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高效液相色谱串联质谱法分析土壤中多溴联苯醚类化合物
Determination of Polybrominated Diphenyl Ethers in Soil with Liquid Chromatography Tandem Mass Spectrometry
投稿时间:2018-07-20  修订日期:2018-12-03
DOI:10.19316/j.issn.1002-6002.2019.06.16
中文关键词:  多溴联苯醚  土壤  液相色谱质谱
英文关键词:Polybrominated Diphenyl Ethers(PBDEs)  soil  Liquid Chromatography Tandem Mass Spectrometry(LC-MS/MS)
基金项目:
作者单位
牛禾 台州市环境监测中心站,浙江台州318000 
余彬彬 台州市环境监测中心站,浙江台州318000
台州学院医药化工与材料工程学院,浙江台州318000 
饶钦全 台州市环境监测中心站,浙江台州318000 
王晖 台州市环境监测中心站,浙江台州318000 
丁苗 台州市环境监测中心站,浙江台州318000 
徐方曦 台州市环境监测中心站,浙江台州318000 
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中文摘要:
      建立了一种超高效液相色谱串联质谱法(UPLC-MS/MS)同时测定土壤中8种多溴联苯醚化合物(PBDEs)的方法,采用快速溶剂萃取(ASE)和凝胶净化色谱(GPC),经BEH反相C18色谱柱分离,10 min内完成分离,使用含0.1%氨水的甲醇和水进行梯度洗脱,采用液相色谱-负离子-大气压化学电离(APCI)串联质谱,多反应监测模式(MRM),加入 13C12-BDE-139和13C12-BDE-209内标作定量分析。结果表明:在优化的分析条件下,PBDEs的线性相关系数为0.998 8~0.999 5,方法检出限为0.22~0.59 μg/kg,在2个添加水平下,平均回收率为71%~126%,标准偏差为3%~18%,土壤实际质控样测定结果均在允许范围内。适合于土壤中PBDEs的快速分析,特别对于高溴代PBDEs,相比气相色谱质谱方法具有更快的分析速度和更好的稳定性。
英文摘要:
      An Ultra Performance Liquid Chromatography Tandem Mass Spectrometry (UPLC-MS/MS) method was developed for the simultaneous determination of eight polybrominated diphenyl ethers (PBDEs) in soil samples. The sample was extracted by accelerated solvent extraction (ASE) and cleaned by gel permeation chromatographic technique (GPC). The separation of PBDEs were performed on a C18 column using gradient elution of alkaline methanol and water, then analyzed under the multiple reaction monitoring (MRM) mode with negative-ion atmospheric pressure chemical ionization (APCI).13C12-BDE-139 and 13C12-BDE-209 were added as internal standard for quantitative determination. Under the optimal conditions, the calibration curves of PBDEs were linear well with correlation coefficients ranging from 0.998 8 to 0.999 5, and the detection limits of PBDEs appeared within the range of 0.22-0.59 μg/kg. At the two spiked levels, the average spiked recoveries were between 71% and 126%, with the relative standard derivations (RSDs) from 3% to 18%. The method was applied to determination of PBDEs in standard reference material (SQC-072), and favorable results were obtained. The developed method is accurate and sensitive for determination of 8 kinds of PBDEs in soils. Compared with the gas chromatography method, this method provides faster analysis ability and better stability, especially for higher brominated PBDEs.
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