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| Rapid Determination of 12 Diuretic Residues in Pork by Modified QuEChERS Combined with Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry |
| ZHAN Hao, XUAN Lei, KONG Weiheng, LIU Wen, CHEN Ranran, MENG Xiaodi, ZHOU Xiaoying, Lü Yaning, HAN Fang, YU Xiaofeng |
| 1. Anhui Provincial Key Laboratory of Food Safety Monitoring and Quality Control, Hefei Customs Technology Center, Hefei 230022, China; 2. Key Laboratory of Sports Training Monitoring and Evaluation, General Administration of Sport of China, Anhui Provincial Institute of Sports Science and Technology, Hefei 230011, China; 3. China Customs Science and Technology Research Center, Beijing 100026, China |
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Abstract A method for the simultaneous determination of 12 diuretic residues in pork was developed using a modified QuEChERS approach and ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). After homogenization, the sample was extracted with acetonitrile and cleaned up with MgSO4, C18 and primary secondary amine. Separation was performed on an Eclipse Plus C18 column (100 mm × 2.1 mm, 1.8 μm) using a mobile phase consisting of 3 mmol/L ammonium formate-0.1% formic acid in water and acetonitrile. Detection was carried out using UPLC-MS/MS in the multiple reaction monitoring (MRM) mode. All analytes exhibited good linearity over the concentration range evaluated with correlation coefficients (R2) > 0.99. The limits of quantitation (LOQ) were 2–5 μg/kg. The average recoveries at three spiked levels of LOQ, 2 LOQ and 10 LOQ ranged from 85.8% to 112.0%, with relative standard deviations (RSDs) of 0.5%–5.1%. The proposed method is a simple yet efficient, sensitive and selective approach for the rapid detection of the 12 diuretics in pork.
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