Citation: WANG Li, ZHONG Donglian, CHEN Guangcai, TANG Fubin, SONG Qiuhua, ZHANG Jianfeng. Determination of antibiotic residues in manure by liquid chromatography-tandem mass spectrometry coupled with solid phase extraction[J]. Chinese Journal of Chromatography, ;2013, 31(10): 1010-1015. doi: 10.3724/SP.J.1123.2013.03048 shu

Determination of antibiotic residues in manure by liquid chromatography-tandem mass spectrometry coupled with solid phase extraction

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1. Research Institute of Subtropical Forestry, Chinese Academy of Forestry, Fuyang 311400, China;

Corresponding author: CHEN Guangcai,
Received Date: 27 March 2013
Available Online: 14 May 2013
Fund Project: 浙江省公益技术项目(2010C33188). (2010C33188)

A method was developed for the simultaneous determination of tetracyclines (TCs), quinolones (QUs) and sulfadimidine (SM2) in pig manure and chicken dung by a combined high performance liquid chromatography (HPLC) and tandem mass spectrometry (MS/MS) detection coupled with solid phase extraction. The residual antibiotics in manure were extracted with the mixture of methanol, acetic acid and water with the volume ratio of 6:3:1, enriched and purified by a hydrophilic lipophilic balance (HLB) solid-phase extraction cartridge. The C₁₈ chromatographic column was used to complete the separation of the analytes which were detected in multiple reaction monitoring (MRM) mode via positive electrospray ionization (ESI⁺). The external standard calibration curves were used for the quantification. All the antibiotics were determined with an excellent linear relationship from 50 to 1000 μg/L for TCs and QUs, and from 5 to 100 μg/L for SM2. The limits of detection for TCs, QUs and SM2 were 0.25-7.18, 0.15-3.16 and 0.04 μg/kg, respectively. The recoveries of TCs, QUs and SM2 in pig manure and chicken dung were 40%-124% at the spiked levels from 0.1 to 10 μg/g (RSDs ranged from 3.0% to 9.5%, n=6). The method was successfully applied to determine the antibiotics in pig manure and chicken dung samples. The method has high accuracy and sensitivity for the determination of TCs, QUs and SM2 in pig manure and chicken dung.
- solid phase extraction (SPE),
- high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS),
- antibiotics,
- pig manure,
- chicken dung
1. [1]
  [1] Li Z J, Yao Z P, Zhang J, et al. Asian Journal of Ecotoxicology (李兆君, 姚志鹏, 张杰, 等. 生态毒理学报), 2008, 3(1): 15
2. [2]
  [2] Sarmah A K, Meyer M T, Boxall A B A. Chemosphere, 2006, 65(5): 725
3. [3]
  [3] Carballo E M, Gonzalez-Barreiro C, Scharf S, et al. Environ Pollut, 2007, 148(2): 570
4. [4]
  [4] Martinez J L. Environ Pollut, 2009, 157(11): 2893
5. [5]
  [5] Arikan O A, Mulbry W, Rice C. J Hazard Mater, 2009, 164(2): 483
6. [6]
  [6] Zhu S C, Wang J, Shao W W, et al. Chinese Journal of Chromatography (朱赛嫦, 王静, 邵卫伟, 等. 色谱), 2013, 31(1): 15
7. [7]
  [7] Arikan O A, Rice C, Codling E. Desalination, 2008, 226(1): 121
8. [8]
  [8] Liu Y C, Xu W H, Yu L L, et al. Journal of Instrumental Analysis (刘玉春, 徐维海, 余莉莉, 等. 分析测试学报), 2006, 25(2): 1
9. [9]
  [9] Zhang J, Yan L J, Pan C S, et al. Chinese Journal of Chromatography (张洁, 严丽娟, 潘晨松, 等. 色谱), 2012, 30(10): 1031
10. [10]
  [10] Wang Z J, Leng K L, Sun W H, et al. Chinese Journal of Chromatography (王志杰, 冷凯良, 孙伟红, 等. 色谱), 2009, 27(2): 138
11. [11]
  [11] Blackwell P A, Lützhft H C H, Ma H P, et al. Talanta, 2004, 64: 1058
12. [12]
  [12] Shen Y, Wei Y S, Guo R, et al. Environmental Chemistry (沈颖, 魏源送, 郭睿, 等. 环境化学), 2009, 28(5): 747
13. [13]
  [13] Hu X G, Luo Y, Zhou Q X, et al. Chinese Journal Analytical Chemistry (胡献刚, 罗义, 周启星, 等. 分析化学), 2008, 36(9): 1162
14. [14]
  [14] Li Y X, Li W, Zhang X L, et al. Chinese Journal Analytical Chemistry (李艳霞, 李帷, 张雪莲, 等. 分析化学), 2012, 40(2): 213
15. [15]
  [15] Guo B, Yao L X, He Z H, et al. Environmental Chemistry (国彬, 姚丽贤, 何兆桓, 等. 环境化学), 2011, 30(12): 2054
16. [16]
  [16] Zhao L J, Xu S K, Zhang B X. China Journal of Chinese Materia Medica (赵陆军, 徐思康, 张保献. 中国中医药信息杂志), 2000, 7(11): 47
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沈阳化工大学材料科学与工程学院沈阳 110142