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固相萃取-超高效液相色谱荧光法测定植物油中苯并(a)芘
引用本文:王红青,韩里明,屠海云,林伟杰. 固相萃取-超高效液相色谱荧光法测定植物油中苯并(a)芘[J]. 食品科学, 2012, 33(14): 216-218
作者姓名:王红青  韩里明  屠海云  林伟杰
作者单位:杭州市质量技术监督检测院
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  
收稿时间:2011-06-10

Determination of Benzopyrene in Cooking Oil by Solid-Phase Extraction Coupled with Ultra Performance Liquid Chromatograph-Fluorescence Detection
WANG Hong-qing,HAN Li-ming,TU Hai-yun,LIN Wei-jie. Determination of Benzopyrene in Cooking Oil by Solid-Phase Extraction Coupled with Ultra Performance Liquid Chromatograph-Fluorescence Detection[J]. Food Science, 2012, 33(14): 216-218
Authors:WANG Hong-qing  HAN Li-ming  TU Hai-yun  LIN Wei-jie
Affiliation:(Hangzhou Institute of Calibration and Testing for Quality and Technology Supervision,Hangzhou 310019,China)
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.
Keywords:solid-phase extraction (SPE)  ultra performance liquid chromatography (UPLC)  fluorescence detection  benzopyrene  cooking oil  
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