摘要
建立了大气压气相色谱-串联质谱(APGC-MS/MS)同时测定人体血清8种多溴二苯醚(PBDEs)和9种新型溴代阻燃剂(NBFRs)的方法。0.3 g血清样品经HLB柱固相萃取和30%酸性硅胶柱净化处理后,用DB-5HT毛细管柱(15 m×0.25 mm×0.10μm)分离,APGC-MS/MS检测分析。PBDEs和NBFRs的检测分别采用同位素稀释法和内标法。采用血清标准参考物质SRM 1958和基质加标进行方法验证,与SRM 1958给出的参考质量分数值范围对比,多溴二苯醚各化合物浓度的测定值均在参考质量分数值的范围内,相对标准偏差(RSD,n=6)为6.1%~18%。NBFRs的基质加标回收率为81.7%~126%,RSD为6.2%~18%。该方法灵敏度和准确度高、方法性能稳定,满足人体血清中溴代阻燃剂检测的要求。
An atmospheric pressure gas chromatography-tandem mass spectrometry(APGC-MS/MS)method was established to simultaneously determine 8 types of polybrominated diphenyl ethers(PB⁃DEs)and 9 types of novel brominated flame retardants(NBFRs).Serum sample of 0.3 g was pretreated with HLB column solid-phase extraction and acidic silica gel column purification,and sep⁃arated by DB-5HT capillary column(15 m×0.25 mm×0.10μm).PBDEs and NBFRs was quantita⁃tively analyzed by APGC-MS/MS.The detection of PBDEs is using isotope dilution method,and the detection of NBFRs is using the internal standard method.This method was further validated using in⁃ternational serum standard reference material sample SRM 1958.Compared with the reference mass fraction range provided by SRM 1958,the measured concentrations of PBDEs were within the refer⁃ence mass fraction range,with a relative standard deviation(RSD,n=6)of 6.1%to 18%.The low,medium,and high concentrations of NBFRs were added to the matrix for validation.The recoveries of matrix spiking ranged from 81.7%to 126%.The RSDs were between 6.2%and 18%.This method has high sensitivity and accuracy,stable performance,which meets the requirements for the deter⁃mination of PBDEs and NBFRs in human serum and the method can be applied to human health risk assessment for PBDEs and NBFRs.
作者
蒋友胜
朱路
彭金铃
宋嘉宜
刘源
林晓仕
孔令权
卓兰
张建清
JIANG You-sheng;ZHU Lu;PENG Jin-ling;SONG Jia-yi;LIU Yuan;LIN Xiao-shi;KONG Ling-quan;ZHUO Lan;ZHANG Jian-qing(Shenzhen Center for Disease Control and Prevention,Shenzhen 518055,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2024年第8期1273-1279,共7页
Journal of Instrumental Analysis
基金
深圳市科技计划项目(JCYJ20210324141207018,JCYJ20210324135000001)。
关键词
多溴二苯醚
新型溴代阻燃剂
血清
大气压气相色谱-串联质谱
polybrominated diphenyl ethers
novel brominated flame retardants
serum
atmo⁃spheric pressure gas chromatography-tandem mass spectrometry
