Determination Of Four β₂-adrenergic Agonists In Environmental Water Samples And Dairy Samples Using GC-MS

At present, the researchers focuse on using chromatography-tandem mass spectrometry analysis of β2-adrenergic agonist in animal origin food, animal tissue, urine and blood, but researching on their residues in environmental water samples and milk products are rarely. The purpose of this paper is to establish two different analysis ways to investigate β2-adrenergic agonist by GC-MS, which provides new choice for their residues analysis in the field of food safety monitoring.The review of this paper introduces the domestic and foreign chromatography-mass spectrometry technique for β2-adrenergic agonist pretreatment, derivatization methods and a variety of detection technologies. The experiment part introduced two aspects. The first aspect is the qualitative and quantitative analysis of β2-adrenergic agonist in environmental water samples by GC-MS technology. And the other one is the qualitative and quantitative analysis of β2-adrenergic agonist in milk and their products by GC-MS technology.The specific research methods and results includs:1. Four β2-adrenergic agonists(terbutaline, salbutamol, salmeterol and fenoterol) in water samples were qualitative analysised by GC-MS technology. At the same time, we optimized the pretreatment processes, including GC oven temperature mode,derivative and extraction method. The extraction means had been emphatically studied, including liquid-liquid extraction and solid phase extraction. Experiment results showed that the liquid-liquid extraction was more suitable for the analysis of them. The optimized sample extraction program used ethyl acetate as extraction solvent and adjusted p H to 9.5 by ammonium chloride buffer solution; 5 m L water samples was divided by equal extracted respectively, then merged them together.2. Under optimal condition, 4 β2-adrenergic agonists in environmental water samples were quantitative analysised by GC-MS technology. The established methodology display, they had a good linear relationship(R2>0.9990), the detection limits of the method were found from 0.104 to 2.326 ng/m L(S/N= 3), the limit of quantification was obtained in range of 0.347~7.753 ng/m L(S/N= 10), intra-day and inter-day precision values were less than 4% and 5%, with the average recovery rate ranged from 97.168% to 108.637%. The method was simple, accurate, and reliable. Meanwhile, they were not detected in real environmental water where came from nine places of Zhengzhou and other cities.3. Four β2-adrenergic agonists in milk and their products were qualitative and quantitative analysised by GC-MS technology. Pretreatment approaches were optimized and 10% trichloroacetic acid to subside protein and C18 column to purify samples were used at last. Under the condition of the qualitative analysis of them, they were quantitatively analyzed. The established methodology display, they had a good linear relationship(R2>0.9962), the detection limits of method were found from 0.085 to 2.568 ng/m L(S/N= 3), the limit of quantification was obtained in range of 0.283~8.560 ng/m L(S/N= 10), intra-day and inter-day precision values were less than 3% and 5%, with the average recovery rate ranged from 93.837% to 99.203%. Meanwhile, they were not detected in 20 real milk samples which came from local supermarket.