基于改进QuEChERS测定植物油中邻苯二甲酸酯类化合物的气相色谱串联质谱质谱方法研究  

Study on improved QuEChERS method of determing phthalate acid esters in plant oil with Gaschromatography-mass/mass spectrometry

作　　者：伍剑[1] 陈杰[1] 罗霞[1] 杨雯雯 朱珠 吉华贵[1] 钟天辉[1] WU Jian;CHEN Jie;LUO Xia;YANG Wen-wen;ZHU Zhu;JI Hua-gui;ZHONG Tian-hui(Deyang Center for Disease Control and Prevention,Deyang,Sichuan 618000,China)

机构地区：[1]德阳市疾病预防控制中心理化检验所,四川德阳618000

出　　处：《现代预防医学》2022年第23期4365-4371,共7页Modern Preventive Medicine

基　　金：2020年度德阳市科技计划项目社会发展领域--民生类重点研发项目(2020SZ042)。

摘　　要：目的针对现有方法的不足,改进QuEChERS程序,采用气相色谱串联质谱质谱仪(GC-MS/MS)建立植物油中16种邻苯二甲酸酯类化合物(PAEs)的检测方法。方法对前处理条件和仪器条件进行优化后,样品经乙腈超声提取,加入PSA+Silica净化,振荡离心后取上清液进行测定,外标法定量。结果各种PAEs出峰良好,方法线性范围为0.02 mg/L~1.00 mg/L,相关系数均大于0.998,方法检出限为0.00021 mg/kg~0.014 mg/kg,定量限为0.00068 mg/kg~0.048 mg/kg,3个加标浓度下的回收率为80.0%~103%,相对标准偏差(RSD%)为1.79%~6.96%,用本法检测了10个植物油样品,共有4种PAEs检出,分别是DBP、DEHP、DIBP和DNOP,本法和国标法检出值的相对偏差均小于10%。结论该方法具有简便、高效、灵敏、快速等优点,能够很好地完成植物油中PAEs含量的检测。Objective To improve QuEChERS process and establish the analytical method of 16 phthalate acid esters(PAEs)in plant oil with Gas chromatography-mass/mass spectrometry(QuEChERS-GC-MS/MS)in view of the shortcomings of the existing methods.Methods After optimizing the sample pretreatment and the instrument conditions,PAEs in samples were extracted by ultrasound-assisted acetonitrile,then cleaned up with PSA+Silica,followed by the supernatant being taken for determination after oscillating and centrifugating.The quantification was based on the external standard curves.Results The peak of various phthalate acid esters was good,and the linear ranges from 0.02 mg/L to 1.00 mg/L with the correlation coefficients were all above 0.998.The limits of detection(LODs)were 0.00021 mg/kg-0.014 mg/kg,and the limits of quantification(LOQs)were 0.00068 mg/kg-0.048 mg/kg.The recoveries at the three spiked concentrations were 80.0%-103%,and the relative standard deviations(RSDs)were 1.79%-6.96%.Ten plants samples were detected with the proposed method,and 4 PAEs were detected,including DBP,DEHP,DIBP and DNOP.The relative deviation of detected values between this method and National Standard Method was below 10%.Conclusion This method possesses the features of simple,highly efficient,sensitive,fast,and it can be adopted to properly determine phthalate acid esters contented in plant oil.

关 键 词：邻苯二甲酸酯类化合物 植物油 QUECHERS 气相色谱串联质谱质谱仪 

分 类 号：R135.1[医药卫生—劳动卫生]