DB43∕T 3265-2025 饲料中141种药物及化合物的快速测定 液相色谱串联质谱法

43Rapiddeterminationof141drI 5.2溶液配制 25.4标准溶液的配制 2 2 2 2 2 2 28.3标准曲线制备 38.4测定 38.5定性检测 48.6定量测定 48.7空白试验 4 4 5 5 5 5附录A（资料性）141种药物及化合 6本文件按照GB/T1.1—2020《标准化工作导则第1部分：标准化文件的结构和起草规则》的规定请注意本文件的某些内容可能涉及专利。本文件的发布机构不承担识别专利的责任。物机电职业技术学院、怀化职业技术学院、吐鲁忆文、张港、周玉洁、邓钧红、周汝顺、张瑞祺、西尔力•阿不都热哈曼、蒋小玲、刘干军、唐金花、1饲料中141种药物及化合物的快速测定液相色谱串联质谱法GB/T6682分析实验室用水规格GB/T20195动物饲料试样用甲酸乙腈水溶液提取，经净化包净化，5.2溶液配制5.2.20.1%甲酸乙腈复溶液（25.3标准品5.4标准溶液的配制5.4.3混合标准工作液：分别准确移取适量的混合标准中间液，用基质空白溶液稀释成系列标准工作5.5材料5.5.1净化包：100mg二氧化锆微球+100mg亲脂的二乙烯基苯和亲水的N-乙烯基吡咯烷酮聚合物。6.4涡旋混匀器。6.6氮吹仪。8.1提取），8.2净化38.3标准曲线制备精密移取混合标准中间液适量，分别加入6份经提取和净化的空白试液中，4为纵坐标，对应的标准溶液浓度为横坐标，绘制标准曲线，8.4测定a)色谱柱：C18（150mm×2.1mm，1.6μm），或者相e)流动相：A相为0.1%甲酸乙酸铵溶液，B相为乙腈，流A%B%3135533a)离子源：电喷雾离子源；b)扫描方式：正离子扫描/负离子扫描；d)定性定量离子对及去簇电压、碰撞能量4离子源雾化器温度(℃)8.5定性检测±20%±25%±30%±50%8.6定量测定9试验数据处理wf····························P——试样溶液待测化合物的质量浓度，单位为微克每升(μg/Lf——稀释倍数；wf··························································P——标准溶液中待测化合物的质量浓度，单位为微克每升(μg/L5f——稀释倍数；10.2准确度本方法在0.05mg/kg～1mg/kg10.3精密度本方法的批内相对标准偏差≤15%，批间相对标准偏6表A.1141种药物及化合物基本信息、质谱参数、类别中文名英文名化学文摘分子式溶剂母离子定量/定性离子扫描方式去簇V碰撞能量eV保留时间min定量限mg/kg兴奋剂氯丙那林clorprenaline3811-25-4CHClNO214.0154.1正离子73235.430.05118.07334硫酸特布他林Terbutalinehemisulfatesalt23031-32-5CHNOS226.0170.1正离子703.620.05152.07021妥布特罗Tulobuterol41570-61-0CHClNO228.0154.0正离子65216.080.05118.06535盐酸可乐定Clonidinehydrochloride4205-91-8CHClN230.0213.0正离子344.440.05160.145西布特罗Cimbuterol54239-39-3CHNO234.1160.1正离子324.160.05216.1321硫酸沙丁胺醇Salbutamolhemisulfatesalt51022-70-9CHNOS240.2148.1正离子70243.610.05222.170齐帕特罗（盐酸盐）Zilpaterolhydrochloride119520-05-7CHNO262.1244.1正离子463.660.05185.14633克伦普罗Clenproperol38339-11-6CHClNO263.1245.0正离子425.490.05203.04227酒石酸美托洛尔Metoprololtartrate56392-17-72CHNO·CHO268.2116.1*正离子78256.090.05191.17825克伦特罗ClenbuterolHydrochloride21898-19-1CHClNO277.0203.0*正离子65216.180.05168.16538盐酸利托君Ritodrinehydrochloride23239-51-2CHClNO288.1150.0正离子60274.470.05121.06030克伦潘特盐酸盐Clenpenterolhydrochloride37158-47-7CHClNO291.0203.0正离子50227.050.05132.05040盐酸羟甲基克伦特罗Hydroxymethylclenbuterolhydrochloride37162-89-3CHClNO293.1203.0正离子45265.230.05132.14540盐酸莱克多巴胺Ractopaminehydrochloride90274-24-1CHClNO302.2164.1正离子80235.340.05107.18051盐酸马布特罗Mabuterolhydrochloride54240-36-7CHClFNO·HCl311.1237.0正离子46247.140.05217.04634克伦塞罗Clencyclohexerol157877-79-7CH0ClNO319.1203.0正离子52274.860.05132.152467类别中文名英文名化学文摘分子式溶剂母离子定量/定性离子扫描方式去簇碰撞能量（eV）保留时间（min)定量限(mg/kg)兴奋剂盐酸溴代克伦特罗Bromchlorbuterolhydrochloride78982-84-0CHBrClNO323.0248.9正离子52256.470.05168.05239盐酸马贲特罗Mapenterolhydrochloride54238-51-6CHClFNO325.237.0正离子64237.980.05217.06435盐酸拉贝洛尔Labetalolhydrochloride32780-64-6CHClNO329.1162.0正离子48347.280.05294.14827苯乙醇胺AphenylethanolamineA1346746-81-3CHNO345.1150.1正离子90308.810.05327.290福莫特罗富马酸盐二水合物Formoterolfumaratedihydrate183814-30-4CHNO345.2121.0正离子66486.10.05149.16626溴布特罗Brombuterol41937-02-4CHBrNO367.0292.8正离子56276.750.05348.956盐酸班布特罗Bambuterolhydrochloride81732-46-9CHClNO368.2312.1正离子72206.860.05294.17227大环类维及霉素Virginiamycin11006-76-1CHNO526.2508.3正离子9010.970.1355.19025竹桃霉素Oleandomycin3922-90-5CHNO688.4158.2正离子30708.30.1544.33042红霉素Erythromycin114-07-8CHNO734.5576.4正离子30268.860.1158.03036克拉霉素Clarithromycin81103-11-9CHNO748.5590.4正离子402910.320.1158.04040交沙霉素Josamycin16846-24-5CHNO828.6174.1正离子703811.210.1109.07070罗红霉素Roxithromycin80214-83-1CHNO837.6679.5正离子503010.560.1158.15037螺旋霉素Spiramycin8025-81-8CHNO843.3142.2正离子60486.580.1174.26050替米考星tilmicosin108050-54-0CHNO869.5696.5正离子527.780.1174.252泰乐菌素tylosin1401-69-0CHNO916.6174.0正离子479.320.1772.543泰地罗新Tildipirosin328898-40-4CHNO734.5576.5正离子60268.990.1158.16036磺胺类磺胺醋酰Sulfacetamide144-80-9CHNOS215.0156.0正离子524.360.05108.05229磺胺脒sulfaguanidine57-67-0CHNOS215.192.0正离子60324.370.05108.060328类别中文名英文名化学文摘分子式溶剂母离子定量/定性离子扫描方式去簇碰撞能量（eV）保留时间（min)定量限(mg/kg)磺胺类磺胺吡啶Sulfapyridine144-83-2CHNOS250.1156.1正离子40236.820.05108.04032磺胺吡唑sulfapyrazole852-19-7CHNOS250.1184.0正离子55225.080.05156.05525磺胺嘧啶Sulfadiazine68-35-9CHNOS251.1156.0*正离子40224.740.0592.04038磺胺甲恶唑Sulfamethoxazole723-46-6CHNOS254.1156.0正离子65227.20.05108.06536磺胺噻唑Sulfathiazole72-14-0CHNOS256.0156.0正离子40224.880.05108.04032磺胺甲基嘧啶Sulfamerazine127-79-7CHNOS265.2156.1正离子82255.390.05172.18225磺胺异恶唑Sulfisoxazole127-69-5CHNOS268.1156.1正离子82227.580.05113.28225磺胺恶唑Sulfamoxol729-99-7CHNOS268.1156.1正离子82225.60.05113.28225磺胺甲噻二唑sulfamethizole144-82-1CHNOS271.0156.1正离子65215.870.05108.06536苯甲酰磺胺sulfabenzamide127-71-9CHNOS277.1156.0正离子608.20.05108.06032磺胺二甲异嘧啶sulfisomidine515-64-0CHNOS279.0124.1正离子80304.230.05186.08023磺胺二甲基嘧啶Sulfamethazine57-68-1CHNOS279.1156.0正离子60275.940.05186.16023磺胺间甲氧嘧啶sulfamonomethoxine1220-83-3CHNOS281.1156正离子75256.560.05126.17530磺胺氯吡嗪Sulfaclozine102-65-8CHClNOS285.092.0*正离子96418.380.05108.19635磺胺氯哒嗪sulfachloropyridazine80-32-0CHClNOS285.1156.0正离子65226.910.05108.16537磺胺喹恶啉sulfaquinoxaline59-40-5CHNOS301.1156正离子80248.660.05108.08036磺胺邻二甲氧嘧啶Sulfadoxine2447-57-6CHNOS311.1108.2正离子70377.270.05156.17030磺胺间二甲氧嘧啶Sulfadimethoxine122-11-2CHNOS311.1156.1正离子70288.590.05218.07028磺胺苯吡唑Sulfaphenazole526-08-9CHNOS315.0327.2正离子908.970.05156.090279类别中文名英文名化学文摘分子式溶剂母离子定量/定性离子扫描方式去簇碰撞能量（eV）保留时间（min)定量限(mg/kg)激素类泼尼松Prednisone53-03-2CHO乙腈359.2147.2正离子80358.80.1341.280可的松Cortisone53-06-5CHO乙腈361.2163.2正离子80348.990.1121.18047泼尼松龙Prednisolone50-24-8CHO乙腈361.2343.2正离子808.750.1147.28034氢化可的松Hydrocortisone50-23-7CHO乙腈363.2121.1正离子80318.870.1105.08068甲基泼尼松龙Methylprednisolone83-43-2CHO乙腈375.2339.2*正离子669.740.1161.26628氟米龙Fluorometholone426-13-1CHFO乙腈377.2279.3正离子802211.120.1321.380倍氯米松Beclomethasone4419-39-0CHClO乙腈409.2391.2正离子8010.320.1279.38029氟米松Flumethasone2135-17-3CHFO乙腈411.3253.2正离子80229.970.1121.08050醋酸氟氢可的松Fludrocortisone21-acetate514-36-3CHFO乙腈423.2239.2正离子803411.170.1343.28031氟氢缩松Flurandrenorlide1524-88-5CHFO乙腈437.3361.2正离子802410.860.1285.28029地夫可特Deflazacort14484-47-0CHNO乙腈442.3124.1正离子806511.380.1142.18045曲安西龙双醋酸酯Triamcinolonediacetate67-78-7CHFO乙腈479.2441.2正离子8110.860.1147.08148驱虫类氯羟吡啶Clopidol2971-90-6CHClNO192.2100.9正离子80354.550.186.98042二硝托胺Dinitolmide148-01-6CHNO226.0139.0正离子80256.510.167.08040乙氧酰胺苯甲酯Ethopabate59-06-3CHNO238.1206.0正离子60208.440.1136.06030噻苯哒唑Thiabendazole148-79-8CHNS202.2175.0正离子60375.010.1130.96048左旋咪唑盐酸盐Levamisolehydrochloride16595-80-5CHClNS205.1178.0正离子314.670.191.046替硝唑Tinidazole19387-91-8CHNOS248.2121.2正离子80215.550.193.08025奥芬达唑Oxfendazole53716-50-0CHNOS316.2159.0正离子70437.750.1191.17027类别中文名英文名化学文摘分子式溶剂母离子定量/定性离子扫描方式去簇碰撞能量（eV）保留时间（min)定量限(mg/kg)驱虫类阿普西特Arprinocide55779-18-5CHClFN278.1143.1正离子347.350.1107.079二甲硝咪唑dimetridazole551-92-8CHNO142.296.0正离子65214.960.181.06536异丙硝唑ipronidazole14885-29-1CHNO170.3124.0正离子50257.910.1109.05033甲硝唑metronidazole443-48-1CHNO172.2127.9正离子50204.190.182.05037罗硝唑ronidazole7681-76-7C6HNO201.2140.0正离子504.510.155.05027奥硝唑Ornidazole16773-42-5CHClNO220.0128.0正离子70236.270.182.07043抗病毒类奥司他韦oseltamivir196618-13-0CHNO乙腈313.1166.0正离子307.490.05225.120金刚烷胺Amantadine768-94-5CHN152.1135*正离子70255.10.0593.07038四环素类强力霉素单盐酸半乙醇半水合物Doxycyclinehyclate24390-14-5CHClNO445.0428.1正离子80247.450.1154.18035盐酸四环素Tetracyclinehydrochloride64-75-5CHClNO445.1410.2正离子80245.690.1427.180土霉素Oxytetracycline79-57-2CHNO461.2426.2正离子80255.160.1443.280盐酸金霉素Chlortetracyclinehydrochloride64-72-2CHClNO479.1462.0正离子80246.380.1444.08028喹诺酮类萘啶酸Nalidixicacid389-08-2CHNO233.0215.0正离子689.70.05187.06834恶喹酸Oxolinicacid14698-29-4CHNO262.0244.1正离子70268.10.05216.17040氟甲喹Flumequine42835-25-6CHFNO262.1244.1正离子772310.040.05202.17742诺氟沙星Norfloxacin70458-96-7CHFNO320.1276.1正离子80265.150.05233.18035依诺沙星Enoxacin74011-58-8CHFNO321.0303.0正离子80244.910.05234.08030环丙沙星Ciprofloxacin85721-33-1CHFNO332.1288.1正离子80355.320.05245.18033类别中文名英文名化学文摘分子式溶剂母离子定量/定性离子扫描方式去簇碰撞能量（eV）保留时间（min)定量限(mg/kg)喹诺酮类培氟沙星（甲磺酸）Pefloxacinmesylate70458-95-6CHFNOS334.1316.1正离子80275.280.05290.28025洛美沙星（盐酸盐）Lomefloxacinhydrochloride98079-52-8CHClFNO352.0265.0正离子80335.560.05308.18028达氟沙星Danofloxacin112398-08-0CHFNO358.1340.1正离子77305.560.05314.17724恩诺沙星Enrofloxacin93106-60-6CHFNO360.0316.1正离子80255.790.05245.18035那氟沙星Nadifloxacin124858-35-1CHFNO361.2283.1*正离子539.770.05257.054氧氟沙星Ofloxacin82419-36-1CHFNO362.2318.1正离子80265.220.05261.18038马波沙星Marbofloxacin115550-35-1CHFNOS363.1320.1正离子80234.980.0572.08046氟罗沙星Fleroxacin79660-72-3CHFNO370.0326.1正离子80275.20.05269.28035沙拉沙星Sarafloxacin98105-99-8CHFNO386.0342.3正离子80256.380.05299.08038司帕沙星Sparfloxacin110871-86-8CHFNO393.0349.2正离子80306.560.05292.08038奥比沙星Orbifloxacin113617-63-3CHFNO396.0352.0正离子80245.960.05295.28032双氟沙星（盐酸盐）Difluoxacinhydrochloride91296-86-5CHClFNO400.1356.1正离子80286.520.05299.18041青霉素及头孢类阿莫西林Amoxicillin26787-78-0CHNOS乙腈/水（1：3）366.2349.1正离子466.570.1114.14630头孢氨苄Cephalexin15686-71-2CHNOS乙腈/水（1：3）348.0157.9正离子554.490.1174.05521头孢拉定Cefradine38821-53-3CHNOS乙腈/水（1：3）350.0175.9正离子554.810.1157.955头孢羟氨苄Cefadroxil50370-12-2CHNOS乙腈/水（1：3）364.0114.0正离子40253.640.1208.040头孢克洛Cefaclor53994-73-3CHClNOS乙腈/水（1：3）367.9174.0正离子554.020.1105.95527头孢匹林钠Cefapirinsodium24356-60-3CHNNaOS乙腈/水（1：3）424.1292.0正离子45213.820.1152.04529头孢唑啉Cefazolin25953-19-9CHNOS乙腈/水（1：3）454.9323.0正离子605.420.1155.86021类别中文名英文名化学文摘分子式溶剂母离子定量/定性离子扫描方式去簇碰撞能量（eV）保留时间（min)定量限(mg/kg)青霉素及头孢类头孢噻肟Cefotaxime63527-52-6CHNOS乙腈/水（1：3）456.0166.9正离子66285.030.1125.06670头孢孟多钠Sodiumcefamandole30034-03-8CHNNaOS乙腈/水（1：3）463.0347.0正离子706.970.1158.17023头孢匹罗Cefpirome84957-29-9CHNOS乙腈/水（1：3）515.0119.9正离子70214.140.1167.07033头孢噻呋Ceftiofur80370-57-6CHNOS乙腈/水（1：3）524.0241.0正离子60237.930.1124.86080头孢喹肟（硫酸盐）Cefquinomesulfate118443-89-3CHNOSHOS乙腈/水（1：3）529.0134.0正离子604.60.1396.060头孢他啶Ceftazidime72558-82-8CHNOS乙腈/水（1：3）547.0467.8正离子603.90.1166.96034头孢哌酮钠Cefoperazonesodium62893-20-3CHNNaOS乙腈/水（1：3）646.4143.0正离子70386.550.1530.270农药灭蝇胺Cyromazine66215-27-8CHN乙腈/水（1：3）167.1125.0正离子60243.450.185.06024敌菌净Diaveridine5355-16-8CHNO261.0245.0正离子90354.640.1123.09031增效剂甲氧苄氨嘧啶trimethoprim738-70-5CHNO291.1230.1正离子95334.980.05123.19534酰胺醇类氯霉素Chloramphenicol56-75-7CHClNO321.0152.1正离子75247.740.05256.975甲砜霉素Thiamphenicol15318-45-3CHClNOS353.9289.9正离子755.430.05184.97528氟苯尼考Florfenicol73231-34-2CHClFNOS356.0119.0正离子80237.210.05184.980解热镇痛类非那西丁Phenacetin62-44-2CHNO180.1138.0正离子71217.850.1110.071274-异丙基氨基安替比林4-Isopr