高效液相色谱-串联质谱法测定双壳类动物中溴代阻燃剂  

Multi-residue determination method for the determination of brominated flame retardants in bivalves

作　　者：钱卓真[1] 王丽娟[1] 位绍红[1] 许翠娅[1] 汤水粉[1] 

机构地区：[1]福建省水产研究所,福建省海洋生物增养殖与高值化利用重点实验室,福建厦门361013

出　　处：《渔业研究》2017年第6期476-484,共9页Journal of Fisheries Research

基　　金：福建省海洋生物增养殖与高值化利用重点实验室开放课题项目(2015fjscq06);福建省海洋高新产业发展专项项目(闽海洋高新[2014]18号);福建省海洋经济创新发展区域示范项目(闽台重要海洋生物资源高值化开发技术公共服务平台,2014FJPT01);厦门南方海洋研究中心项目(福建重要海洋经济生物种质库与资源高效开发技术公共服务平台,14PZY017NF17)

摘　　要：建立高效液相色谱-串联质谱同时定量检测双壳类动物中六溴环十二烷(HBCD)、四溴双酚A(TBBPA)方法。样品经正己烷和二氯甲烷混合液(1∶1,V/V)提取,浓硫酸除脂,硅胶固相萃取柱净化,Thermo Hypersil Gold C_(18)色谱柱分离,水和甲醇-乙腈梯度洗脱,电喷雾负离子模式下以多反应监测方式检测,内标法定量分析。结果表明,六溴环十二烷(α,β,γ-HBCD)和四溴双酚A在0.5~100 ng/mL范围内线性关系良好(R2>0.995),方法定量限(S/N≥10)为0.05μg/kg。在0.05~0.5μg/kg添加水平内,平均回收率为70.5%~92.4%,日内相对标准偏差(RSD)为3.4%~9.1%,日间RSD为6.3%~10.2%。A multi-residue method based on high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) was developed for the quantitative determination of hexabromocyclododecane(HBCD) and tetrabromobisphenol A(TBBPA) in bivalves.The target analytes were extracted with the mixture of hexane and dichloromethane(1 ∶ 1,V/V).Then the co-extracted lipid was removed by sulfuric acid treatment.The newly obtained extract was cleaned up with silicone solid phase extraction column.The analytes were separated on a Thermo Hypersil Gold C_(18) column by gradient elution with water as mobile phase A and methanol-acetonitrile as mobile phase B,and detected by multiple reaction monitoring(MRM) with electrospray ionization(ESI) under negative ion mode.And the quantitative results were calculated by the internal standard method.The results showed that the calibration curves were linear(R2> 0.995) in the concentration range of 0.5 ~ 100 ng/m L for HBCD and TBBPA.The limits of quantitation for HBCD and TBBPA were 0.05 μg/kg.The average recoveries at three spiked levels ranged from 70.5% to 92.4%.Intra-day and inter-day relative standard deviations(RSDs) were 3.4% ~ 9.1% and 6.3% ~ 10.2%,respectively.

关 键 词：双壳类动物 多残留测定 六溴环十二烷 四溴双酚A 

分 类 号：R155.5[医药卫生—营养与食品卫生学]