NCI\|GCMS法测定运动场地面层合成材料中短链氯化石蜡(C10—C13)含量
Quantification of short-chain chlorinated paraffins in plastic track by negative ion chemical ionization(NCI) combined with gas chromatography-mass spectrometry
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摘要: 本文建立了气相色谱质谱法负化学离子化方式检测运动场地面层合成材料中短链氯化石蜡（SCCPs）（C10-13Cl5-10）的定量方法.样品经正己烷超声萃取60 min，提取液使用浓硫酸净化后，使用GCMS对SCCPs的24组同类物进行分离和检测.在5.0 mg·L-1浓度下，连续6次进样，SCCPs的24组同系物峰面积RSD%值均小于10.0%.以3倍信噪比计算检测限，24组同类物检测限分布在0.049-2.53 mg·L-1之间.加标回收实验中，加标浓度为25 mg·kg-1和100 mg·kg-1，SCCPs平均加标回收率为122.2%和107.5%.实验结果证明，此方法能够较为准确测定运动场地面层合成材料中短链氯化石蜡的含量.Abstract: In this paper, a quantitative method for the determination of short chain chlorinated paraffins (C10-13Cl5-10) in the synthetic materials of athletic ground surface layer by negative ion chemical ionization combined with gas chromatography-mass spectrometry was established. The samples were extracted with n-hexane for 60 min, and the extracted solution was purified with 98% sulfuric acid. 24 homologues of short chain chlorinated paraffins(SCCPs) in the extracted solution were separated and analyzed by GCMS. The RSD% of the peak area of 24 homologues of SCCPs was less than 10.0% when the concentration of SCCPs standard solution was 5.0 mg·L-1 for six times of repeated injection. The detection limit of 24 groups of homologues was 0.049 -2.53 mg·L-1, when it was calculated based on three times of signal-to-noise ratio (peak to peak). In the standard addition recovery experiment, when the standard addition concentration is 25 mg·kg-1, the average recovery rate is 122.2%, and when the standard addition concentration is 100 mg·kg-1, the average recovery rate is 107.5%. The experimental results show that the method can accurately determine the content of SCCPs in the synthetic materials of sports ground.
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Key words:
- short chain chlorinated paraffins /
- GCMS /
- NCI
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[1] 王亚韡, 傅建捷, 江桂斌. 短链氯化石蜡及其环境污染现状与毒性效应研究[J].环境化学,2009,28(1):1-9. WANG Y W, FU J J, JIANG G B. The research of environmental pollutions and toxic effect of short chain chlorinated paraffins[J]. Environmental Chemistry,2009,28(1):1-9(in Chinese).
[2] TOMY G T, FISK A T, WESTMORE J B,et al, Environmental chemistry and toxicology of polychlorinated n-alkanes//WARE G W. Reviews of Environmental Contamination and Toxicology[M]. New York:Springer,1998:53-128. [3] GB 36246-2018《中小学合成材料面层运动场地》附录G短链氯化石蜡(C10-C13)含量的测试气相色谱-电子捕获负化学电离源质谱法[S].27-30 GB 36246-2018 Sports areas with synthetic surfaces for primary and middle schools Appendix G:Determination of short chain chlorinated paraffins (C10-C13) by gas chromatography-negative ion chemical ionization mass spectrometry[S].27-30(in Chinese). -
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