QuEChERS—气相色谱—串联质谱测定食品中的多溴联苯和多溴二苯醚类阻燃剂  

Determination of Polybrominated Biphenyls and Polybrominated Diphenyl Ethers in Food by QuEChERS-Gas Chromatography Tandem Mass Spectrometry

作　　者：占永超 吴易峰 徐敦明 郭泽镔[2] 王鹭骁 袁文萱 钟莺莺 ZHAN Yongchao;WU Yifeng;XU Dunming;GUO Zebin;WANG Luxiao;YUAN Wenxuan;ZHONG Yingying(Technical Center of Xiamen Customs,Xiamen 361026;College of Food Science,Fujian Agriculture and Forestry University,Fuzhou 350002;Technical Center of Ningbo Customs,Ningbo 315048)

机构地区：[1]厦门海关技术中心,福建厦门361026 [2]福建农林大学食品科学学院,福建福州350002 [3]宁波海关技术中心,浙江宁波315048

出　　处：《分析科学学报》2023年第1期73-80,共8页Journal of Analytical Science

基　　金：福建省科技计划(2020I0032);海关技术规范项目(2020B167)。

摘　　要：建立了QuEChERS-气相色谱-串联质谱(GC-MS/MS)法测定食品的多溴联苯和多溴二苯醚类物质。采用正己烷或乙腈提取并浓缩目标物后,用无水MgSO4、乙二胺-N-丙基硅烷(PSA)和十八烷基硅烷键合硅胶(C18)净化,以DB-5HT色谱柱(15 m×0.25 mm×0.1μm)进行分离,质谱采用电子轰击电离源,在多反应监测模式下进行检测,外标法定量。实验优化了提取条件,比较了提取溶剂的种类和体积、酸的体积对检测结果的影响。结果表明,12种多溴联苯和13种多溴二苯醚共25种目标物均呈现良好线性关系,相关系数(r2)≥0.999,方法的检出限为3~180μg/kg,定量限为10~600μg/kg,平均加标回收率为60.23%~106.97%,相对标准偏差(RSDs,n=6)为0.20%~11.96%。该测定方法操作简单,灵敏度高,适用于食品中多溴联苯和多溴二苯醚类物质的高效分析检出。In this thesis,a QuEChERS-gas chromatography tandem mass spectrometry(GC-MS/MS)method was developed to detect the possible presence of polybrominated biphenyls(PBB)and polybrominated diphenyl ethers(PBDE)in pork,shrimp and citrus foods.After extracting and concentrating the target with n-hexane or acetonitrile,the target was purified with anhydrous magnesium sulfate,primary-secondary amine(PSA)and octadecylsilane bonded silica gel(C18),separated on a DB-5HT chromatographic column with an electron ionization source,detected in multiple reaction monitoring mode,and quantified by external standard method.The method optimized the extraction conditions and determined in detail the effect of the type and volume of extraction solvent and the volume of acid on the assay results.The results showed that 12 PBBs and 13 PBDEs showed good linearity for a total of 25 target species with correlation coefficients(r~2)≥0.999,the detection limit of the method was 3-180μg/kg,the quantification limit of the method was 10-600μg/kg,the average spiked recoveries were 60.23%-106.97%,and the relative standard deviations(n=6)were 0.20%-11.96%.The method is simple and sensitive,and suitable for efficient and accurate detection of PBBs and PBDEs in food.

关 键 词：气相色谱-串联质谱 多溴联苯 多溴二苯醚 

分 类 号：O657.63[理学—分析化学]