蜂蜜中烟曲霉素残留量测定 液相色谱串联质谱法英文意见稿.docVIP

Method for the determination of fumagillin residues in honey 棗Liquid chromatography-tandem mass spectrometry method Scope This standard specifies the method of determination of fumagillin in honey. This standard is applicable to the determination of fumagillin in honey. Normative reference The following normative documents contain provisions which，through reference in this text，constitute provisions of this standard. For dated references，subsequent amendments to，or revisions of.,any of these publications do not apply. However protocol to agreements based on this standard are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below.For undated references，the latest edition of the normative document referred to applies. GB/T 6682 Water for analytical laboratory use-Specification and test methods. Principle The honey samples are diluted with water, and cleaned by HLB solid phase extraction. Determined by LC/MS-MS(ESI+), using external standard method. Regents and materials Unless otherwise specified ,all regents used are A.R. and “water” is deionized water. Methanol：HPLC grade. Acetonitrile: HPLC grade. Formic acid: guarantee reagent. Ethyl acetate: HPLC grade. Methanol-water（3+7，V:V): Mix 30ml methanol(4.1)and 100ml water. Acetonitrile-water（1+1，V:V): Mix 50ml acetonitrile(4.2)and 50ml water. Standards: Fumagillin, purity≥98%. Stock standard solutions(1.0mg/mL):Separately accurately weigh an adequate amount of fumagillin standards(4.7), dissolve in methanol and prepare a solution of 1.0mg/mL as the stock standard solutions. Solutions are stable for a year at –18 ℃. Working standard solutions(1.0μg/ml): According to the requirement, pipette adequate amount of fumagillin stock standard solutions(4.8), and dissolve in methanol and prepare a solution of 1.0μg/mL. dilute with the extraction solution for blank sample to prepare working standard mix solutions in sample matrix of appropriate concentration. H