MIP-SPE-HPLC法测定功能性油脂中15种多环芳烃  

Determination of 15 Polycyclic Aromatic Hydrocarbons in Functional Oils by Molecularly Imprinted Solid Phase Extraction with High Performance Liquid Chromatography

作　　者：邓龙[1] 周思 罗晓燕[2] 黄佳佳[1] DENG Long;ZHOU Si;LUO Xiaoyan;HUANG Jiajia(Guangdong Food and Drug Vocational College,Guangzhou 510520;Guangzhou Centre for Disease Control and Prevention,Guangzhou 510440)

机构地区：[1]广东食品药品职业学院,广州510520 [2]广州市疾病预防控制中心,广州510440

出　　处：《食品工业》2023年第9期315-320,共6页The Food Industry

基　　金：广东省医学科学技术研究基金项目(A2020197、A2022496);广东省普通高校青年创新人才项目(2020KQNCX172);广东食品药品职业学院自然科学研究项目(2019ZR21,2020ZR16,2022ZR12)。

摘　　要：建立分子印迹固相萃取-高效液相色谱测定功能性油脂中15种多环芳烃的检测方法。通过优化淋洗、洗脱和氮吹等条件提高轻质多环芳烃回收率。样品经正己烷稀释,多环芳烃分子印迹固相萃取柱净化,二氯甲烷洗脱,氮吹至100μL,乙腈定容。以乙腈和水为流动相进行梯度洗脱,采用Waters PAH C18色谱柱分离,通过荧光检测器进行测定。结果表明:15种目标物在0.2~50μg/L质量浓度范围内线性关系良好,相关系数均大于0.997,方法定量限为0.1~0.6μg/kg;1, 5和10μg/kg这3个水平加标回收率在72.3%~98.5%之间,相对标准偏差(S_(RSD), n=6)小于6.1%。用该方法对27份市售功能性油脂进行检测,目标多环芳烃检出率为100.0%。该方法简单、快速、可靠,可满足功能性油脂中多环芳烃的检测。A rapid method for the determination of 15 polycyclic aromatic hydrocarbons(PAHs)in functional oils was developed by using molecularly imprinted solid phase extraction(MIP-SPE)with high performance liquid chromatography(HPLC).The conditions of washing,elution and nitrogen blowing were optimized to improve the recovery of light PAHs.After dilution with hexane,the samples were purified using a MIP-SPE column and eluted with dichloroethane.The obtained solution was evaporated to 100μL under N_(2) gas flow before being reconstituted in acetonitrile.Separation of the 15 kinds of PAHs was achieved on a PAH C_(18) column and detected by fluorescence detector with acetonitrile and water mobile phases.The results indicated good linear relationships in the range of 0.2-50μg/L for 15 targets with correlation coefficients were higher than 0.997.The limits of quantification of the individual PAHs ranged from 0.1 to 0.6μg/kg,and the recoveries at three spiked levels of 1,5 and 10μg/kg ranged from 72.3%to 98.5%with relative standard deviation(S_(RSD), n=6)less than 6.1%.The established method was applied to the analysis of PAHs in 27 commercially available products,and PAHs were 100%detected.The method was fast,reliable and sensitive,which could be applied to detect 15 kinds of PAHs in functional oil.

关 键 词：功能性油脂 多环芳烃 分子印迹固相萃取 高效液相色谱 

分 类 号：O657.72[理学—分析化学] TS227[理学—化学]