固相萃取-高效液相色谱法检测植物油中15种多环芳烃  

Determination of 15 polycyclic aromatic hydrocarbons in vegetable oils by solid phase extraction coupled with high performance liquid chromatography

作　　者：杜瑞 万丽斌 高火亮 高海东 DU Rui;WAN Li-bin;GAO Huo-liang;GAO Hai-dong(Henan Commerce Science Institute Co.,Ltd.,Zhengzhou 450002,Henan,China)

机构地区：[1]河南省商业科学研究所有限责任公司,河南郑州450002

出　　处：《粮食与油脂》2022年第1期158-162,共5页Cereals & Oils

基　　金：河南省科学院基本科研业务费项目(200611085)。

摘　　要：建立了固相萃取-高效液相色谱荧光法检测植物油中15种多环芳烃(PAHs)的新方法。植物油样品经正己烷稀释后,非芝麻油样品采用多环芳烃专用柱净化,芝麻油样品采用硅胶柱串接多环芳烃专用柱净化,ZORBAX Eclipse PAH色谱柱(4.6 mm×250 mm,5μm)分离,以水-乙腈作为流动相,梯度洗脱,外标法定量。15种PAHs在1~200μg/L范围内呈线性关系,相关系数(r)均大于0.995。方法检出限为0.15~0.65μg/kg、定量限为0.5~2μg/kg。在2、5、20、50μg/kg这4个添加水平范围内,14种PAHs的回收率为62%~96%,萘(Nap)的回收率为53%~57%;相对标准偏差为0.5%~6.2%(n=6)。方法前处理操作简单、重复性好、检测灵敏度高,可适用于植物油中15种多环芳烃的检测。A new method for the determination of 15 polycyclic aromatic hydrocarbons( PAHs) in vegetable oils by solid phase extraction and high performance liquid chromatography with fluorescence was established. The vegetable oil samples were diluted with n-hexane,and then the non-sesame oil samples were purified by PAHs special column,whereas sesame oil samples were purified by silica gel column connected with PAHs special column. Chromatographic separation was performed on a ZORBAX Eclipse PAH column( 4.6 mm × 250 mm,5 μm) with water-acetonitrile as mobile phase by gradient elution. The external standard method was used for quantification. The 15 kinds of PAHs showed a linear relationship in the range of 1 ~ 200 μg/L with all the correlation coefficients( r) greater than 0. 995. The detection limit( LOD) and limit of quantification( LOQ) were 0. 15 ~0. 65 μg/kg and 0. 5 ~2 μg/kg,respectively. At the four levels of 2,5,20,50 μg/kg,the recoveries of 14 PAHs were in the range of 62 % ~ 96 %,and the recoveries of naphthalene( Nap) were in the range of 53 % ~ 57 %. The relative standard deviation was 0. 5 % ~ 6. 2 %( n = 6). The method provided simple pretreatment,good reproducibility and high detection sensitivity,which could be applied to detect 15 kinds of PAHs in vegetable oil.

关 键 词：固相萃取 高效液相色谱-荧光法 多环芳烃 植物油 

分 类 号：TS227[轻工技术与工程—粮食、油脂及植物蛋白工程]