The Applied Research On Detecting Vetrerinary Drug Residues Of Animalistic Food By Liquid Chromatography-Tandem Mass Spectrometer Technology

Food safety problem has always been bone of contention in trade around the world because of its high risk, high sensitivity and high profile. For example, Japan, EU and other developed countries or regions regularly inspect China’s exported foods, and they will take measures to deal with those foods which do not conform to the standard technical requirements (especially food safety requirements). The relative measures mainly are bulletin, return, destruction, increasing the strength of sampling and even stopping import such foods from China. Today, China has joined WTO more than ten years, our foods still be abandoned and refunded owing to the detection of nitrofuran and other chemicals. Therefore, it is significant to establish a rapid detection method which adapt to foreign technological regulations and estimate it using foreign equivalent evaluation standard. Equivalent detecting standard plays more and more important role in solving international trade disputes. EU, America and other developed economies spare no efforts to develop and promote their own evaluation system, because the rule makers will be policy deciders in the future. Consequently, our country should pay attention to investigate and establish detection evaluation standard or set up the international applicable standard evaluation system, which can enhance our country’s voice in international rules and will greatly enrich our technology to cope with the international trade disputes.This paper was focus on detecting chloramphenicol, nitrofurans and tetracycline of animalistic food, such as eel, lobster, casing, egg, and honey, with liquid chromatography-tandem mass spectrometer technology.1.Using liquid chromatography combined with tandem mass spectrometry (LC-MS/MS) to detect casings, chloramphenicol residues in honey. Chloramphenicol sample under alkaline conditions, extracted with ethyl acetate, the extract after drying of the liquid nitrogen gas, the residue was washed with acetonitrile+water dissolved, liquid-liquid distribution defatted with hexane. Liquid chromatography-tandem mass spectrometry detection, internal standard amount. The limit of quantification of chloramphenicol can be set at0.1mg/kg. Cubic matrix produced a calibration curve for each point are less than10%deviation from the calibration curve, calibration curve correlation coefficients were greater than0.99, and adds a concentration of0.1g/kg,0.2g/kg,0.4g/kg (corresponding to the concentration of the solution was0.05ng/mL,0.1ng/mL,0.2ng/mL) were within the linear range. Repeatability RSD<43%. Quantitative methods in the concentration levels of p (p1microg/kg) recoveries ranged from-50%to+20%. API4000Q-TRAP mass spectrometer API4000+mass spectrometer recovery results small difference, robustness.2.Detected by liquid chromatography tandem mass spectrometry (LC-MS/MS) associated with a lobster nitrofuran residues. Lobster residues of nitrofuran metabolites under acidic conditions with2-nitrobenzaldehyde derivative, ethyl acetate extract secondary electrospray ionization liquid chromatography-tandem mass spectrometry. Isotopically labeled internal standard. Four nitrofuran metabolites in the limit of quantification can be defined as0.5μg/kg. Repeatability RSD<43%of lobster matrix Add0.5μg/kg,1.0μg/kg,2.0μg/kg3levels, each level2parallel tests, the same person three times repeated trials, to meet the quantitative The method analytes quality score of10μg/kg repeatability RSD values<21%of requirements.3.Using liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) was detected in the eel, honey, chicken tetracyclines residues. Tetracycline family of antibiotics residues in the sample is extracted with0.1mol/L Na2EDTA-Mcllvaine buffer (pH to4.0±0.05), after filtration and centrifugation, the supernatant HLB solid phase extraction column purification by high performance liquid chromatography-mass spectrometry/mass spectrometer, quantified by the matrix external standard peak area. Of tetracycline drugs in the limit of quantification can be set at10.0μg/kg. Preparation of a matrix of points (J-std0,5.0,10.0,20.0,40.0,100ng/mL) standard solution, three times worked matrix calibration curve, each point deviates from the calibration curve are less than10%, the correlation coefficients were greater than0.99, and the added concentration10.Oμg/kg20.0μg/kg40.0μg/kg (corresponding to a solution concentration of10.0ng/mL,20.0ng/mL,40.0ng/mL) are linear range.