固相萃取净化-气相色谱法测定食用菌及其栽培基质中26种多溴联苯醚  

Dermination of polybrominated diphenyl ethers in mushrooms and substrates by SPE-GC-ECD

作　　者：张其才[1] 饶钦雄[1] 王献礼 汤倩倩[2] 陈珊珊[1] 刘星 宋玮[1] 关舒会 程琳 宋卫国[1] ZHANG Qicai;RAO Qinxiong;WANG Xianli;TANG Qianqian;CHEN Shanshan;LIU Xing;SONGWei;GUAN Shuhui;CHENG Lin;SONG Weiguo(Institute of Agro-food Standard and Testing Technolo‐gy,Shanghai Academy of Agricultural Sciences/Shanghai Engineering Research Center of Agro-food Quality and Safety,Shanghai 201403,China;Shanghai Agricultural Technology Promotion Center,Shanghai 201103,China)

机构地区：[1]上海市农业科学院农产品质量标准与检测技术研究所,上海市农产品质量安全评价技术服务平台,上海农产品质量安全工程技术研究中心,上海201403 [2]上海市农业技术推广服务中心,上海201103

出　　处：《分析试验室》2022年第5期558-563,共6页Chinese Journal of Analysis Laboratory

基　　金：上海市科技兴农攻关项目[沪农科产字(2017)第9号]资助。

摘　　要：建立了食用菌及其栽培基质中26种多溴联苯醚(PBDEs)的检测方法。考察了不同提取溶剂,不同净化材料,不同仪器条件对检测结果的影响,确立了乙腈提取,盐析分层,乙二胺-N-丙基硅烷(PSA)复合去活化硅胶固相萃取柱净化,气相色谱-电子捕获器(GC-ECD)分析,外标法定量的检测方法。方法的线性相关系数大于0.996,检出限为0.02~0.06µg/kg,定量限为0.06~0.2µg/kg,方法加标回收率在72.5%~119.2%之间,相对标准偏差在2.2%~14%之间。A novel method for the determination of 26 kinds of polybrominated diphenyl ethers(PBDEs)in mushrooms and substrates was established. The preparation parameters were investigated,including extraction solvents,solid-phase extraction(SPE) materials and instrument conditions. Samples were extracted with acetonitrile,salted out by NaCl,and cleaned up with SPE consisting of primary secondary amine(PSA)and deactivated silica gel. And the samples were detected by gas chromatography with electron capture detection(GCECD). With the proposed method,the calibration curves had good linearities with the correlation coefficients(R^(2))more than 0.996. The method detection limits of PBDEs were 0.02-0.06 μg/kg,and the method quantitation limits of PBDEs were 0.06-0.2 μg/kg,respectively. The average recoveries in mushroom and substrates ranged from 72.5% to 119.2%,and the relative standard deviations(RSDs)ranged from 2.2% to 14%.

关 键 词：多溴联苯醚 食用菌 栽培基质 固相萃取 气相色谱 

分 类 号：X56[环境科学与工程—环境工程]