| During the growth process,livestock and poultry are susceptible to viral or bacterial infections,which leads to a large number of deaths.Therefore,antiviral and antibiotic drugs are often fed to livestock and poultry by breeding enterprises or individuals to prevent or treat animal diseases.However,there are few standards for human-used antiviral and antibiotic drugs in animal-derived foods.In this paper,detection methods were established by combining Solid Phase Extraction with UPLC-MS/MS for the detection of protease inhibitors and antituberculosis agents in animal-derived foods.Residues of 46veterinary drugs in chicken were analyzed by using improved Qu ECh ERS technology and UPLC-MS/MS.The main findings were as followed:1.For the antiviral drugs of protease inhibitors in poultry meat,a UPLC-MS/MS method for the determination of the four protease inhibitor residues in chicken was established by optimizing the instrument conditions and pretreatment conditions.Good linearities of the four protease inhibitors were showed in the range of 0.1-20.0?g/L,and the correlation coefficients(r~2)were greater than 0.99.The limits of detection(LODs,S/N=3)and the limits of quantification(LOQs,S/N=10)of the four protease inhibitors were 0.06-0.30?g/kg and 0.20-0.90?g/kg.At the spiked levels of 1.0,2.0 and 10.0?g/kg.The average recovery rates of the four compounds in chicken were between 69.0%to 106.0%.The intra-day and inter-day relative standard deviations(RSDs)were2.2%-13.8%(n=6)and 3.6%-14.6%(n=3),respectively.The method is simple,efficient,sensitive and accurate,and it can be used to detect the residues of saquinavir,ritonavir,nelfinavir,indinavir in chicken.2.Aiming at the antituberculous antibiotics in animal tissue,a method for the determination of the four antituberculosis agents in chicken,beef and pork by UPLC-MS/MS was established by optimizing the instrument conditions and pretreatment conditions.The samples were ultrasonically extracted with acidified acetonitrile,purified by HLB column,and separated on Luna~?C8 column(150 mm×2 mm,3?m)using0.2%formic acid aqueous solution(containing 5 mmol/L ammonium acetate)and acetonitrile as the mobile phases with gradient elution.The determination was carried out by using an electrospray ion source in the positive and multiple-reaction monitoring(MRM)modes.The linear ranges of rifampin,rifamycin,rifapentine and rifabutin were 0.3-20.0,0.1-20.0,0.3-20.0,0.2-20.0?g/L,respectively,and the correlation coefficients(r~2)were greater than 0.99.The limits of detection(LODs)and the limits of quantification(LOQs)of the four compounds were0.24-0.36?g/kg and 0.80-1.20?g/kg.The average recoveries of the four compounds in chicken,beef and pork were 69.6%-103.8%,87.2%-104.5%,66.3%-100.9%,respectively,and the relative standard deviation(RSD,n=6)were 4.6%-13.1%,5.6%-13.8%,4.2%-12.2%.This method is sensitive,simple and efficient.3.Aiming at various antiviral and antibiotics drugs in poultry meat,this experiment established a method for the detection of 46 veterinary drug residues in chicken by optimizing instrument conditions and pretreatment conditions,using improved Qu ECh ERS technology combined with UPLC-MS/MS method.The 46 compounds have good linear relationships in their respective linear ranges,with correlation coefficients(r~2)were greater than 0.99,and the limits of detection(LODs)were in the range of 0.05-20.00?g/kg,the limits of quantification(LOQs)were range from 0.10?g/kg to 50.00?g/kg.Because the lower detection limits of each compound were different,the average recoveries of 46compounds were between 61.7%to 103.3%,and the relative standard deviation(RSD,n=6)was 1.9%-14.7%at their respective addition levels.This method has the advantages of simple and quick pretreatment,good purification effect,high sensitivity and low cost,and it is suitable for the rapid identification and quantitative detection of various kinds of drug residues in poultry meat. |
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