聚合物整体柱微萃取-液相色谱-串联质谱法测定工业废水中6种喹诺酮药物残留量

陈志冉, 崔鹏

现代化工 ›› 2018, Vol. 38 ›› Issue (5) : 228 -232.

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现代化工 ›› 2018, Vol. 38 ›› Issue (5) : 228-232. DOI: 10.16606/j.cnki.issn0253-4320.2018.05.052
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聚合物整体柱微萃取-液相色谱-串联质谱法测定工业废水中6种喹诺酮药物残留量

    陈志冉, 崔鹏
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Determination of six quinolones residues in industrial wastewater by polymer monolithic column microextraction-liquid chromatography-tandem mass spectrometry

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摘要

以甲基丙烯酸丁酯为功能单体,二甲基丙烯酸乙二醇酯为交联剂,正丙醇和聚乙二醇400为致孔剂,偶氮二异丁腈为引发剂,在不锈钢管模具中制备聚合物整体柱(BMA-co-EDMA);以BMA-co-EDMA柱为萃取介质,利用聚合物整体柱微萃取技术,结合液相色谱-串联质谱法(LC-MS),建立了同时测定工业废水中6种喹诺酮药物残留量的分析方法。结果表明,在0.2~100.0 ng/mL质量浓度范围内,各目标物定量离子峰面积与其质量浓度呈现良好线性关系,相关系数在0.999 6~0.999 9之间,检出限在0.07~0.35 ng/L,定量限在0.2~1.0 ng/L,回收率在92.3%~98.6%,相对标准偏差在0.7%~3.7%。与其他方法相比,BMA-co-EDMA柱稳定性和重现性良好,可反复使用10次以上。

Abstract

A polymer monolithic column is prepared in a stainless steel tube mold with butyl methacrylate as functional monomer,ethylene glycol dimethacrylate as crosslinking agent,n-propanol and polyethylene glycol 400 as porogen,and azo-bis-isobutyronitrile as initiator.The method to determine simultaneously 6 kinds of quinolones residues in industrial waste is developed by polymer monolithic microextraction combining with LC-MS through using BMA-co-EDMA column as extractive medium.The results show that the peak area of quantitation ion of each target substance shows a good linear relationship with its concentration in the range of 0.2-100.0 ng·mL-1,with correlation coefficient ranging from 0.999 6 to 0.999 9.The detection limits range from 0.07 ng·L-1 to 0.35 ng·L-1.The quantitation limits range from ng·L-1 to 1.0 ng·L-1.The recovery rates range from 92.3% to 98.6%,and the relative standard deviations range from 0.7% to 3.7%.Compared with other methods,BMA-co-EDMA column has good stability and reproducibility,which can be used repeatedly more than 10 times.

关键词

聚合物整体柱 / 喹诺酮 / 工业废水 / LC-MS / 固相微萃取

Key words

polymer monolithic column / quinolone / industrial waste / LC-MS / solid-phase microextraction

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聚合物整体柱微萃取-液相色谱-串联质谱法测定工业废水中6种喹诺酮药物残留量[J]. 现代化工, 2018, 38(5): 228-232 DOI:10.16606/j.cnki.issn0253-4320.2018.05.052

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