食品科学 ›› 2012, Vol. 33 ›› Issue (14): 216-218.

• 分析检测 • 上一篇    下一篇

固相萃取-超高效液相色谱荧光法测定植物油中苯并(a)芘

王红青,韩里明,屠海云,林伟杰   

  1. 杭州市质量技术监督检测院
  • 收稿日期:2011-06-10 修回日期:2012-05-17 出版日期:2012-07-25 发布日期:2012-07-27
  • 通讯作者: 王红青 E-mail:wanghq@hzzjy.net

Determination of Benzopyrene in Cooking Oil by Solid-Phase Extraction Coupled with Ultra Performance Liquid Chromatograph-Fluorescence Detection

  • Received:2011-06-10 Revised:2012-05-17 Online:2012-07-25 Published:2012-07-27

摘要: 采用中性氧化铝小柱净化样品,建立固相萃取-超高效液相色谱荧光法测定植物油中苯并(a)芘的方法。样品以正己烷为提取剂,净化、蒸发浓缩后正己烷溶解,荧光检测器检测。流动相为乙腈-水(75:25,V/V),流速0.5mL/min,外标法定量。苯并(a)芘在0.10~50.0μg/L质量浓度范围内线性关系良好,相关系数R2为0.9998;在空白样品中添加3个水平的标准品,回收率在91.7%~97.5%之间,相对标准偏差均小于2%(n=3);最低检出限为0.01μg/kg,定量限为0.03μg/kg。方法操作简便、分析时间短、稳定性好、选择性好、灵敏度高,为植物油中苯并(a)芘的测定提供参考。

关键词: 固相萃取, 超高效液相色谱, 荧光检测, 苯并(a)芘, 植物油

Abstract: A method was developed for the determination of benzopyrene by solid-phase extraction on a neutral Al2O3 cartridge coupled with ultra performance liquid chromatography (UPLC). Benzopyrene in samples were extracted into n-hexane, cleaned up, and concentrated by rotary evaporation and dissolved in n-hexane again before chromatographic separation and fluorescence detection. The mobile phase was acetonitrile-water (75:25, V/V) at a flow rate of 0.5 mL/min. Benzopyrene was quantified by external standard method. A good linear relationship between peak area and benzopyrene concentration was achieved in the range of 0.10-50.0 μg/L (R2 = 0.9998). The mean spike recovery rates of benzopyrene at three concentration levels were in the range of 91.7%-97.5%, with relative standard deviation (RSD) of less than 2%. The limits of detection (LOD) and quantification (LOQ) were 0.01 μg/kg and 0.03 μg/kg, respectively. The developed method is characteristics of simple operation, good reproducibility, high sensitivity, and rapid, reliable and suitable determination for benzopyrene in cooking oil.

Key words: solid-phase extraction (SPE), ultra performance liquid chromatography (UPLC), fluorescence detection, benzopyrene, cooking oil

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