色谱

色谱 ›› 2012, Vol. 30 ›› Issue (03): 292-297.DOI: 10.3724/SP.J.1123.2011.11034

• 研究论文 • 上一篇    下一篇

固相萃取-高效液相色谱-蒸发光散射检测法同时检测食品中5种人工合成甜味剂

刘芳1, 王彦1, 王玉红2,3, 周君裔1, 阎超1*   

  1. 1. 上海交通大学药学院, 上海 200240; 2. 上海通微分析技术有限公司, 上海 201203; 3. 华东师范大学化学系, 上海 200062
  • 收稿日期:2011-11-21 修回日期:2012-01-04 出版日期:2012-03-28 发布日期:2012-05-02
  • 通讯作者: 阎超,博士生导师,教授,主要从事微分离分析和电色谱分离领域的研究. Tel: (021)34205673,
  • 基金资助:

    国家自然科学基金项目(21175092, 21105064)和国家重大科学仪器设备开发专项(2011YQ150072, 2011YQ15007204, 2011YQ15007207, 2011YQ15007210).

Simultaneous determination of five synthetic sweeteners in food by solid phase extraction-high performance liquid chromatography-evaporative light scattering detection

LIU Fang1, WANG Yan1, WANG Yuhong2,3, ZHOU Junyi1, YAN Chao1*   

  • Received:2011-11-21 Revised:2012-01-04 Online:2012-03-28 Published:2012-05-02

PDF

418

被引次数

92

摘要： 建立了高效液相色谱-蒸发光散射检测仪(HPLC-ELSD)同时检测食品中安赛蜜、糖精钠、甜蜜素、三氯蔗糖和阿斯巴甜5种甜味剂的方法。甜味剂经0.1%(v/v)甲酸缓冲液提取后,利用C18固相萃取小柱净化浓缩,以3 μm C18柱为分离柱,0.1%(v/v)甲酸(氨水调节pH=3.5)-甲醇(61:39, v/v)为流动相,经高效液相色谱法分离,蒸发光散射检测器进行检测。结果表明,5种甜味剂在30～1000 mg/L的范围内,具有良好的线性关系(相关系数大于0.997);在3个添加水平下,样品的平均回收率为85.6%～109.0%,相对标准偏差小于4.0%;方法检出限(LOD,信噪比(S/N)=3)分别为安赛蜜2.5 mg/L、糖精钠3 mg/L、甜蜜素10 mg/L、三氯蔗糖2.5 mg/L及阿斯巴甜5 mg/L。该方法简单、灵敏、操作成本低,可用于不同形态食品中多种甜味剂的同时检测。

关键词: 高效液相色谱, 固相萃取, 食品安全, 甜味剂, 蒸发光散射检测

Abstract: A high performance liquid chromatographic method with evaporative light scattering detection (HPLC-ELSD) was developed for the simultaneous determination of five synthetic sweeteners (acesulfame-K, saccharin sodium, sodium cyclamate, sucralose and aspartame) in food. The sweeteners were extracted by 0.1% (v/v) formic acid buffer solution. The extract of sample was cleaned up and concentrated with solid phase extraction (SPE) cartridge. Then the sweeteners were separated on a C18 column (3 μm) using 0.1% (v/v) formic acid buffer (adjusted to pH=3.5 with aqueous ammonia solution)-methanol (61:39, v/v) as mobile phase, and finally detected by ELSD. The results showed that the reasonable linearity was achieved for all the analytes over the range of 30~1000 mg/L with the correlation coefficients (r) greater than 0.997. The recoveries for the five sweeteners ranged from 85.6% to 109.0% at three spiked concentrations with the relative standard deviations (RSDs) lower than 4.0%. The limits of detection (LODs, S/N=3) were 2.5 mg/L for both acesulfame-K and sucralose, 3 mg/L for saccharin sodium, 10 mg/L for sodium cyclamate, and 5 mg/L for aspartame. The method is simple, sensitive and low cost, and has been successfully applied to the simultaneous determination of the five synthetic sweeteners in food.

Key words: evaporative light scattering detection (ELSD), food safety, high performance liquid chromatography (HPLC), sweeteners, solid-phase extraction (SPE)