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
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.
2025, Vol. 39 
