高效液相色谱法快速筛查环境水体中16种氟喹诺酮类抗生素及质谱确证

李玉静, 陈志冉, 王雪平

现代化工 ›› 2018, Vol. 38 ›› Issue (9) : 237 -241.

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现代化工 ›› 2018, Vol. 38 ›› Issue (9) : 237-241. DOI: 10.16606/j.cnki.issn0253-4320.2018.09.054
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高效液相色谱法快速筛查环境水体中16种氟喹诺酮类抗生素及质谱确证

    李玉静, 陈志冉, 王雪平
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Rapid determination of 16 fluoroquinolones in environmental water by high performance liquid chromatography and their verification by mass spectrometry

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摘要

利用HLB固相萃取柱对环境水体中16种氟喹诺酮类抗生素(FQs)进行富集、净化,经可变波长扫描紫外检测器测定,建立了高效液相色谱法快速筛查环境水体中残留FQs种类及其残留量;对于疑似FQs残留阳性水样,采用液相色谱-串联质谱法进行进一步确证。结果表明,16种FQs在5.0~100.0 μg/mL范围内,FQs质量浓度与其峰面积具有良好的线性关系,相关系数为0.998 9~0.999 9,检出限为0.9~7.3 μg/mL,定量限为3.0~24.3 μg/mL,平均回收率为89.3%~98.6%,相对标准偏差为0.9%~3.1%。

Abstract

HLB solid-phase extraction column is used to enrich and purify 16 kinds of fluoroquinolones (FQs) in environmental waters.After detection by a variable wavelength scanning ultraviolet detector, the method for determination of remindering FQs in environmental water by high performance liquid chromatography are established.Suspected FQs residual positive water samples are confirmed by liquid chromatography-mass spectrometry.It is found that in the range of 5.0-100.0 μg/mL, the concentrations of 16 kinds of FQs all have a good linear relationship with their peak areas, with correlation coefficient ranging from 0.998 9 to 0.999 9, detection limit ranging from 0.9 μg/mL to 7.3 μg/mL, quantitation limit ranging from 3.0 μg/mL to 24.3 μg/mL, average recoveries ranging from 89.3% to 98.6% and the relative standard deviations ranging from 0.9% to 3.1%.

关键词

氟喹诺酮类抗生素 / 环境水体 / 质谱确证 / 高效液相色谱

Key words

fluoroquinolones / environmental water / mass spectrometric verification / high performance liquid chromatography

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高效液相色谱法快速筛查环境水体中16种氟喹诺酮类抗生素及质谱确证[J]. 现代化工, 2018, 38(9): 237-241 DOI:10.16606/j.cnki.issn0253-4320.2018.09.054

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