Simultaneous Determination of 61 Veterinary Drug Residues in Animal Derived Food by Clean-up LPAS Combined with LC-MS/MS
Yan Zeng1, Qiaohui Yang1, Xiaxue Li1, Yu Zhang1, Ya Chen1, Jian Yang1, Xin Zhou2*
Abstract
A method of rapid test of 61 veterinary drugs which can divide into 13 types in 5 kinds of animal derived food, namely, pork, pork liver, chicken, egg and beef by Clean-up LPAS combined with LC-MS/MS. The animal derived samples, after preparation, are extracted from 8 ML acetonitrile: water (90:10, with 0.2% of formic acid), and can determine by a mass spectrometer after Clean-up LPAS without stripping. The test is carried out to optimize the LC-MS conditions, extraction reagents, extraction volumes, clean-up ways of the 61 veterinary drugs, etc.; to verify the method performance, including accuracy, precision, limit of detection (LOD), limit of quantitation (LOQ), linear range and matrix effects, and to achieve satisfactory method performance. The results have shown that the 61 veterinary drugs have strong linearity in the range of 0.5~50?g/L with the correlation coefficient (R2) ?0.995, and have obtained satisfactory recovery efficiency in 5 matrix samples under the three high, medium and low addition levels of (5, 10 and 50?g/kg) with the overall recovery rates in the range of 70.9%~119.0% and RSD in the range of 0.1%~10.9%. The overall LOD is in the range of 0.03-1.5 ?g/kg, and the LOQ is in the range of 0.1-5.00 ?g/kg. When the method was applied to test 731 real animal derived samples, a total of 13 types of drugs were detected 64 times; 12 types of restricted drugs were detected 57 times; 2 types of prohibited drugs were detected 7 times, and no other veterinary drug were detected . Thus, it is suggested that the simple Clean-up LPAS is superior to the traditional QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method and can be used for testing batch samples of multiple veterinary drugs in animal derived food.