Determination Of Multiple Residues In Aquatic Product By UPLC-MS-MS

With the development of stock raising, all kind of antibiotics had been used as veterinary drug, e.x. chloramphenicols, sulfonamides and albendazoles. They are widely used for the treatment of bacterial diseases and promotion of growth in animal husbandry. The residues of veterinary drug had been appeared in animal derived food as the illogicality application of veterinary drug. People's health is harmed by the toxic effect. This thesis focus on the developing of the analytical methods for monitoring three kinds of drug residues in aquatic products employing by ultra performance liquid chromatography-tandem mass spectrometry, the main research area in this thesis can be included as follows:1. An untra-performance liquid chromatography-electrospray tandem mass spectrometry (UPLC-MS/MS) for the simultaneous determination of CAPs in aquatic products has been developed. Fish tissues are extracted with ethyl acetate solvent, and purification with multi-walled carbon nanotubes (MWCNTs) solid phase extraction cartridge, followed by liquid chromatography-tandem mass spectrometry analysis. The residues were separated by reverse phase liquid chromatography using 20% acetonitrile and 80% water as the initial elution solvents at 0.45 mL/min drip rate, confirmation and quantification by mass spectrum in the multiple reaction monitoring (MRM) mode via negtive electrospray ionization (ESI-), the MRM transition m/z 321.0, the parent ion of CAP, to m/zl51.9 and 194.0, transition m/z 356.0(FF)to 184.9 and 336.0, transition m/z 326.0(CAP-D5)to 157.0 and 262.0. The linear ranges is (CAP) 0.1-20.0 ng/mL, (FF) 0.1-10.0 ng/mL, and the linear correlation coefficient R2 is individually 0.9994 and 0.9990. In the three add concentration 0.5,1.0,2.5μg/kg, mean fortification recoveries are (CAP) 99.8%,103.4% and 94.7%, (FF) 99.0%,102.2% and 97.6%, the relative standard deviation are (CAP) 2.6%,4.3%,2.4%, (FF) 7.1%,4.1%,2.6%. Limits of detection are (CAP) 0.0014μg/kg, (FF) 0.0018μg/kg.2. A reversed-phase ultra performance liquid chromatography method with tandem mass-spectrometry detection was developed for the simultaneous determination of sulfonamides in aquatic products. The analyses were extracted with methanol, and then cleaned up with Multi-walled nanotubes solid phase extraction cartridges, followed by liquid chromatography-tandem mass spectrometry analysis. The analyzer confirmed and quantified by mass spectrum in the multiple reaction monitoring (MRM) mode via positive electrospray ionization (ESI+). The linear ranges of the sulfonamides are between 1.0-500.0 ng/mL and the linear correlation coefficient R2 0.9982-0.9996. In the three add concentration 0.5,1.0,2.5μg/kg, mean fortification recoveries are between 50.1%-126.6%, the relative standard deviations are 1.1%-11.3%. Limits of detection are 0.004-0.071μg/kg.3. An ultra-performance chromatography-electrospray tandem mass spectrometry (UPLC-MS/MS) for the simultaneous determination of ABZs in aquatic products has been developed. Tissues are extracted with ethyl acetate solvent, and purification with Agilent PS-DVB solid phase extraction cartridge, followed by liquid chromatography-tandem mass spectrometry analysis. The residues were separated by reverse phase liquid chromatography using 10% methanol and 90% water with 0.1% formic acid as the initial elution solvents at 0.45 mL/min drip rate, confirmation and quantification by mass spectrum in the multiple reaction monitoring (MRM) mode via positive electrospray ionization (ESI+), The linear ranges is (ABZ-NH2-SO2) 0.4-20.0 ng/mL, (ABZ) 0.2-20.0 ng/mL, (ABZSO) 0.8-20.0 ng/mL, (ABZSO2) 0.1-10.0 ng/mL and the linear correlation coefficient R2 is between 0.9988 and 0.9998. In the three add concentration 0.5,1.0,5.0μg/kg, mean fortification recoveries are between 75.9% and 112.1%, the relative standard deviation are between 0.56% and 4.79%. Limits of detection are (ABZ-NH2-SO2) 0.0210μg/kg, (ABZ) 0.0019μg/kg, (ABZSO) 0.0328μg/kg, (ABZSO2) 0.0023μg/kg.The experimental results indicated that the established ultra performance liquid chromatography-tandem mass spectrometry protocol was specific:chloramphenicols sulfonamides and albendzaoles residues in complex matrix sample could analyzed and determined rapidly. The experimental results could be used in provided drug application reference, safety for the aquatic product. This is an important theoretical and practical significance to monitor aquatic product and protect people's health. In addition, the established method could be used in resolving lag technical standards of China's export products in aquatic product and play a positive role in crossing TBT.