气相色谱-静电场轨道阱高分辨质谱测定植物油中57种持久性有机污染物  

Determination of 57 persistent organic pollutants in vegetable oil by gas chromatography-electrostatic field orbitrap high resolution mass spectrometry

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作  者:黄云霞 孟志娟 范素芳[1] 赵丽敏 李强[1] HUANG Yun-xia;MENG Zhi-juan;FAN Su-fang;ZHAO Li-min;LI Qiang(Hebei Food Safety Key Laboratory,Key Laboratory of Special Food Supervision Technology for State Market Regulation,Hebei Engineering Research Center for Special Food Safety and Health,Hebei Food Inspection and Research Institute,Shijiazhuang 050000,Hebei,China)

机构地区:[1]河北省食品安全重点实验室,国家市场监管重点实验室(特殊食品监管技术),

出  处:《粮食与油脂》2024年第8期156-162,共7页Cereals & Oils

基  金:国家重点研发计划青年科学家项目(2022YFF1102900);河北省市场监督管理局科研计划项目(2022ZD14)。

摘  要:建立一种LPAS快速滤过净化柱结合气相色谱-静电场轨道阱高分辨质谱测定植物油中57种持久性有机污染物(POPs)残留量的方法。样品用乙腈-乙酸乙酯(体积比2:1)超声重复提取3次,提取液氮吹浓缩后经LPAS柱净化,用气相色谱-静电场轨道阱高分辨质谱在全扫描模式下检测。结果表明:57种POPs在0.4~100μg/L范围内线性关系良好,相关系数均大于0.9950;检出限为0.25~2.00μg/kg,定量限为0.8~6.0μg/kg;基质加标水平为0.8~60μg/kg时,平均回收率为62.4%~125.3%,相对标准偏差为1.2%~9.9%。利用该方法检测市售30例样品,其中8例检出多环芳烃,多氯联苯和有机氯农药均未检出。建立的方法简单、准确,适用于植物油中POPs残留的快速筛查。A method for determination of 57 persistent organic pollutants(POPs)residues in vegetable oil was established by LPAS rapid filtration purification combined with gas chromatography-electrostatic field orbitrap high resolution mass spectrometry(GC-Orbitrap-MS).The samples were ultrasonically extracted with acetonitrile-ethyl acetate(volume ratio 2:1)for three times.The extract was concentrated by nitrogen blowing,purified by LPAS column,and detected by GC-Orbitrap-MS in full scann mode.The results showed that the linear relationships for 57 POPs were good in the range of 0.4-100μg/L,and the correlation coefficients were above 0.9950.The limits of detection were in the range of 0.25-2.00μg/kg and the limits of quantitation were in the range of 0.8-6.0μg/kg.With spike levels in the range of 0.8-60μg/kg,the average recoveries were in range of 62.4%-125.3%,and relative standard deviations were in range of 1.2%-9.9%.Polycyclic aromatic hydrocarbons were detected in 8 of 30 vegetable oil samples by the method,but no polychlorinated biphenyls and organochlorine pesticides were detected.The method was simple,accurate and suitable for the rapid screening of POPs in vegetable oil.

关 键 词:气相色谱-静电场轨道阱高分辨质谱 LPAS快速滤过型净化 持久性有机污染物 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]

 

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