| 摘要: |
| 建立了一种测定鱼肉中六溴环十二烷（HBCD）的QuEChERS-超高效液相色谱-串联质谱方法。方法采用QuEChERS法进行样品前处理，采用C18色谱柱分离，以水为流动相A，以甲醇-乙腈（V∶V=50∶50）为流动相B进行梯度洗脱；采用超高效液相色谱-串联质谱法在负离子模式下以多反应监测方式检测，用同位素稀释法定量。该方法在 0.5~50μg/L范围内具有良好的线性关系（相关系数≥0.999），检出限为0.05~0.27 μg/kg，3个加标质量分数（2.5，125，25 μg/kg）的回收率范围为99.3%~107%，相对标准偏差为0.4%~8.4%。该方法简便准确、灵敏度高，可满足鱼肉中HBCD的检测要求。 |
| 关键词: 超高效液相色谱-质谱法 QuEChERS 六溴环十二烷 鱼肉 |
| DOI： |
| 分类号:X835 |
| 基金项目:江苏省重点研发计划-社会发展基金资助项目（BE2021740）；江苏省卫生健康委面上基金资助项目（M2021028） |
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| Determination of Hexabromocyclododecane in Fish by QuEChERS Extraction Ultra High Performance Liquid Chromatography Tandem Mass Spectrometry |
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SHEN Fei, ZHU Feng, JI Wen-liang
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Jiangsu Provincial Center for Disease Control and Prevention, Nanjing, Jiangsu 210009, China
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| Abstract: |
| A quick, easy, cheap, effective, rugged and safe(QuEChERS) method coupled with ultra performance liquid chromatography tandem mass spectrometry (UPLC MS/MS) was established for the determination of hexabromocyclododecane (HBCD) in fish. QuEChERS method was used for sample pretreatment. The chromatographic separation was performed on a C18 column by gradient elution with water (mobile phase A) and methanol acetonitrile solution (mobile phase B, volume ratio =50∶50) as mobile phase. UPLC MS/MS method was used for MS/MS analysis with electrospray ion source in negative mode under multiple reaction monitoring mode, and isotope dilution internal standard method was used for quantification. The method had a good linear relationship in the concentration range of 0.5~50 μg/L (r≥0.999). The limits of detection (LOD) were in the range of 005~0.27μg/kg. The recovery rates of the three concentrations (2.5, 12.5, 25 μg/kg) were in the range of 99.3%~107%. The relative standard deviations were 0.4%~8.4%. The method is simple, accurate and sensitive, and can meet the detection requirements of HBCD in fish. |
| Key words: Ultra performance liquid chromatography tandem mass spectrometry QuEChERS Hexabromocyclododecane Fish |
