飼料中溴苯那敏和氯苯那敏的測(cè)定 液相色譜-串聯(lián)質(zhì)譜法 編制說(shuō)明

2《飼料中氯苯那敏和溴苯那敏的測(cè)定液相色譜-串聯(lián)質(zhì)譜法》一、工作簡(jiǎn)況3定性定量分析.方法血液經(jīng)過(guò)乙腈沉淀蛋白后,振蕩,離心,過(guò)0.2LC-MS/MS分析,采用多反應(yīng)監(jiān)測(cè)模式。但缺乏飼料中氯苯那敏和NNChemicalFormula:C16H19ClN2MolecularWeight:274.8ChlorphenamineNNChemicalFormula:C16H19BrN2MolecularWeight:319.2brompheniramine)圖1.氯苯那敏和溴苯那敏的化學(xué)結(jié)構(gòu)4成立了標(biāo)準(zhǔn)工作小組，進(jìn)行標(biāo)準(zhǔn)的研制及起草工作，具體工色譜—質(zhì)譜聯(lián)用儀的儀器參數(shù)進(jìn)行研究，對(duì)方法的試驗(yàn)條件、主要技術(shù)指標(biāo)等進(jìn)行進(jìn)一混合飼料以及牛的精料補(bǔ)充料中氯苯那敏和溴二、標(biāo)準(zhǔn)編制原則和主要技術(shù)內(nèi)容確定的依據(jù)5本文件規(guī)定了飼料中氯苯那敏和溴苯那敏的進(jìn)行質(zhì)譜條件的優(yōu)化。通過(guò)一級(jí)全掃描質(zhì)譜得到氯表1溴苯那敏和氯苯那敏的質(zhì)譜條件藥物名稱Drug出峰時(shí)間Time(min)離子對(duì)Ionpairs(m/z)去簇電壓DP(V)碰撞能CE(eV)氯苯那敏2.72275.2>167.2275.2>230.2*4445溴苯那敏2.79319.1>167.1*319.1>274442.3.2色譜柱和流動(dòng)相的組成的選擇6進(jìn)行比較。結(jié)果表明采用BEHC18色譜柱時(shí)，梯度淋洗。發(fā)現(xiàn)氯苯那敏和溴苯那敏在C18色表2流動(dòng)相梯度條件時(shí)間(min)流速(mL/min)0.1甲酸水溶液(％)乙腈(％)TimeFlow0.1%FormicacidaqueoussolutionAcetonitrile00.4200.50.42020.4400.454.50.4207.00.42072.3.3提取條件的優(yōu)化和確定圖3氯苯那敏和溴苯那敏提取效果圖882.3.4凈化條件的優(yōu)化和確定910mL加入小柱內(nèi)，待樣液全部流出后，再加入3mL水清洗小柱，然后用3mL甲醇淋洗小柱，最后MCX用3mL5%氨水甲醇洗脫，MAX用3mL甲酸甲醇洗脫，C18、HLB小柱用3圖4不同固相萃取對(duì)凈化效果表3固相萃取柱容量考察結(jié)果樣至SPE小柱（SPE小柱依次用3mL甲醇和3mL水活化再先后用3mL水和3mL甲醇液質(zhì)檢測(cè)具有高靈敏度和高選擇性的同時(shí)也存在基質(zhì)效應(yīng)，不同飼3.2穩(wěn)定性考察2.3.7標(biāo)準(zhǔn)溶液有效期實(shí)驗(yàn)圖5氯苯那敏和溴苯那敏標(biāo)準(zhǔn)儲(chǔ)備液保存期實(shí)驗(yàn)2.4.1線性方程和線性范圍表4氯苯那敏和溴苯那敏線性方程33圖6空白雞配合飼料色譜圖圖7雞配合飼料陽(yáng)性添加（添加濃度10ng/g）色譜圖圖8雞空白預(yù)混合飼料色譜圖圖9雞預(yù)混合飼料陽(yáng)性添加（添加濃度10μg/kg）色譜圖圖10空白雞濃縮飼料色譜圖圖11雞濃縮飼料陽(yáng)性添加（添加濃度10μg/kg）色譜圖圖12空白豬配合飼料色譜圖圖13豬配合飼料陽(yáng)性添加（添加濃度10μg/kg）色譜圖圖14空白豬預(yù)混合飼料色譜圖圖15豬預(yù)混合飼料陽(yáng)性添加（添加濃度10μg/kg）色譜圖圖16空白奶牛精料補(bǔ)充料色譜圖圖17奶牛精料補(bǔ)充料陽(yáng)性添加（添加濃度10μg/kg）色譜圖圖18玉米載體空白色譜圖圖19玉米載體陽(yáng)性添加（添加濃度10μg/kg）色譜圖圖20石粉載體空白色譜圖圖21石粉載體陽(yáng)性添加（添加濃度10μg/kg）色譜圖2.5方法的回收率和重現(xiàn)性（%）（%）（%）（%）（%）（%）（%）（%）（%）（%）（%）（%）（%）（%）2022年4月，標(biāo)準(zhǔn)編制小組委托廣西飼料檢測(cè)料中氯苯那敏和溴苯那敏的測(cè)定》規(guī)定的方法能滿足飼料中氯苯那敏和溴苯那敏的測(cè)定要求，六、與有關(guān)法律、法規(guī)的關(guān)系七、重大分歧意見的處理經(jīng)過(guò)和依據(jù)對(duì)標(biāo)準(zhǔn)的《征求意見稿》進(jìn)行修改，無(wú)重大八、涉及專利的有關(guān)說(shuō)明九、貫徹國(guó)家標(biāo)準(zhǔn)的要求，以及組織措施、技術(shù)措施、過(guò)渡期和實(shí)施日期的建議等措施建議無(wú)maleateexhibitpotentantiviralactivityagainstabroadspectrumofinflFrontiersinMicrobiology.2018;9:2643.[2]DuF.Therapeuticeffectofchlorpheniramineintreatinandchronicrhinitis/sinusitis[J].PakistanJournalofPharmaceuticalSciences.2018;3[3]Chong-Chi,Chiu,Kuo-Sheng,etal.ChlorpheniramineproduPharmacologicalreports:PR[4]LirkP,HollmannMW,StrichartzG.Thescienceofapplication,andfuturedirections[5]劉芳,高登慧,歐德淵,等.兩種組胺受體拮抗劑對(duì)高致病性豬藍(lán)耳病臨床癥狀的影響[J].LiuFang,GaoDenghui,OuDeyuan,etal.EffectsofTwoHistamiClinicalSymptomsofHighlyPathogenicPorcineReproductiveandResSyndrome(PRRS)[J].GuizhouAnimalHusbandryandVeterinary,20[6]張楚珺,歐德淵,姚紅艷,等.組胺受體拮抗劑對(duì)低致病性禽流感患雞血液指標(biāo)的影響[J].ZHANGChujun,OUDeyuan,YAOHongyan,etal.Effectofhistaminereceptolowpathogenicavianinfluenzahematology[J].AnimalHusbandryandVeterinary2017,49(02):98-102.（inChinese）[7]GhandforoushanM,ZendehdelM,BabpourV.InteractionsDopamineD1Receptorsonfeedingbehaviorinchicken[J].IranianJourna[8]ZahraSB,RezaM,MohammadS,etal.Effeantagonist)onfoodanSongYuqing.Clinicaltreatmentofrabiesimmuneallergicreaction[J].ChinaAandVeterinaryAbstracts,2012,28(01):106-107.（inChinese）物殘留[J].農(nóng)產(chǎn)品加工,2020(07):45-49.DOI:10.16693/ki.1671-9646(X).2WANGJing,YEJiaming,WANGDrugsResiduesinLivestockandPoultryMeatbyUPLC-MS/MS[J].AgricultProcessing,2020(07):45-49.DOI:10.16693/ki.1671-9646(X).2020.04.012.（inChinese）[11]AdedapoA,AdemowoOG,AdedapoKS,etal.Potentialtochloroquineforthetreatmentofchildhoodmalaria[J].NigerianJournalofClinicalPractice,[12]HuaYM,HungCH,YuhYS.AcuteintoxicationoflidZengQiaoying.Analysisofafataldrugusecaseofoverdoseofchlorpheniramine[J].Physicianpharmaceuticalsintabletdosageformbyreversed-phasehighperforchromatography[J].TropicalJoudeterminationofactiveingredientsincoughandcoldpharmaceuticalsbyhighperformaliquidchromatography[J[16]劉凱雙,閆研,殷果,等.HPLC法同時(shí)測(cè)定復(fù)方金DOI:10.19778/j.chp.2021.LIUKaishuang,YANYan,YINGuo,etal.HPLCdeterminatiuniformityofaminopyrineandchlorphenaminemaleateinCompoundAmantadineAminopyrineTablets[J].ChineseDrugStandards,（inChinese）[17]沈曉燕,劉曉瑜,邱海強(qiáng).HPLC法測(cè)2021,40(03):171-175.DOSHENXiaoyan,LIUXiaoyu,QIUHaiqiang.DeterminationoffiveGanmaolingCapsulesbyHPLC[J].PharmaceuDOI:10.13506/ki.jpr.2021.03.007.（inChinese）[18]HassaniSAM.SimultaneousDeterminationofActiveOvertheCounterTabletsinthePresentofParabensand4-AminophenolbyHPLC[J].[19]AliA,UFarooq,AhmedM,determinationofchlorpheniraminemaleateandprednisoloneinveterinaryinjection[J].ActaChromatographica,2019,[20]ZhaoS,LiD,QiuJ,etal.Simultaneousdechlorpheniramineinanimal-derivedfoodbyliquidchromatography-tafterfastsamplepr[21]孫會(huì)會(huì),袁明俊,杜鴻雁,等.超快速液相色譜-事技術(shù),2020,45(01):55-59.DOI:10.16467/j.1008-3650.2020.SUNHuihui,YUANMingjun,DUHongyan,etal.DeterminationofChlorphHumanPlasmabyUltraFastLiquidChromatography-TandemMassSpeTechnology,2020,45(01):55-59.DOI:10.16467/j.1008-3650.2020.01.011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