| 高效液相色谱-串联质谱法测定废水中5种喹诺酮类抗生素 |
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| 引用本文： | 姚倩钰,贺德春,龚道新,丁紫荣,赵波,张漫雯,黎玉清.高效液相色谱-串联质谱法测定废水中5种喹诺酮类抗生素[J].中国环境监测,2017,33(3):139-146. |
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| 作者姓名： | 姚倩钰 贺德春 龚道新 丁紫荣 赵波 张漫雯 黎玉清 |
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| 作者单位： | 湖南农业大学资源环境学院, 湖南 长沙 410000;环境保护部华南环境科学研究所, 广东 广州 510000;原广州军区工程环境质量监督站, 广东 广州 510507,环境保护部华南环境科学研究所, 广东 广州 510000,湖南农业大学资源环境学院, 湖南 长沙 410000,环境保护部华南环境科学研究所, 广东 广州 510000,环境保护部华南环境科学研究所, 广东 广州 510000,环境保护部华南环境科学研究所, 广东 广州 510000,环境保护部华南环境科学研究所, 广东 广州 510000 |
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| 基金项目： | 环保公益性行业科研专项项目（201509038） |
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| 摘 要： | 建立高浓度有机废水中5种喹诺酮类抗生素的高效液相色谱-串联质谱测定方法。水样经HLB固相萃取小柱富集净化,12 ml甲醇洗脱、浓缩并加入内标溶液后,定容至1 mL待测。以C18柱为分离柱,含0.01%甲酸的甲醇-含0.01%甲酸的水溶液为流动相,目标物质在10 min内分离。在0.25~1 250 ng/mL范围内,目标物质线性关系良好(R20.99)。基质加标试验结果表明,纯水中的回收率为61.40%~91.92%,废水中的回收率为54.92%~101.87%,检出限为0.25~2.5 ng/L,方法定量限为0.36~3.99 ng/L。应用该方法对21家猪场的64份废水样品进行分析,5种喹诺酮类抗生素的检出频率为47%~95%,平均检出浓度为980~5 734 ng/L。该方法快速、准确,适用于高浓度有机废水中喹诺酮类抗生素的同时测定。
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| 关 键 词： | 高效液相色谱-串联质谱 固相萃取 废水 喹诺酮类抗生素 |
| 收稿时间： | 2017/1/9 0:00:00 |
| 修稿时间： | 2017/3/6 0:00:00 |
Determination of Five Fluoroquinolone Antibiotics in Wastewater by High Performance Liquid Chromatography-Tandem Mass Spectrometry |
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| YAO Qianyu,HE Dechun,GONG Daoxin,DING Zirong,ZHAO Bo,ZHANG Manwen and LI Yuqing.Determination of Five Fluoroquinolone Antibiotics in Wastewater by High Performance Liquid Chromatography-Tandem Mass Spectrometry[J].Environmental Monitoring in China,2017,33(3):139-146. |
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| Authors: | YAO Qianyu HE Dechun GONG Daoxin DING Zirong ZHAO Bo ZHANG Manwen and LI Yuqing |
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| Institution: | College of Resource and Environment, Hunan Agricultural University, Changsha 410000, China;South China Institute of Environmental Science, MEP, Guangzhou 510000, China;The Constructional and Environmental Quality Supervising Station of Original Guangzhou Military Region, Guangzhou 510507, China,South China Institute of Environmental Science, MEP, Guangzhou 510000, China,College of Resource and Environment, Hunan Agricultural University, Changsha 410000, China,South China Institute of Environmental Science, MEP, Guangzhou 510000, China,South China Institute of Environmental Science, MEP, Guangzhou 510000, China,South China Institute of Environmental Science, MEP, Guangzhou 510000, China and South China Institute of Environmental Science, MEP, Guangzhou 510000, China |
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| Abstract: | A method was established for determination of 5 fluoroquinolone antibiotics in high concentration of organic wastewater using solid phase extraction (SPE) followed by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) in this paper. Aqueous samples were developed with Oasis HLB solid-phase extraction (SPE) cartridges and the targeted antibiotics were subsequently eluted by 12 mL methanol. After concentration, the elutes were added internal standards and determined by HPLC-MS/MS equipped with a reverse-phase C18 column. The results of method development showed that the 5 kinds of fluoroquinolone could be efficiently separated within 10 minutes by HPLC-MSMS; the calibration curve ranged 0.25-1 250 ng/mL and showed high relationship (R2>0.99). The recoveries for all analytes in pure water matrices were above 60%, and the recoveries of target compounds in real wastewater samples ranged 54.92%-101.87%; detection limits varied between 0.25-2.5 ng/L and quantization limits were 0.36-3.99 ng/L. The presented method was successfully applied to quantify the five fluoroquinolones in 64 wastewater samples from 21 pig farms. The detection frequency of five quinolones in real samples was 47%-95% and the average detection concentration was found to be 980 to 5 734 ng/L. All the results indicate that this method is suitable for rapid determination of fluoroquinolone antibiotics in high concentration of organic wastewater. |
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| Keywords: | high performance liquid chromatography-tandem mass spectrometry solid phase extraction wastewater fluoroquinolone antibiotics |
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