中華人民共和國出入境檢驗檢疫行業(yè)標(biāo)準(zhǔn)出口食品中六種合成甜味劑的檢測方法液相色譜-質(zhì)譜/質(zhì)譜法DeterminationofsixkindsofartificialsweI1出口食品中六種合成甜味劑的檢測方法4.1020%乙酸鋅溶液：20g乙酸鋅溶解于100mL水中。4.12甲酸-三乙胺緩沖溶液(pH=4.5):取0.8mL甲酸、2.5mL三乙胺，用水稀釋并定容至4.15標(biāo)準(zhǔn)貯備液：準(zhǔn)確稱取適量的4.14中的標(biāo)準(zhǔn)物質(zhì)，用甲醇-水(1+1,體積比)分別配制成質(zhì)量濃210%亞鐵氰化鉀(4.9)和1mL20%乙酸鋅溶液(4.10)以及5mL三氯甲烷，渦旋混勻2min,以3依次用5mL甲醇、5mL水活化HLB固相萃取小柱，棄去淋洗液，然后將上述所得的提取液0.5mL/min,收集洗脫液至刻度離心管，在40℃下空氣吹濃縮至0.5mL,并用甲醇-水(4.13)定容至1.0mL,過0.45μm有機(jī)濾膜，供液相色譜-質(zhì)譜/質(zhì)譜儀測定。時間%銨乙腈%4析。在上述色譜條件下甜蜜素、糖精鈉、安賽蜜、阿斯巴甜、阿力甜、紐甜的參考保留時間分別為6.03min、5.03min、4.31min、6.79min、7.31min反應(yīng)監(jiān)測色譜圖參見附錄C中圖C.1。7.3.3.2定性測定士20士25士30士507.4空白試驗8.1測定低限5添加水平及回收率數(shù)據(jù)見表3和表4?；厥章史秶?奶油安賽蜜阿斯巴甜阿力甜回收率范圍%糕點6表4(續(xù))回收率范圍%糕點蜜餞安賽蜜阿斯巴甜阿力甜7中文名稱安賽蜜阿斯巴甜阿力甜8參考質(zhì)譜條件1c)氣簾氣(CUR):0.172MPa;f)碰撞氣(CAD):Medium;i)定性離子對、定量離子對、碰撞能量、去簇電壓、碰撞室出入口電壓和碰撞室出口電壓見化合物中文名留時間去簇電壓(DP)V碰撞能量(CE)入口電壓(EP)V出口電壓(CXP)V80.1”安賽蜜阿斯巴甜阿力甜注：帶“*”的離子為定量離子。9(資料性附錄)標(biāo)準(zhǔn)溶液的多反應(yīng)監(jiān)測(MRM)色譜圖b)圖C.1標(biāo)準(zhǔn)溶液的多反應(yīng)監(jiān)測(MRM)色譜圖foodstuffsforexport—LC-MThisstandardspecifiesthedeterminationanacesulfame-K,aspartame,alitame,neotameinfoodacesulfame-K,aspartame,alitame,neotameredwine,juice,cookie,sweetmeatanapplytothisstandard.Forundatedrformic-triethylaminebuffersolution(pH=4.5).Theextractextractedwithmethanol-water(1+1,V/V),th4.1Acetonitril:HPLCgrade.4.4Ammoniumformatewater.4.12Formicacid-triethylaminebuffersolution(pH=4-5):accu4.13Methanol-water(1+1,v/v)4.14Standardofsodiumcy4.15Standardstocksolution:AextractsolutiontoprepareaseriesofstanIncourseofsampling,itmustbetakentoavoidcoThetestsamplesofstoredat0℃~4℃.Thetestsamplesofmilk,yoghourt,butter,cheeseandicecreamshouldbeter,cheese,icecream,respectively.Forbutterandicecream,add5gmarinesandandgroundade-Methanol-water(4.eluentandblownearlydrywithnitrogenat40℃.Dissoe)Injectionvolum0.1%formicacid-5mmol/Lammoni%%Accordingtotheestimatedapproximateconcsesofartificialsweetenelinearrangeoftheinstrumentaldetection.Iftheresponseisabovethelinearrange,dilutethesamplesolutionwithmethanol.UndertheaboveLC-MS/MSoperatingumcyclamate,saccharinSodium,acesulfaUnderabovedeterminentandtherelativeionaard,atcomparableconcentrations,witpermittedrelativetolerawithoutadditionofsamA—thepeakareaofartificialsweeteneV—thefinalvolumeofsamplesolution,mL;A?—thepeakareaofartificialsweetenerinthestandardwm—thecorrespondingmassoftesThelimitofdeterminationofartAccordingtotheexperimentaldataformilk,milkpowder,yoghourt,butter,chwine,juice,cookie,sweetmeat,alinmilk,milkpowder,yogh%77.8～86.0%f)Collisiongas(CAi)Confirmationion,quantificationVVV80.1*VVV5.000