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摘要
利用加速溶剂萃取法(ASE)萃取污泥中合成麝香(SMs),石墨化炭黑和佛罗里硅藻土在线净化,经HP-5MS毛细管柱分离,建立了气相色谱-串联质谱法(GC-MS/MS)同时测定污泥中12种SMs残留量的分析方法。结果表明,12种SMs在0.01~1.0 μg/mL质量浓度范围内呈良好线性关系,相关系数(r2)为0.999 6~0.999 9;该方法检出限为1.5~3.0 μg/kg,定量限为5.0~10.0 μg/kg,回收率为91.5%~98.8%,相对标准偏差为0.9%~2.8%。老化效应、基质效应对ASE萃取污泥中12种SMs的影响较小。该方法具有检出限低、回收率高、精密度好等特点。
Abstract
Synthetic musk (SM) in sludge is extracted by accelerated solvent extraction (ASE),purified on-line by graphitized carbon black and Florian diatomite,and separated by HP-5MS capillary column.A method for the simultaneous determination of 12 kinds of SM residues in sludge by gas chromatography tandem mass spectrometry (GC-MS/MS) is developed.The results show that 12 kinds of SM show a good linear relationship in the concentration range of 0.01-1.0 μg·mL-1,with correlation coefficient ranging from 0.999 6 to 0.999 9.The detection limits range from 1.5 μg·kg-1 to 3.0 μg·kg-1 and the quantization limits range from 5.0 μg·kg-1 to 10.0 μg·kg-1.The recovery rates range from 91.5% to 98.8% and the relative standard deviations range from 0.9% to 2.8%.Aging effect and matrix effect have little impact on extraction of 12 kinds of SM in sludge by ASE.This method features with low detection limit,high recovery rate and good precision.
关键词
污泥
/
麝香
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合成
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气相色谱-串联质谱法
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加速溶剂萃取
Key words
sludge
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musk
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synthetic
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gas chromatography-tandem mass spectrometry
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accelerated solvent extraction
ASE萃取-GC-MS/MS法同时测定污泥中12种合成麝香[J].
现代化工, 2019, 39(10): 220-225,229 DOI:10.16606/j.cnki.issn0253-4320.2019.10.049