色谱

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离子抑制剂对苯甲酸等9种食品添加剂的反相液相色谱行为的影响

赵永纲, 陈晓红, 李小平, 姚珊珊, 金米聪*   

  1. 宁波市疾病预防控制中心 宁波市毒物研究与控制重点实验室, 浙江 宁波 315010
  • 收稿日期:2011-04-29 修回日期:2011-06-20 出版日期:2011-10-28 发布日期:2011-10-13
  • 通讯作者: 金米聪,博士,研究员,主要从事食品安全的检测技术研究. Tel: (0574)87274559,
  • 基金资助:
    宁波市自然科学基金项目(No. 2010A610010)和浙江省医药卫生科学研究基金项目(No. 2010KYB098).

Influences of ion-suppressors on retention behaviors of nine food additives in reversed-phase high performance liquid chromatographic separation

ZHAO Yonggang, CHEN Xiaohong, LI Xiaoping, YAO Shanshan, JIN Micong*   

  1. Ningbo Municipal Center for Disease Control and Prevention, Ningbo Key Laboratory of Poison Research and Control, Ningbo 315010, China
  • Received:2011-04-29 Revised:2011-06-20 Online:2011-10-28 Published:2011-10-13

摘要: 研究了反相高效液相色谱(RP-HPLC)流动相中酸性离子抑制剂三氟乙酸(TFA)与缓冲盐离子抑制剂TFA-乙酸铵(AmAc)对安赛蜜、糖精、咖啡因、阿斯巴甜、苯甲酸、山梨酸、甜菊糖苷、脱氢乙酸和纽甜等9种食品添加剂色谱保留行为的影响。着重探讨了TFA与TFA-AmAc作为离子抑制剂的有机调节剂作用,考察了乙腈-TFA水溶液和乙腈-TFA-AmAc水溶液流动相体系中溶质的保留因子与离子抑制剂体积分数之间的关系。在最佳流动相组成(乙腈-TFA (0.01%, v/v)-AmAc (2.5 mmol/L)水溶液)条件下梯度洗脱,苯甲酸等9种食品添加剂实现了基线分离。9种食品添加剂在10.0~100.0 mg/L内具有良好的线性关系(r2>0.9991);检出限为0.33~2.36 mg/L,定量限为1.11~7.80 mg/L;9种食品添加剂在空白干红葡萄酒中的添加回收率为87.61%~108.4%,其相对标准偏差为2.2%~9.4%。本实验结果对于食品中多组分食品添加剂的RP-HPLC分离分析方法的建立和优化具有较好的指导意义。

关键词: 反相高效液相色谱, 离子抑制剂, 葡萄酒, 三氟乙酸, 食品添加剂, 乙酸铵

Abstract: The influences of ion-suppressors on retention behaviors of nine food additives, i.e., acesulfame, saccharin, caffeine, aspartame, benzoic acid, sorbic acid, stevioside, dehydroacetic acid and neotame in reversed-phase high performance liquid chromatographic (RP-HPLC) separation were investigated. The organic modification effects of acids, i.e., trifluoroacetic acid (TFA) and buffer salts, i.e., TFA-ammonium acetate (AmAc) were studied emphatically. The relationships between retention factors of solutes and volume percentages of ion-suppressors in the mobile phase systems of acetonitrile-TFA aqueous solution and acetonitrile-TFA-AmAc aqueous solution were quantitatively established, separately. The separation of nine food additives was completed by a gradient elution with acetonitrile-TFA (0.01%, v/v)-AmAc (2.5 mmol/L) aqueous solution as the mobile phases. An RP-HPLC method was established for the simultaneous determination of nine food additives in red wine. In the range of 10.0~100.0 mg/L, nine food additives showed good linearity with the correlation coefficients (r2) larger than 0.9991. The limits of detection (LODs) were in the range of 0.33~2.36 mg/L and the limits of quantification (LOQs) were in the range of 1.11~7.80 mg/L. The spiked recoveries were between 87.61% and 108.4% with the relative standard deviations (RSDs) of 2.2%~9.4%. These results are of referential significance for the rapid establishment and accurate optimization of RP-HPLC separation for the simultaneous determination of food additives in other foods.

Key words: ammonium acetate, food additives, ion-suppressor, wine, reversed-phase high performance liquid chromatography (RP-HPLC), trifluoroacetic acid