Research On The Determination Method Of Carbofuran And Its Metabolites Residues In Bee Products

This study is based on the different bee products substrate, a variety of differentextraction and purification conditions of research method and instrument. The rusults:acidic acetonitrile is used to extract carbofuran and its metabolites, purificating withCarb/NH2double SPE column, collecting with toluene/acetonitrile (1+3) mixtureelution; high performance liquid chromatography-tandem mass spectrometry(HPLC/MS/MS) using in different bee products were simultaneously detectingcarbofuran and3-hydroxycarbofuran carbofuran phenol which are the metabolites ofcarbofuran.1) Chosing the honey, royal jelly, pollen and propolis, into which are added thestandard material of carbofuran and its metabolites, respectively with methylenechloride, acetone--methylene chloride, acetonitrile-ethyl ether, acetonitrile and acidicacetonitrile to compare their treatment effects.The results show that the extracted byacidic acetonitrile as the solvent is superior to other reagent extraction method, whoserecovery rate is83.1%~91.2%and variation coefficient is1.3%~7.1%.2) Chosing the honey, royal jelly, pollen and propolis, added with carbofuran andits metabolite that are standard materials, which are adopting the HLB small column,amino SPE column, column C18SPE small, and Carb/NH2double SPE column thatare purification columns. The results show that the Carb/NH2double column has thebest capacity of purification, and that the recovery were87.1%~97.1%and thevariation coefficient is1.7%~5.2%. 3) Optimizing the conditions of determining liquidity that carbofuran and itsmetabolites need, the chromatographic column chromatographic conditions and theway of ionization, taper hole such as voltage, collision energy, qualitative quantitativeion mass spectrometry conditions, to solve the complexity of bee products matrix andspecial chemical properties that carbofuran and its metabolites have, leading the wayof chromatographic analysis.4) The results show that carbofuran and its metabolites in the range of0.08~100ng/mL and peak area exist a good linear relationship between response value, and thatcorrtelation coefficients were greater than0.99. And in detection of honey, royal jellyand pollen, carbofuran and its metabolites have the low detection limit of1.0μg/kg,and the quantitative limit of2.0μg/kg. In the detection of propolis, the low detectionlimit is5.0μg/kg, and quantitative limit is10.0μg/kg. Detecting different beeproducts at the same time show that under1times detection limit, twice detectionlimit and10times detection limit respectively joined with standard materials, therecovery rate is between75.4%~119%, with the variation coefficient between1.6%~16.4%.