Citation: SUN Xiao-Liang, LI Xue-Lian, CAO Xu-Min, YANG Yan-Fei, WANG Juan, WANG Shu-Ting, WANG Yu-Dong, WANG Xiao-Yin, QU Zhi-Na, ZHAO Si-Jun. An Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometric Method for Fast Determination of 30 Different Species of Lean Meat Agents Residues in Pig Urine[J]. Chinese Journal of Analytical Chemistry, ;2017, 45(1): 124-132. doi: 10.11895/j.issn.0253-3820.160530 shu

An Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometric Method for Fast Determination of 30 Different Species of Lean Meat Agents Residues in Pig Urine

SUN Xiao-Liang ^1,2, ,
LI Xue-Lian ³ ,
CAO Xu-Min ^1,2 ,
YANG Yan-Fei ^1,4 ,
WANG Juan ^1,2 ,
WANG Shu-Ting ^1,2 ,
WANG Yu-Dong ^1,2 ,
WANG Xiao-Yin ^1,2 ,
QU Zhi-Na ^1,2 ,
ZHAO Si-Jun ^1,2

1.
China Animal Health and Epidemiology Center, Qingdao 266032, China;
2.
Livestock and Poultry Products Quality and Safety Risk Assessment Laboratory, Ministry of Agriculture(Qingdao), Qingdao 266032, China;
3.
Qingdao Yebio Biological Engineering Co., Ltd., Qingdao 266032, China;
4.
College of Animal Science and Technology, Anhui Agriculture University, Hefei 230000, China

Received Date: 12 July 2016
Revised Date: 20 October 2016

An ultra-high performance liquid chromatography-tandem mass spectrometric (UPLC-MS/MS) method for simultaneous determination of thirty different species of ‘lean meat agents’ (including clonidine, cyproheptadine, and other 28 β-agonists) residues in swine urine was developed. The parameters of separation conditions of liquid chromatography, MS/MS detection parameters and sample preparation procedure were optimized. After centrifuged at 5000 r/min for 5 min, the swine urine samples were performed directly by MCX column. Then the column was washed with 3 mL of water and 3 mL of methanol, respectively, and then the compounds were eluted with 5% ammonium hydroxide in methanol. The analytes were detected by UPLC-MS/MS after the elution was evaporated to dryness at 45℃ under a stream of nitrogen gas. Under the optimum conditions, thirty of analytes could be well separated in less than 5 min. The linear ranges were 0.1-10 μg/L for all analytes with the correlation coefficient (r²) higher than 0.992. Limits of detection (LOD) and limits of quantification (LOQ) of this method were less than 0.1 μg/L and 0.3 μg/L, respectively. The mean recoveries of three spiked concentration levels in blank sample varied from 67.6% to 103.2% with the intra-and inter-relative standard deviations of 2.8% to 16.8% and 2.6% to 15.8%, respectively. Overall, the proposed method is simple, quick, reliable, sensitivity, and can be applied in large scale supervision of illegal usage of 30 kinds of ‘lean meat agents’.
- Ultra-high performance liquid chromatography-tandem mass spectrometry,
- Trace residues,
- Swine urine,
- Lean meat agents
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