气相色谱-静电场轨道阱高分辨质谱测定植物油中氯丙醇酯和缩水甘油酯  

Analysis of Chloropropanol Ester and Glycidyl Esters in Vegetable Oils by Gas Chromatography Orbitrap High-resolution Mass Spectrometry

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作  者:刘印平[1] 云鹏[1] 陈福尊[1] 路杨[1] 董彬[1] Liu Yinping;Yun Peng;Chen Fuzun;Lu Yang;Dong Bin(Hebei Provincial Center for Disease Control and Prevention,Shijiazhuang 050021)

机构地区:[1]河北省疾病预防控制中心,石家庄050021

出  处:《中国粮油学报》2025年第3期174-178,共5页Journal of the Chinese Cereals and Oils Association

基  金:河北省卫生健康委医学科学研究课题项目(20210363)。

摘  要:建立了气相色谱-静电场轨道阱高分辨质谱同时测定植物油中氯丙醇酯和缩水甘油酯的方法。样品经水解、净化、衍生后利用气相色谱-静电场轨道阱高分辨质谱仪进行测定,内标法定量。在全扫描模式下测定目标化合物的精确质量数,能够有效地去除植物油中基质干扰。测定FAPAS植物油质控样品进行方法验证,测定结果均在定值范围内。氯丙醇酯和缩水甘油酯在10~300 ng范围内线性良好,相关系数均大于0.9990。在10、100、300 ng 3个加标水平下,平均回收率为94.0%~105.3%之间,相对标准偏差(RSDs)小于15%。该方法检出限为0.01 mg/kg;定量限为0.03 mg/kg。经过实际样品的验证,发现该方法受灵敏度和基质干扰的影响较小,可以为复杂基质中氯丙醇酯和缩水甘油酯的筛查和确证提供新的技术手段。In this paper,an efficiency evaluation of chloropropanol ester and glycidyl esters in vegetable oils was established by gas chromatography Orbitrap high-resolution mass spectrometry(GC-Orbitrap MS).The oil sample was hydrolyzed,purified and derived,detected by internal standard method.Accurate mass measurements of the target compounds in full scan mode could eliminate matrix interference effectively.FAPAS quality control materials of vegetable oil were tested for method verification,and all the results were within the assigned value.The linear ranges of the chloropropanol ester and glycidyl esters were from 10 ng to 300 ng with good correlation coefficients greater than 0.9990.At the spiked levels of 10,100 ng and 300 ng,the average recoveries were from 94.0%to 105.3%,with the relative standard deviations(RSDs)below 15%.The limits of detection(LODs)were 0.01 mg/kg and the limits of quantification(LOQs)were 0.03 mg/kg,respectively.The validated method was applied to 32 real vegetable oils,demonstrating that this instrumentation was less affected by sensitivity and matrix interferences,and could provide a new technical tool for screening and further confirmation of chloropropanol esters and glycidyl esters in complex matrices.

关 键 词:氯丙醇酯 缩水甘油酯 高分辨质谱 筛查 确证 植物油 

分 类 号:O656[理学—分析化学]

 

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