 50 ℃ for 3 min,increased to 100 ℃ at the rate of 10 ℃/ min,kept for 0.5 min,increased to 200 ℃ at the rate of 20 ℃/ min,and kept for 3 min.The temperature of the detector was 265 ℃.The hydrogen flow rate was 35 mL/min.The air flow rate was 350 mL/min.The optimized experimental method was compared with the national standard method to analyze and draw chromatogram.The peak time of cyclamate derivatives was relatively shorter,the mass concentration of cyclamate had a good linear relationship with the chromatographic peak area in the range of 0–1.6 mg/mL,and the correlation coefficient was 0.999 2,the detection limit was 0.01 g/kg.The relative standard deviation of the sample determination results was less than 0.7% (n=6),and the recoveries of spiked standard were 88.5%–103.3%.This method is easy to operate,efficient and reproducible.It provides a reference for the determination of sodium cyclamate in beverages.

关 键 词：甜蜜素 气相色谱法 检出率 饮料 

分 类 号：O657.7[理学—分析化学]