分散固相萃取结合稳定同位素内标-气相色谱-串联质谱法快速测定牛奶中7种多溴二苯醚
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(广州市疾病预防控制中心,广东 广州 510440)

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李晓晶 女 副主任技师 研究方向为食品安全与理化检验 E-mail:saiint@163.com

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广州市科技计划项目(201707010196)


Fast determination of polybrominated diphenyl ethers residues in milk by dispersive solid phase extraction and isotope labeled internal standard-gas chromatography-tandem mass spectrometry
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(Guangzhou Center for Disease Control and Prevention, Guangdong Guangzhou 510440, China)

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    摘要:

    目的 建立同时测定牛奶中7种多溴二苯醚(PBDEs)的分散固相萃取结合13C稳定同位素内标-气相色谱-串联质谱(GC-MS/MS)法。方法 样品添加13C12同位素内标后,以1%乙酸乙腈提取,采用新型Z-Sep+C18为吸附剂净化,DB-5色谱柱(30 m×0.25 mm,0.25 μm)分离,选择电子轰击源(EI)多反应监测模式(MRM)气相色谱-串联质谱进行测定,基质匹配标准曲线同位素内标法定量。结果 7种PBDEs在0.500~100 ng/mL范围内均呈良好的线性关系,相关系数r均大于0.999;在0.1、1.0、10 μg/kg 3个加标水平下的平均回收率为89.7%~102.9%,相对标准偏差(n=6)为3.8%~8.3%;检出限和定量下限分别为2.4~9.8和7.5~30 ng/kg。结论 该方法简单、快速、重现性好、灵敏度高,可满足牛奶中7种多溴二苯醚的检测要求。

    Abstract:

    Objective A 13C isotope labeled internal standard-gas chromatography-tandem mass spectrometric (GC-MS/MS) with dispersive solid phase extraction (d-SPE) method was developed for the simultaneous determination of 7 polybrominated diphenyl ethers(PBDEs)residues in milk. Methods After adding13C12 isotope internal standard and extracted with 1% acetic acid acetonitrile,purified with the new Z-Sep+C18 dispersive agent, the analytes in the sample solutions were seperated by DB-5 column(30 m×0.25 mm,0.25 μm). Operated by electron impact ion source (EI) with multiple reactions monitoring (MRM) mode, the samples were analyzed by gas chromatography-tandem mass spectrometer.(GC-MS/MS). The quantifications were performed by the isotope internal standard method with matrix-matched calibration standards. Results Good linearity was obtained for 7 PBDEs in the concentration range of 0.500-100 ng/mL with correlation coefficients (r) above 0.999. Recoveries for 7 PBDEs at three spiked levels of 0.1,1.0, and 10 μg/kg were in the range of 89.7%-102.9% with relative standard deviations (RSDs,n=6) of 3.8%-8.3%. The limits of detection and the limits of quantification were in the ranges of 2.4-9.8 and 7.5-30 ng/kg, respectively.Conclusion The established method was simple, efficient and sensitive, and could be applied in the determination of 7 PBDEs in milk.

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李晓晶,甘平胜,黄聪,于鸿,罗晓燕,潘心红.分散固相萃取结合稳定同位素内标-气相色谱-串联质谱法快速测定牛奶中7种多溴二苯醚[J].中国食品卫生杂志,2020,32(6):641-647, 669.

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  • 收稿日期:2020-09-15
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  • 在线发布日期: 2021-02-18
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