高效液相色谱法测定饮料中10种防腐杀菌剂  

Simultaneous determination of 10 preservatives and bactericides in drinks using high performance liquid chromatography

作　　者：徐宜宏[1] 金雁[1] 姜玲玲[1] 于丽[1] 赵颖[1] 蒋施[1] 刘瑜[1] 钟钰[1] 李晓东[1] 周建南[1] 

机构地区：[1]沈阳出入境检验检疫局,辽宁沈阳110016

出　　处：《中国食品卫生杂志》2014年第5期445-448,共4页Chinese Journal of Food Hygiene

基　　金：国家质检总局科技计划项目(2011IK215;2014IK129);"十二五"国家科技支撑计划项目(2011BAK10B04-9)

摘　　要：目的建立了同时测定饮料中10种防腐杀菌剂的高效液相色谱-二极管阵列检测器（HPLC-DAD）测定方法。方法样品用甲醇提取,通过C8固相萃取柱净化,以甲醇-0.02 mol/L乙酸铵为流动相,经C18反相色谱柱（250 mm×4.6 mm,5.0μm）分离,二极管阵列检测器检测,外标法定量。结果 10种防腐杀菌剂在0.1～10.0μg/ml范围内线性关系良好（r≥0.995 1）,检出限为0.25～1.0μg/ml（S/N=10）,10种防腐杀菌剂在两种饮料基质（果汁饮料、碳酸饮料）中添加3个水平的样品中的回收率74.1%～94.1%;相对标准偏差为5.3%～15.1%。结论该方法操作简单、快速、检出限低,满足国内外对饮料类食品中上述10种防腐杀菌剂的限量要求,适用于饮料中10种防腐杀菌剂的检测。Objective A method was developed for the determination of 10 preservatives and bactericides in drinks by HPLC-DAD. Methods The samples were extracted by methanol and purified by solid phase extraction with a Cs SPE column. The analytes were separated on a Clseolumn, eluted by a gradient elution with 0. 02 mol/L ammonium acetate buffer and methanol, detected by diode assay detector, and quantified by external standard method. Results The calibration curve was linear within the concentration range of 0. 1-10. 0 ~g/mL （ r~〉0. 995 1 ）. The lower limit of detection in drink was 0. 25- 1.0 0,g/ml （S/N = 10）. The relative recoveries of 10 preservatives-bactericides in fruit juice drinks and carbonated drinks with 3 spiked levels were 74. 1% -94. 1% , and relative standard deviations （RSD） were 5.3% -15.1%. Conclusion The method was simple, fast, low detection limit, meet for drinks foods at home and abroad in the above 10 kinds of antiseptic fungicide limited requirements, applicable to 10 kinds of preservatives and bactericides in drinks.

关 键 词：固相萃取 高效液相色谱 防腐剂 饮料 食品安全 

分 类 号：O657.72[理学—分析化学] R155[理学—化学]