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《超高效液相色譜_四極桿_飛行時間質(zhì)譜法快速篩查牛奶中的農(nóng)藥和獸藥殘留》由會員上傳分享,免費在線閱讀,更多相關(guān)內(nèi)容在行業(yè)資料-天天文庫。
1、2012年6月Vol.30No.6June2012ChineseJournalofChromatography560~567研究論文DOI:10.3724/SP.J.1123.2012.02021超高效液相色譜-四極桿-飛行時間質(zhì)譜法快速篩查牛奶中的農(nóng)藥和獸藥殘留1,231,2*1,2高馥蝶,趙妍,邵兵,張晶(1.首都醫(yī)科大學(xué)公共衛(wèi)生與家庭醫(yī)學(xué)學(xué)院,北京100069;2.北京市疾病預(yù)防控制中心,食物中毒診斷溯源技術(shù)北京市重點實驗室,北京100013;3.南京市產(chǎn)品質(zhì)量監(jiān)督檢驗院,江蘇南京210028)摘要:利用超高效液相色譜
2、-四極桿-飛行時間質(zhì)譜(UPLC-Q-TOF-MS)技術(shù)建立了牛奶中42種農(nóng)藥和獸藥殘留的快速檢測方法。目標藥物包括常用的13種農(nóng)藥和29種獸藥,采用QuEChERS(Quick,Easy,Cheap,Effective,Rugged,andSafe)方法進行樣品前處理。牛奶樣品經(jīng)含1%甲酸的乙腈溶液提取,同時加入無水硫酸鈉和氯化鉀TM鹽析,提取液經(jīng)C18填料凈化后直接測定。目標藥物經(jīng)ACQUITYUPLCBEHC18柱分離,以乙腈和0.1%甲酸E水溶液為流動相進行梯度洗脫,采用正離子全信息串聯(lián)質(zhì)譜掃描模式(MS)進行檢測。
3、結(jié)果表明,牛奶中42種農(nóng)藥和獸藥的定量限(LOQ,S/N=10)為1~100μg/kg;3個加標水平的平均回收率為68.2%~129.1%,相對標準偏差為2.8%~30.8%。該方法快速簡便、靈敏度較高,可用于牛奶中42種農(nóng)獸藥的快速篩查。關(guān)鍵詞:超高效液相色譜-四極桿-飛行時間質(zhì)譜;QuEChERS;農(nóng)藥殘留;獸藥殘留;牛奶中圖分類號:O658文獻標識碼:A文章編號:1000-8713(2012)06-0560-08Determinationofresiduesofpesticidesandveterinarydrugsi
4、nmilkbyultraperformanceliquidchromatographycoupledwithquadrupole-timeofflightmassspectrometry1,231,2*1,2GAOFudie,ZHAOYan,SHAOBing,ZHANGJing(1.SchoolofPublicHealthandFamilyMedicine,CapitalMedicalUniversity,Beijing100069,China;2.BeijingKeyLaboratoryofDiagnosticandTra
5、ceabilityTechnologiesforFoodPoisoning,BeijingCentersforDiseasesControlandPrevention,Beijing100013,China;3.NanjingInstituteofSupervisionandTestingonProductQuality,Nanjing210028,China)Abstract:Ananalyticalmethodwasestablishedforthesimultaneousdeterminationof42pesti-c
6、idesandveterinarydrugsinmilkbyultraperformanceliquidchromatographycoupledwithquadrupole-timeofflightmassspectrometry(UPLC-Q-TOF-MS).Thetargetcompoundsarethecommonlyuseddrugsincluding13pesticidesand29veterinarydrugs.TheQuEChERS(Quick,Easy,Cheap,Effective,Rugged,andS
7、afe)methodwasusedforsamplepreparation.Theanalytesinmilksampleswereextractedwithacetonitrilecontaining1.0%(v/v)formicacid,andweresaltedoutbyaddinganhydroussodiumsulfateandpotassiumchloride.Afterthat,theextractsolutionwaspurifiedbydispersivesolidphaseextractionwithC1
8、8sorbent.InTMthechromatographicanalysisof42targetcompoundswereseparatedonanACQUITYUPLCBEHC18columnwiththegradientelutionusingthemobilephasesoface