lcmsms测定蜂蜜中兽药多残留-determination of multi-residue of veterinary drugs in honey by lcm sms.docxVIP

摘要摘要随着人们生活水平的提高，食品质量和安全问题越来越受到人们的关注，尤其是近几年我国频发的食品安全事件，直接危害到人类的身体健康，因此更是引起了全社会的广泛关注。为了保证动物源食品安全，建立准确灵敏的兽药多残留检测方法具有重要意义。蜂蜜是广受人们欢迎的天然保健食品，但蜂农为降低蜜蜂死亡率，提高蜂蜜产量，常存在不合理用药现象，导致蜂蜜中存在不同程度的兽药残留。而蜂蜜基质较复杂，兽药理化性质也各不相同，这就给蜂蜜中多类兽药残留检测带来了一定的困难。因此，建立蜂蜜中兽药多残留的分析方法是控制蜂产品质量的迫切要求。本文以养蜂业中常用的兽药为检测对象，对蜂蜜中多类兽药残留的提取、净化方法进行考察，建立了LC-MS/MS同时检测蜂蜜中60种兽药残留的分析方法，主要研究结果如下：蜂蜜样品采用Mcllvaine缓冲溶液（pH=4）稀释，5%醋酸乙腈提取，经盐析吸水，由NH2净化，氮吹浓缩，重溶过膜后，LC-MS/MS进行测定。60种兽药在3个添加水平（n=6）下，平均回收率在70%～120%范围内的分别占96.7%，98.3%和98.3%，相对标准偏差（RSD）为0.6%~19.8%。检出限（LOD）和定量限（LOQ）分别在0.01~17.99μg/kg和0.02~59.97μg/kg范围内，线性相关系数（r2）＞0.995占总数的81.7%。该方法简单、快速、准确，适用于蜂蜜中多类兽药的高通量筛查检测。关键词蜂蜜兽药多残留QuEChERSLC-MS/MSAbstractAbstractWiththeimprovementofpeopleslivingstandards,moreandmoreattentionhasbeenpaidtotheissuesoffoodqualityandsafety,especiallyinrecentyears,severalfoodsafetyeventswhichdoharmtohumanhealthdirectly,havecausedconcernfromthewholesociety.Inordertoensurethesafetyofanimaloriginalfood,itisimportanttodevelopanaccurateandsensitiveveterinarymulti-residueanalysismethod.Asanaturalhealthyfood,honeyisgreatlywelcomedbytheconsumers.Toreducebeedeathrateandimprovehoneyproduction,beekeepersoftenusedifferentveterinarydrugswhichcauseveterinarydrugresiduesinhoney.Ashoneyisacomplexmatrixandtheveterinarymedicineshavedifferentphysicalandchemicalproperties,itismuchdifficulttodetecttheveterinarydrugresiduesinhoney.Therefore,itisnecessarytoestablishamulti-residueanalysismethodforthequalitycontrolofhoney.Inthisthesis,wechosecommonlyusedveterinarydrugsasthetargetcompoundsandoptimizedtheextractionandpurificationmethodandfinallyestablishedaQuEChERS-LC-MS/MSmethodforthesimultaneousdeterminationof60veterinarydrugresiduesinhoney,themainconclusionsareasfollows:ThehoneysamplewasdilutedwithMcllvainebuffersolution(pH=4.0),andextractedwith5%aceticacid-acetonitrile.Aftereliminationofwaterbysaltingouteffect,theextractwaspurifiedbyNH2sorbentandevaporatedundernitrogenstream.Theresiduewasre-dissolvedandfiltered,thefinalsolutionwasanalyzedbyLC-MS/MS.Atthreespikedlevels(n=6),thepercent