Citation: QIU Panzi, GUO Xinyan, WANG Na, KONG Xiangji, HE Hua. Simultaneous determination of ten antibiotics in pharmaceutical wastewater using ultra-high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2015, 33(7): 722-729. doi: 10.3724/SP.J.1123.2015.03039 shu

Simultaneous determination of ten antibiotics in pharmaceutical wastewater using ultra-high performance liquid chromatography-tandem mass spectrometry

QIU Panzi ^1,2 ,
GUO Xinyan ¹ ,
WANG Na ^1,, ,
KONG Xiangji ¹ ,
HE Hua ²

1.
1. Nanjing Institute of Environmental Science, Ministry of Environmental Protection, Nanjing 210042, China;

Corresponding author: WANG Na,
Received Date: 27 March 2015

Fund Project: 环保公益性行业科研专项(201109038,201309031). (201109038,201309031)

A simultaneous analytical method was established for ten selected antibiotics from three categories in pharmaceutical wastewater with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The water samples were enriched and cleaned-up by solid phase extraction cartridges. The types of solid phase extraction cartridges and eluents were optimized by comparing the recoveries of the analytes in water samples under different conditions. The target compounds were separated on an Agilent C18 column (75 mm×2.1 mm, 2.7 μm) with the mobile phases of acetonitrile and 0.2% (v/v) formic acid aqueous solution, and then determined by electrospray ionization mass spectrometry (ESI-MS). The results showed that the calibration curves were linear in the range of 0.1-1000 μg/L (r² > 0.995). The limits of detection (LODs, S/N≥3) and the limits of quantification (LOQs, S/N≥10) of the ten compounds were 0.07-4.37 ng/L and 0.22-14.55 ng/L, respectively. The recovery experiments were performed with samples spiked in the range of 0.002-40 μg/L. The recoveries of the target compounds were in the range of 50.4%-114.1% (RSDs≤9.89%, n=3). Based on this analytical method, the raw and treated sewage samples from a pharmaceutical manufacturer wastewater treatment plant in Jiangsu Province were analyzed. Three compounds were detected in the samples from different sewage treatment units in the range of 0.46-1033.60 μg/L. It shows that the method is accurate, reliable, highly sensitive and can be used to analyze the water samples of pharmaceutical wastewater treatment plant containing aminoglycosides, spiramycin and fluoroquinolones antibiotics.
- ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS),
- antibiotics,
- aminoglycosides,
- spiramycin,
- fluoroquinolones,
- pharmaceutical wastewater
1. [1]
  [1] Sui Q, Huang J, Deng S, et al. Water Res, 2010, 44(2): 417
2. [2]
  [2] Yang C Q, Wang L X, Hou X H, et al. Chinese Journal of Chromatography (杨常青, 王龙星, 侯晓虹, 等. 色谱), 2012, 30(8): 756
3. [3]
  [3] Wang N, Shan Z J, Ge F, et al. The Administration and Technique of Environmental Monitoring (王娜, 单正军, 葛峰, 等. 环境监测管理与技术), 2010, 22(5): 14
4. [4]
  [4] Luo H T, Xie M T, Huang X L, et al. Chinese Journal of Chromatography (罗辉泰, 谢梦婷, 黄晓兰, 等. 色谱), 2015, 33(4): 354
5. [5]
  [5] Du J, Zhao H X, Chen J W. Chinese Journal of Chromatography (杜鹃, 赵洪霞, 陈景文. 色谱), 2015, 33(4): 348
6. [6]
  [6] Luo Y, Xu L, Rysz M, et al. Environ Sci Technol, 2011, 45(5): 1827
7. [7]
  [7] Li B, Zhang T. Environ Sci Technol, 2010, 44(9): 3468
8. [8]
  [8] Cherlet M, De Baere S, De Backer P. J Mass Spectrom, 2007, 42(5): 647
9. [9]
  [9] Hamamoto K, Mizuno Y, Koike R, et al. Shokuhin Eiseigaku Zasshi, 2003, 44(2): 114
10. [10]
  [10] Gbylik M, Posyniak A, Mitrowska K, et al. Food Addit Contam: Part A, 2013, 30(6): 940
11. [11]
  [11] Zhu W X, Yang J Z, Wei W, et al. J Chromatogr A, 2008, 1207(1): 29
12. [12]
  [12] Kaufmann A, Butcher P, Kolbener P. Rapid Commun Mass Spectrom, 2003, 17(22): 2575
13. [13]
  [13] Li J S, Qiu Y M, Wang C. Analysis of Veterinary Drug Residue. Shanghai: Shanghai Scientific and Technical Publishers (李俊锁, 邱月明, 王超. 兽药残留分析. 上海: 上海科学技术出版社), 2002: 340
14. [14]
  [14] Yang Z H, Du G C, Qiao H X, et al. Shanghai Journal of Animal Husbandry and Veterinary Medicine (杨智洪, 杜根成, 乔宏兴, 等. 上海畜牧兽医通讯), 2005(5): 2
15. [15]
  [15] Tang X Y, Zuo J E, Yu X, et al. China Environmental Science (汤薪瑶, 左剑恶, 余忻, 等. 中国环境科学), 2014, 34(9): 2273
16. [16]
  [16] Kaufmann A, Butcher P, Maden K. Anal Chim Acta, 2012, 711: 46
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