高效液相色谱法测定饮料中10种防腐杀菌剂
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(沈阳出入境检验检疫局,辽宁 沈阳 110016)

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徐宜宏 女 工程师 研究方向为食品中有毒有害物质残留E-mail: daicybear1101@163.com

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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)


Simultaneous determination of 10 preservatives and bactericides in drinks using high performance liquid chromatography
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(Shenyang Entry-Exit Inspection and Quarantine Bureau,Liaoning Shenyang 110016,China)

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    摘要:

    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,5.0 μm)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0.1~10.0 μg/ml范围内线性关系良好(r≥0.995 1),检出限为0.25~1.0 μg/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。

    Abstract:

    A method was developed for the determination of 10 preservatives and bactericides in drinks by HPLC-DAD.MethodsThe samples were extracted by methanol and purified by solid phase extraction with a C8 SPE column. The analytes were separated on a C18 column, 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.ResultsThe calibration curve was linear within the concentration range of 0.1-10.0 μg/mL(r≥0.995 1). The lower limit of detection in drink was 0.25-1.0 μg/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%.ConclusionThe 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.

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徐宜宏,金雁,姜玲玲,于丽,赵颖,蒋施,刘瑜,钟钰,李晓东,周建南.高效液相色谱法测定饮料中10种防腐杀菌剂[J].中国食品卫生杂志,2014,26(5):445-448.

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  • 收稿日期:2014-06-09
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  • 在线发布日期: 2014-10-16
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