Study On Analytical Method Of The Multi-Risk Substance Residues In Chicken Muscle

In this paper, a liquid chromatography tandem mass spectrometry method was established to determin 120 veterinary drugs. A gas chromatography tandem mass spectrometry was also established to determin 43 environmental pollutants. A Q-TOF spectral datebase covers statins, antibiotics, β-Adrenergic receptor agonists, hormones and other drugs sum up to 150 kinds of compounds was built.The research contents and results are as follows:1. Simultaneous determination of 120 compounds including quinolones, sulfanilamide, nafiles, statins drugs in chicken muscle was established by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The analytes were separated on a BEH C18(2.1mm×100mm,1.7 μm) column after pretreatment, eluted by gradient with 5 mmol ammonium acetate (added by 0.1% formic acid) and methanol, identified by electrospray ionization mass spectrometry in both positive and negative mode using multiple reaction monitoring, quantified by external standard method. The limits of detection (LOD, S/N=3) and quantification (LOQ, S/N=10) of 120 compounds were 0.1～1.0 μg/kg and 0.3～3.0 μg/kg, respectively. The correlation coefficients of linear calibration curve were over 0.9900 in the ranges varied from 1.0～100 μg/kg. The recoveries of analytes in chicken muscle samples were 56.7% ～114.9% at the spiked level of 5,10 and 20 μg/kg, and the relative standard deviations were in the ranges 0.53% -11.18%. The proposed method has been applied to the determination of statins drugs in actual chicken muscle sample, a satisfied results was obtained.2. Simultaneous determination of 43 environmental pollutants including polycyclic aromatic hydrocarbons, alkylphenols, phthalate esters was established.The total ion flow spectra of 43 kinds of environmental pollutants were determined by single stage mass spectrometry (SCAN) method, and the retention time of each environmental pollutant was determined. Then, the MRM method was used to analyze the 43 environmental pollutants, The limits of detection (LOD, S/N=3) and quantification (LOQ, S/N=10) of 43 environmental pollutants were 0.5～12.1 μg/kg and 1.0～200 μg/kg, respectively. The correlation coefficients of linear calibration curve were over 0.9950 in the ranges varied from 1.0～200 μg/kg, The recoveries of analytes in chicken muscle samples were 70.0%-110.8% at the spiked level of 5.0,20 and 50 μg/kg, and the relative standard deviations were in the ranges 5.23%～9.76%.3. A Q-TOF spectral datebase covered statins, sulfonamides, macrocyclic ster, hormones and beta receptor agonists was established. Full scan accurate mass spectrum can be obtained through the spectral library, and the number of scanning object is infinite, the scanning spectrum graph can be extracted and processed subsequently, on this base, the informations including compound name, molecular formula, rentention time, accurate molecular weight of parent ion and 2 daughter ions were established, the unknown target compounds can be identified by these parameters.