固相萃取-超高效液相色谱荧光法测定植物油中苯并(a)芘  被引量:13

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

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作  者:王红青[1] 韩里明 屠海云 林伟杰[1] 

机构地区:[1]杭州市质量技术监督检测院,浙江杭州310019

出  处:《食品科学》2012年第14期216-218,共3页Food Science

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。A method was developed for the determination of benzopyrene by solid-phase extraction on a neutral A1203 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 g/kg and 0.03 vtg/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.

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 

分 类 号:O657.72[理学—分析化学]

 

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