全自动固相萃取-高效液相色谱法测定植物油中苯并(a)芘

许文雅,刘 瀛,周长民,张宏宏,林 洋,王 

(沈阳市食品药品检验所,辽宁沈阳 110122

摘要:建立了全自动固相萃取-高效液相色谱法测定植物油中苯并(a)芘的方法。采用正己烷作为提取溶剂,经分子印迹固相萃取柱净化,用二氯甲烷洗脱,按照优化的全自动固相萃取程序进行净化,将试样溶液注入高效液相色谱仪中进行检测,经Thermo Betasil C18柱分离,以乙腈-水=8218为流动相,流速1.0 mL/min,柱温30 ℃,采用荧光检测器检测,激发波长384 nm,发射波长406 nm。结果表明,苯并(a)芘在0.520.0 ng/mL浓度范围内与峰面积具有良好的线性关系,相关系数为0.999 999,方法检出限为0.06 μg/kg,定量限为0.2 μg/kg3个浓度水平下的平均加标回收率为92.2%103.8%,相对标准偏差(n6)为2.2%6.0%。该方法可大批量、全自动化处理样品,工作效率高;减少检验人员与试剂接触机会,安全性高;降低人员操作误差,准确性高,适用于植物油中苯并(a)芘的测定。

关键词:全自动固相萃取;高效液相色谱法;苯并(a)芘;植物油

中图分类号:TS207.3    文献标识码:A    文章编号:1674-506X202306-0150-0005


Determination of Benzo (a) pyrene in Vegetable Oil by Automated Solid Phase Extraction-High Performance Liquid Chromatography

XU Wenya, LIU Ying, ZHOU Changmin, ZHANG Honghong, LIN Yang, WANG Yun

Shenyang Institute for Food and Drug Control, Shenyang Liaoning 110122, China

AbstractAn automated solid phase extraction-high performance liquid chromatography method was established for the determination of benzo (a) pyrene in vegetable oil. N-hexane was used as the extraction solvent, the sample was purified by molecularly imprinted column, and eluted with dichloromethane. An automated solid phase extraction procedure was used for purification, and the sample solution was detected by high performance liquid chromatography, separated by Thermo Betasil C18 column with using acetonitrile-water82∶18 as mobile phase, the flow rate was 1.0 mL/min, column temperature was 30 ℃, and fluorescence detector was used for detection with excitation wavelength of 384 nm and emission wavelength of 406 nm. The method had a good linear relationship with the peak area in the mass concentration range of 0.520.0 ng/mL, the correlation coefficient was 0.999 999, the limit of detection was 0.06 μg/kg, the limit of quantification was 0.2 μg/kg, The average recoveries were 92.2%103.8%, and the relative standard deviations (n6) were 2.2%~6.0% . The method enables automated batch processing samples, has high working efficiency, reduces the exposure of tester to reagents, has high security, reduces personnel operation errors,and has high accuracy, and is suitable for the determination of benzo (a) pyrene in vegetable oil.

Keywords:automated solid phase extraction; high performance liquid chromatography; benzo (a) pyrene; vegetable oil

doi10.3969/j.issn.1674-506X.2023.06-025


收稿日期:2023-02-08

作者简介:许文雅(1990-),女,硕士,工程师。研究方向:食品检测。


引用格式:许文雅,刘瀛,周长民,.全自动固相萃取-高效液相色谱法测定植物油中苯并(a)芘[J].食品与发酵科技,2023,59(6):150-154.




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