饲料中溴苯那敏和氯苯那敏的测定 液相色谱-串联质谱法 编制说明

2《饲料中氯苯那敏和溴苯那敏的测定液相色谱-串联质谱法》一、工作简况3定性定量分析.方法血液经过乙腈沉淀蛋白后,振荡,离心,过0.2LC-MS/MS分析,采用多反应监测模式。但缺乏饲料中氯苯那敏和NNChemicalFormula:C16H19ClN2MolecularWeight:274.8ChlorphenamineNNChemicalFormula:C16H19BrN2MolecularWeight:319.2brompheniramine)图1.氯苯那敏和溴苯那敏的化学结构4成立了标准工作小组，进行标准的研制及起草工作，具体工色谱—质谱联用仪的仪器参数进行研究，对方法的试验条件、主要技术指标等进行进一混合饲料以及牛的精料补充料中氯苯那敏和溴二、标准编制原则和主要技术内容确定的依据5本文件规定了饲料中氯苯那敏和溴苯那敏的进行质谱条件的优化。通过一级全扫描质谱得到氯表1溴苯那敏和氯苯那敏的质谱条件药物名称Drug出峰时间Time(min)离子对Ionpairs(m/z)去簇电压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色谱柱和流动相的组成的选择6进行比较。结果表明采用BEHC18色谱柱时，梯度淋洗。发现氯苯那敏和溴苯那敏在C18色表2流动相梯度条件时间(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提取条件的优化和确定图3氯苯那敏和溴苯那敏提取效果图882.3.4净化条件的优化和确定910mL加入小柱内，待样液全部流出后，再加入3mL水清洗小柱，然后用3mL甲醇淋洗小柱，最后MCX用3mL5%氨水甲醇洗脱，MAX用3mL甲酸甲醇洗脱，C18、HLB小柱用3图4不同固相萃取对净化效果表3固相萃取柱容量考察结果样至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甲醇液质检测具有高灵敏度和高选择性的同时也存在基质效应，不同饲3.2稳定性考察2.3.7标准溶液有效期实验图5氯苯那敏和溴苯那敏标准储备液保存期实验2.4.1线性方程和线性范围表4氯苯那敏和溴苯那敏线性方程33图6空白鸡配合饲料色谱图图7鸡配合饲料阳性添加（添加浓度10ng/g）色谱图图8鸡空白预混合饲料色谱图图9鸡预混合饲料阳性添加（添加浓度10μg/kg）色谱图图10空白鸡浓缩饲料色谱图图11鸡浓缩饲料阳性添加（添加浓度10μg/kg）色谱图图12空白猪配合饲料色谱图图13猪配合饲料阳性添加（添加浓度10μg/kg）色谱图图14空白猪预混合饲料色谱图图15猪预混合饲料阳性添加（添加浓度10μg/kg）色谱图图16空白奶牛精料补充料色谱图图17奶牛精料补充料阳性添加（添加浓度10μg/kg）色谱图图18玉米载体空白色谱图图19玉米载体阳性添加（添加浓度10μg/kg）色谱图图20石粉载体空白色谱图图21石粉载体阳性添加（添加浓度10μg/kg）色谱图2.5方法的回收率和重现性（%）（%）（%）（%）（%）（%）（%）（%）（%）（%）（%）（%）（%）（%）2022年4月，标准编制小组委托广西饲料检测料中氯苯那敏和溴苯那敏的测定》规定的方法能满足饲料中氯苯那敏和溴苯那敏的测定要求，六、与有关法律、法规的关系七、重大分歧意见的处理经过和依据对标准的《征求意见稿》进行修改，无重大八、涉及专利的有关说明九、贯彻国家标准的要求，以及组织措施、技术措施、过渡期和实施日期的建议等措施建议无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]刘芳,高登慧,欧德渊,等.两种组胺受体拮抗剂对高致病性猪蓝耳病临床症状的影响[J].LiuFang,GaoDenghui,OuDeyuan,etal.EffectsofTwoHistamiClinicalSymptomsofHighlyPathogenicPorcineReproductiveandResSyndrome(PRRS)[J].GuizhouAnimalHusbandryandVeterinary,20[6]张楚珺,欧德渊,姚红艳,等.组胺受体拮抗剂对低致病性禽流感患鸡血液指标的影响[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）物残留[J].农产品加工,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]刘凯双,闫研,殷果,等.HPLC法同时测定复方金DOI:10.19778/j.chp.2021.LIUKaishuang,YANYan,YINGuo,etal.HPLCdeterminatiuniformityofaminopyrineandchlorphenaminemaleateinCompoundAmantadineAminopyrineTablets[J].ChineseDrugStandards,（inChinese）[17]沈晓燕,刘晓瑜,邱海强.HPLC法测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]孙会会,袁明俊,杜鸿雁,等.超快速液相色谱-事技术,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.（inChinese）[22]IoutsiAN,IoutsiVA,ShapovalovaEN,etal.DeterminationofPharmacologicallyActiveNitrogen-ContainingCompounSulphatebyHigh-PerformanceLiquidChromatography–ofAnalyticalChemistry,2020,75(7):930-935.[23]YanruLiu,BolinZhu,MengyaoXue,etal,StudiesitsenantioselectivepharmacokineticsinratplasmabyHPLC-MS/MS,MicrochemicalJo[24]HuiyaYuan,ShihuiYu,Guihoofthecysticfibrosistherapeuticdrugscolistin,ivacaftorandciprofloxacin[J].Journalof[25]LisaStrasser,GiorgioOliviero,CraigJakes,etal.DetectionandqunmonoclonalantibodydrugproductsusingautomatedsampleprtacquisitionLC-MS/MS[J].JournalofPharmaceuticalAnalysis[26]刘静,王震红,王晓黎,等.LC-MS快速检测降糖类中成药中14种非法添加化学药物中国现代应用药学,2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