| 王帆,杨燕,官悦,陈杨武,谭周亮,邓钦文.市政污水厂污水和污泥中15种典型抗生素同步测定方法优化[J].南华大学学报(自然科学版),2021,(2):25~32.[WANG Fan,YANG Yan,GUAN Yue,CHEN Yangwu,TAN Zhouliang,DENG Qinwen.Simultaneous Determination Method Optimization for 15 Typical Antibiotics in Municipal Wastewater Treatment Plants[J].Journal of University of South China(Science and Technology),2021,(2):25~32.] |
| 市政污水厂污水和污泥中15种典型抗生素同步测定方法优化 |
| Simultaneous Determination Method Optimization for 15 Typical Antibiotics in Municipal Wastewater Treatment Plants |
| 投稿时间：2020-12-11 |
| DOI：10. 19431/ j. cnki. 1673-0062. 2021. 02. 004 |
| 中文关键词: 市政污水厂 抗生素 超高效液相色谱-串联质谱 固相萃取 超声辅助萃取 |
| 英文关键词:municipal wastewater treatment plants antibiotics ultra-high performance liquid chromatography-tandem mass spectrometry solid phase extraction ultrasonic assisted extraction |
| 基金项目:中国科学院科技服务网络计划(STS计划)区域重点项目(KFJ-STS-QYZD-098)；中国博士后科学基金面上项目(2020M673293)；湖南省自然科学基金立项项目(2018JJ2332) |
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| 中文摘要: |
| 采用固相萃取/超声辅助萃取-超高效液相色谱-质谱联用技术,建立了一种适用于市政污水厂污水和污泥中15种典型抗生素的同步测定方法。污水样品经过滤、酸化及固相萃取柱富集净化;污泥样品用体积比为3∶1的McIlvaine缓冲液-乙腈和Mg(NO3)2-NH3·H2O超声提取后经固相萃取柱富集净化。以体积分数为0.1%甲酸水溶液和乙腈为流动相进行梯度洗脱,采用电喷雾离子源,在多反应监测、正离子模式下进行定量分析。结果表明,在优化条件下,15种目标分析物在1~1 000 μg/L范围内线性关系良好(R2均大于0.995),污水和污泥的加标回收率分别为57.02%~156.79%和36.98%~143.76%,相对标准偏差分别为0.18%~10.64%和0.77%~8.31%。该方法成功应用于资阳市某污水处理厂污水和污泥样品的检测,污水和污泥中各有10目标抗生素被检出,浓度分别为9.70 ng/L~551.27 ng/L和15.73 ng/g~2 972.20 ng/g。 |
| 英文摘要: |
| A method was developed for the simultaneous determination of 15 typical antibiotics in the wastewater and sludge from wastewater treatment plants,using ultrasonic-assisted extraction followed by solid phase extraction and ultra-high performance liquid chromatography-tandem mass spectrometry.The wastewater samples were enriched and cleaned-up by filtration, acidification and solid phase extraction cartridges.The sludge samples were firstly extracted by ultrasonic-assisted extraction with a mixture of McIlvaine buffer-Acetonitrile and Mg(NO3)2-NH3·H2O with a volume ratio of 3∶1, and then followed by SPE process.All antibiotics were separated by gradient elution with the mobile phase of 0.1% formic acid aqueous solution and acetonitrile, and then quantitatively analyzed with an electrospray ionization source in the positive ion and multiple reaction monitoring modes. After Optimization, the 15 antibiotics achieved great linearity in the range of 1~1 000 μg/L (R2>0.995), and the average recoveries of wastewater and sludge were 57.02%~156.79% and 36.98%~143.76%, respectively, and the relative standard deviations were 0.18%~10.64% and 0.77%~8.31%, respectively. This method has been successfully applied in determining samples of the wastewater and sludge from a municipal wastewater treatment plant in Ziyang.Ten target antibiotics were identified in the wastewater and sludge, with the concentration ranges of 9.70 ng/L~551.27 ng/L and 15.73 ng/g~2 972.20 ng/g in wastewater and sludge samples, respectively. |
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