| With the continuous improvement of China economic development and people's living standards, the national consumption level are constantly rising, increasing demands for food.When food safety incidents have occurred in recent years, food safety is under unprecedented attention, food safety issues related to the health and survival of each person's relationship to the rise and development of the nation's food safety is extremely heavy philosophy into every human heart.For the health and prosperity of the people of a normal market economy, improve food safety testing methods and techniques have a very important practical significance.In recent years, the negative reports about the safety of dairy products after another, of which of course include veterinary drug residues. Determination of veterinary drug residues in milk products has been more and more people's attention. Veterinary drugs in dairy farming or in the process of a large number of non-standard use can cause excessive veterinary drug residues in dairy products. Based on this paper studies the most common dairy products in the most common liquid milk and milk powder, ultra-fast liquid chromatography- tandem mass spectrometry technology, the establishment of liquid milk and milk powder antibiotics, quinolones and sulfonamides veterinary drug residues in rapid quantitative and qualitative analytical methods.Research content of this paper is divided into three areas, the following key elements:Chapter One: In the case of existing methods and determination of veterinary drug residues in dairy products overview.Chapter Two: ultra-fast liquid chromatography- tandem mass spectrometry technology, the establishment of dairy products 12 antibiotics Residues ultra fast liquid chromatography-mass spectrometry confirmatory analysis.Chapter Three: ultra-fast liquid chromatography- tandem mass spectrometry technology, the establishment of 12 sulfonamides and five quinolones ultra-fast liquid chromatography-mass spectrometry confirmatory analysis.The results are as follows:1.The proteins in samples of milk products were precipitated by acetonitrile and degreased by n-hexane with liquid-liquid extraction, then cleaned by 0.22 ?m millipore filter. The filtrate was separated on a EndeavorsilTM C18 column by gradient elution in 12 minutes with acetonitrile-0.1 % formic acid as mobile phase. Identified by electrospray ionization in positive mode using multiple reaction monitoring, and quantified with external standards. The calibration curves of residues of 12 antibiotics in milk products showed good linearity in the range of 0.1~100 ?g/L with correlation coefficient in the range of 0.9900~0.9998. The detection limit of the method was from 0.1 to 5 ?g/kg. The recoveries ranged from 66.30~107.7 %, and relative standard deviations in the range of 1.2~12 % were obtained. The screening results of a spiked milk sample showed that all the spiked antibiotics could be detected with their deviations of retention time ?0.05 min. The method was applied to determine residues of 12 antibiotics in milk products by UPLC-MS/MS and proved to be simple, rapid, and accurate, and meet the requirements of monitoring of antibiotics in milk products.2. The proteins in milk products were precipitated by acetonitrile, then cleaned by 0.22 ?m millipore filter. The filtrate was separated on a EndeavorsilTM C18 column by gradient elution with acetonitrile-0.1 % formic acid as mobile phase. The calibration curves of 17 veterinary drugs in milk products showed good linearity in the range of 0.05~100 ?g/L with correlation coefficient in the range of 0.9906~0.9998. The detection limit was 0.05~0.1 ?g/L. The recoveries ranged from 75.88~116.0 %, and relative standard deviations in the range of 1.5~13 % were obtained.The established method is rapid, simple, sensitive and green features, to meet the daily testing requirements for food inspection industry to detect liquid milk and milk solids antibiotics, sulfonamides and quinolones residues of veterinary drugs. |
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