Several Biochemical Drugs In Veterinary Drug Residue Of Uplc/ms/ms Method

UPLC-MS/MS technology has the unique capabilities of multi-component analysis and the advantages of rapid analysis, which is very useful in detecting residues in food of animal origin. Biochemical drug is the drug extracted from the animals. The quality and safety of biochemical drug depends in part on its animal origin. Due to irrational drug use, illegal drug use is a very serious problem. Residues of veterinary drugs and additives in food of animal origin in China are very serious. The safety of foods of animal origin are had widespread attention and come up with a lot of testing methods. Relative to food safety, drug safety is more important and deserves the more attention in detecting veterinary drug residues of biochemical drugs of animal origin. The main work of this paper is used ultra-high performance liquid and triple quadrupole mass spectrometry technology to have qualitative and quantitative analysis of veterinary drug residues in two biochemical drugs.The dissertation consists of two main parts:1. By optimizing (the conditions of chromatography and mass spectrometry) and comparing (different methods of sample preparation). To establish a method for determination of four metabolites of nitrofuran antibiotics in heparin by UPLC-MS/MS. This analytical method had high sensitivity and passed the method verification. Chromatographic condition was using a Waters ACQUITY UPLC(?) BEH C18column (2.1mm×100mm,1.7μm), and the column temperature was30℃; The mobile phase was2mmol/L Ammonium acetate and Methanol at a flow rate of0.2ml-min-1; Samples were hydrolyzed with0.125mol/LHCl, and derivatized at37℃for16h with2-nitrobenzaldenhyde.The target compounds were eluted with ethyl acetate from the derivatized solutions, MS detection was performed in the positive ion mode using multiple reaction monitoring (MRM). The quantification was obtained ultilizing the homologous internal standards.The Heparin Sodium、Heparin Calcium Injection and three kinds of low molecular heparins had been quantified with the above analytical method.2. Developed a new method for determination of nine B-agonists in medical gelatin hard capsule shells by UPLC-MS/MS. Homogenized in buffer solution and hydrolyzed by enzyme, sample tissue with much protein was deposited with HCIO4, centrifuged, and extracted with additional organic solution at adjusted alkaline pH which was evaporated revolvely later. The residue was dissolved in salt, transited by MCX and analysed after washed by aminated methanol. A linearity of nine β-agonists was obtained from2.5to50μg·kg-1. r=0.9943～0.9981, respectively. The LODs of method were between0.010-0.086μg·kg-1and the average recoveries were70.01%～113.72%. The method was rapid and sensitive, and suitable for the determination of nine β-agonists in medical gelatin hard capsule shells.