Study Of Analytic Methods Of Veterinary Drug Residue In Royal Jelly And Milk

Food safety problem of animal origin is a public health problem widely concerned by the whole society. In recent years, Veterinary drug residue in food excessive events occurs frequently, long-term low intake of veterinary drug residue will lead to a variety of chronic, chemicals, and induction of human pathogenic bacteria to produce the problem such as drug resistance. The European Union, the United States and China's ministry of agriculture, etc established the maximum residue limits(MRLs) of veterinary drug residue in food of animal origin. Therefore, strengthen the detection of veterinary drug residue in food analysis, development a rapid, simple, time-saving and efficient detection method to guarantee food safety and human health is of great importance. This paper is divided into three chapters:Chapter one: described the research status of veterinary drug residue Briefly,the pretreatment methods of veterinary drug residue in food detection and ultra performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry technology.Chapter two: A simple and rapid multi-class multi-residue analytical method was developed for rapid screening and quantitative determination of multiple classes of veterinary drug residues in royal jelly by improved QuEChERS-ultra performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry. 90 kinds of veterinary drugs secondary mass spectrum database for the confirmation and identification of the target compounds was established. Using matrix matching standard solution for Quantitative determination. The response of the detector was linear for each target compounds in wide concentration range(at least, two orders of magnitude) with correlation coefficient(R2) of 0.9921~0.9999. The range of the limit of quantification for these compounds in the royal jelly ranged from 0.21 to 20 mg/kg. The repeatability and reproducibility were in the range of 3.01~11.6% and 5.97~14.9%, respectively. The average recoveries ranged from 70.21 to 120.1% with relative standard deviation of 1.77~9.90% at three concentration levels, The result is satisfactory. This method can be applied to the actual royal jelly samples screening analysis and the quantitative determination of veterinary drug residue.Chapter three: An ultra-performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry(UPLC-QTOF-MS) was developed for the screening and quantification of more than 90 kinds of veterinary drug residues in milk,It is a simple and rapid multi-class multi-residue analytical method.A modified quick, easy, cheap, effective, rugged, and safe(QuEChERS) procedure was developed for the sample preparation without the solid-phase extraction step. Using secondary mass spectral database for the qualitative screening and matrix matching standard solution for Quantitative determination. The linearity, sensitivity, accuracy, repeatability, and reproducibility of the method were fully validated. Implementation of veterinary drug residues in the actual of milk samples rapid screening and confirmation.The proposed analytical method can quickly identify identification and quantitative determination of trace of veterinary drug residues in milk samples.