飼料中慶大霉素的測(cè)定 液相色譜-串聯(lián)質(zhì)譜法 編制說(shuō)明

1 1 1 5 7 7 7 7 9 11 12 14 15 15 16 17 172.3.1檢出限（LOD）與定量限（ 17 17 18 19 31三、試驗(yàn)驗(yàn)證的分析、綜述報(bào)告，技術(shù)經(jīng)濟(jì)論證，預(yù)期的經(jīng)濟(jì) 31四、與國(guó)內(nèi)、國(guó)際、國(guó)外同類標(biāo)準(zhǔn)技術(shù)內(nèi)容的對(duì)比情況，或者與測(cè)試的國(guó)機(jī)的有關(guān)數(shù)據(jù)對(duì)比情況 32 32 32 32 32 331根據(jù)《國(guó)家標(biāo)準(zhǔn)化管理委員會(huì)關(guān)于下達(dá)2021年第四批推薦性國(guó)家標(biāo)準(zhǔn)計(jì)按無(wú)水物計(jì)算，每1mg的效價(jià)不得少于590慶大449.5（C1a463.6（C2+C2a）。是由小單孢子屬產(chǎn)生的多組分氨基糖苷類療效和毒理也存在差異：C1組份毒理副作用較小，也不容易產(chǎn)生抗藥性，在23少網(wǎng)絡(luò)上報(bào)道加入飼料中用于預(yù)防和治療疾??；根據(jù)相關(guān)資料，一般慶大霉在人類正常生理pH值時(shí)，慶大霉素中游離的正電荷氨基基團(tuán)和腎臟中腎小管上皮細(xì)胞或毛細(xì)胞表面的特異性受體結(jié)合→自由氨基基團(tuán)和結(jié)合的受體合成，導(dǎo)致細(xì)胞代謝障礙，結(jié)構(gòu)破壞。慶大農(nóng)業(yè)部出臺(tái)了一系列公告禁止抗生素在飼料中的使用，并于2019年發(fā)布1944號(hào)公告，規(guī)定自2020年起，飼料生產(chǎn)企業(yè)停止生產(chǎn)含有促生長(zhǎng)類藥物飼料添然而慶大霉素在飼料中非法添加和外源污染問(wèn)題時(shí)有發(fā)生，對(duì)飼料工業(yè)發(fā)展、用的獸藥之一，但由于其毒性，我國(guó)在GB31650-2019《食品安全國(guó)家標(biāo)準(zhǔn)食目前關(guān)于慶大霉素檢測(cè)標(biāo)準(zhǔn)則有“GB/T21329-2007動(dòng)物源性食品中慶大留檢測(cè)高效液相色譜法”以及“GBT21323-2007動(dòng)物組織中氨基糖苷類藥物殘留量的測(cè)定高效液相色譜-質(zhì)譜/質(zhì)譜法”等，不少學(xué)者也建立不同的慶大霉素譜分析方法無(wú)法準(zhǔn)確測(cè)定慶大霉素各組分的含量。因此液相色譜-串聯(lián)質(zhì)譜法如DavidN.Heller等人在2005年開(kāi)發(fā)并驗(yàn)證了幾種牛組織中慶大霉素濃度的5析方法，方法檢出限為10μg/kg，本標(biāo)準(zhǔn)旨在建立一種能同時(shí)提取并凈化飼料中慶大霉素的前處理方法及表1標(biāo)準(zhǔn)主要起草人員和任務(wù)分工任務(wù)分工項(xiàng)目主持人，負(fù)責(zé)項(xiàng)目的全面工作檢測(cè)方法研究，標(biāo)準(zhǔn)文本和編制說(shuō)明編寫(xiě)和完善、方法驗(yàn)證實(shí)施方案制定，標(biāo)準(zhǔn)文本和編制說(shuō)明編寫(xiě)和完善、征求意見(jiàn)樣品檢測(cè)、數(shù)據(jù)收集分析樣品采集、數(shù)據(jù)收集分析標(biāo)準(zhǔn)文本和編制說(shuō)明編寫(xiě)和完善、征求意見(jiàn)樣品采集、標(biāo)準(zhǔn)文本和編制說(shuō)明編寫(xiě)和完善標(biāo)準(zhǔn)文本和編制說(shuō)明編寫(xiě)和完善6容和技術(shù)路線草案，確定標(biāo)準(zhǔn)修訂的主要內(nèi)容、技術(shù)路線（見(jiàn)圖2）、LC-MS/MS方法研究、方法比較形成標(biāo)準(zhǔn)征求意見(jiàn)稿和編制說(shuō)明形成標(biāo)準(zhǔn)征求意見(jiàn)稿和編制說(shuō)明標(biāo)準(zhǔn)的預(yù)審、終審和報(bào)批1.3.3樣品收集、方法學(xué)研究和實(shí)際樣1.3.4編寫(xiě)編制說(shuō)明和征求意見(jiàn)稿、定向征求意見(jiàn)和標(biāo)準(zhǔn)驗(yàn)證7二、標(biāo)準(zhǔn)編制原則和主要技術(shù)內(nèi)容確定的依據(jù)（1）遵循國(guó)家頒布的相關(guān)法律法規(guī)；（2）有關(guān)國(guó)家或行業(yè)標(biāo)準(zhǔn)；（3）國(guó)內(nèi)外有關(guān)標(biāo)準(zhǔn)和參考文獻(xiàn)；（4）標(biāo)準(zhǔn)編制小組調(diào)研和實(shí)測(cè)的樣品檢測(cè)數(shù)據(jù)。2.2主要技術(shù)內(nèi)容確定的依據(jù)2.2.1質(zhì)譜條件的選擇和優(yōu)化89母離子子離子去簇電壓（V）碰撞能量（eV）慶大霉素C1a450.2322.1*20慶大霉素C2+C2a464.2322.1*2025慶大霉素C1478.2322.1*25注：*為定量離子。2.2.2色譜條件的選擇和優(yōu)化過(guò)對(duì)出峰時(shí)間、分離效果、峰形和靈敏度等因素分別考察了0.1%甲酸溶液圖4不同流動(dòng)相的慶大霉素C1MRM色譜圖），），05582.2.3不同濃度七氟丁酸甲醋酸溶液的比較0.85min、0.81min、0.81min；0.82min、0.81min、0.81min；分離度較差。分進(jìn)行測(cè)定的方法[13]；也有利用2%三氯乙酸溶液對(duì)慶大霉素提取，用NaOH則有利用3%三氯乙酸溶液提取，SCX柱凈化后使用LC-MS進(jìn)行測(cè)定；利用5%三氯乙酸進(jìn)行提取，用HLB柱凈化后利用LC-MS進(jìn)行測(cè)定。慶大霉素常較，用氫氧化鈉和乙腈提取慶大霉素樣品時(shí)需要調(diào)pH到酸取慶大霉素的常用提取液，根據(jù)樣品成分復(fù)雜情況，常用的濃度一般為2%~洗固相萃取柱，最后PCX、MCX用3mL10%氨水甲醇溶液洗脫，加入3mL從圖8可以看出，經(jīng)過(guò)PCX固相萃取柱凈化后，飼料中2.2.6洗脫試劑的選擇和優(yōu)化本試驗(yàn)研究了不同比例的氨水甲醇對(duì)慶大霉素的洗脫效果，按照上述操作，洗脫時(shí)用不同比例的氨水甲醇進(jìn)行洗脫，最終上機(jī)檢測(cè)，結(jié)2.2.7洗脫溶液用量的選擇和優(yōu)化洗脫溶劑用量的選擇是一個(gè)關(guān)鍵參數(shù)，因此，試驗(yàn)評(píng)估了1.0mL~5.02.2.8標(biāo)準(zhǔn)儲(chǔ)備溶液穩(wěn)定性考察2.2.9樣品提取和凈化方法脫，收集洗脫液于10mL塑料離心管中，于40℃下用mL1%七氟丁酸甲酸溶液復(fù)溶，充分渦旋，用0.22μm濾膜過(guò)濾，濾液裝塑料2.3.1檢出限（LOD）與定量限（LOQ）的確定在空白基質(zhì)中添加一定量的慶大霉素標(biāo)準(zhǔn)品，樣品經(jīng)前處理后，用大霉素的濃度即為檢出限，樣品中慶大霉素的峰的信噪比大于等于10時(shí)，添加慶大霉素的濃度即為定量限。該慶大霉素分析方法對(duì)飼料的檢測(cè)限0.05共46.8%）各組分所占的比例，所以慶大霉素組分C1、C（90∶10，v/v）溶液配制的標(biāo)準(zhǔn)溶液對(duì)比，結(jié)果見(jiàn)圖11。慶大霉素表現(xiàn)為基由低到高濃度的基質(zhì)標(biāo)準(zhǔn)溶液，其質(zhì)量濃度分別為5ng/mL、10ng/mL、50量離子色譜峰面積與基質(zhì)添加標(biāo)準(zhǔn)溶液濃度作標(biāo)準(zhǔn)曲線。結(jié)果見(jiàn)表5?；|(zhì)添表5基質(zhì)添加標(biāo)準(zhǔn)曲線的線性方程和相關(guān)系數(shù)2.3.4準(zhǔn)確度和精密度考察表6豬配合飼料中慶大霉素的添加回收率、批內(nèi)和批間精密度(mg/kg)測(cè)定批次回收率(%)平均回(%)批內(nèi)RSD(%)批間RSD(%)Ⅰ83.481.282.00.942.18Ⅱ82.377.883.981.577.480.62.87Ⅲ82.682.384.283.978.382.22.350.2Ⅰ80.582.292.980.680.683.35.364.75Ⅱ77.283.079.892.483.55.82Ⅲ77.878.883.885.979.581.23.4925Ⅰ84.384.885.985.584.385.00.702.23Ⅱ84.085.883.583.583.90.94Ⅲ86.389.885.590.83.20Ⅰ79.589.880.389.379.083.65.464.60Ⅱ79.486.779.282.979.281.53.31Ⅲ83.291.077.278.083.382.55.50表7豬濃縮飼料中慶大霉素的添加回收率、批內(nèi)和批間精密度(mg/kg)測(cè)定批次回收率(%)平均回(%)批內(nèi)RSD(%)Ⅰ80.880.680.292.482.283.25.15Ⅱ78.379.683.982.477.980.42.64Ⅲ67.981.385.977.883.779.37.040.2Ⅰ80.967.582.080.885.979.47.00Ⅱ82.285.485.267.980.47.22Ⅲ92.992.962.982.867.679.8Ⅰ79.977.378.080.482.679.62.08Ⅱ81.878.083.482.379.9Ⅲ82.883.378.880.082.681.5Ⅰ82.978.081.578.680.82.41Ⅱ82.877.879.577.882.62.47Ⅲ80.679.379.383.880.980.8表8豬預(yù)混料中慶大霉素的添加回收率、批內(nèi)和批間精密度(mg/kg)測(cè)定批次回收率(%)平均回(%)批內(nèi)RSD(%)批間RSD(%)Ⅰ78.085.379.178.880.32.915.55Ⅱ94.087.289.590.680.088.35.23Ⅲ93.888.387.983.090.488.73.960.2Ⅰ79.985.862.878.99.267.67Ⅱ83.682.983.080.382.0Ⅲ92.392.280.383.867.483.2500Ⅰ67.179.862.867.385.372.59.618.72Ⅱ82.881.385.392.585.44.31Ⅲ83.892.579.983.984.084.84.645000Ⅰ79.692.883.681.267.981.08.956.20ⅡⅢ表9雞配合飼料中慶大霉素的添加回收率、批內(nèi)和批間精密度(mg/kg)測(cè)定批次回收率(%)平均回(%)批內(nèi)RSD(%)批間RSD(%)Ⅰ78.890.183.885.684.34.10Ⅱ85.294.991.877.991.488.26.77Ⅲ82.687.282.978.283.2Ⅰ92.880.086.297.184.888.26.796.79Ⅱ86.884.977.877.15.42Ⅲ85.887.387.081.688.87.86Ⅰ96.886.096.097.281.64Ⅱ77.080.378.083.580.22.70Ⅲ77.878.284.081.080.82.79Ⅰ96.398.299.884.385.092.77.488.62Ⅱ80.382.386.281.583.382.72.24Ⅲ80.578.877.867.177.476.35.28表10雞預(yù)混料中慶大霉素的添加回收率、批內(nèi)和批間精密度(mg/kg)測(cè)定批次回收率(%)平均回(%)批內(nèi)RSD(%)批間RSD(%)Ⅰ77.892.882.085.684.35.556.49Ⅱ92.980.692.680.867.983.0Ⅲ81.080.879.879.482.680.70.2Ⅰ80.482.385.481.892.984.65.025.78Ⅱ67.892.285.280.981.28.90Ⅲ85.381.279.483.982.882.52.31Ⅰ81.887.682.678.981.30Ⅱ82.480.382.281.281.40.86Ⅲ84.381.383.380.882.52000Ⅰ82.983.481.492.279.083.85.01Ⅱ85.982.2Ⅲ85.862.362.592.277.6表11魚(yú)配合飼料中慶大霉素的添加回收率、批內(nèi)和批間精密度(mg/kg)測(cè)定批次回收率(%)平均回(%)批內(nèi)RSD(%)批間RSD(%)Ⅰ78.082.079.21Ⅱ83.480.979.486.980.582.23.02Ⅲ80.283.883.278.078.980.82.600.2Ⅰ80.281.579.097.683.884.47.596.50Ⅱ82.880.478.079.677.379.62.17Ⅲ82.592.382.997.183.587.76.6820Ⅰ77.180.878.877.078.8Ⅱ81.879.481.380.579.880.6Ⅲ79.980.082.585.282.82.21200Ⅰ81.481.478.378.581.580.25.53Ⅱ83.898.877.583.479.384.68.42Ⅲ82.491.686.082.982.085.04.01表12魚(yú)濃縮飼料中慶大霉素的添加回收率、批內(nèi)和批間精密度(mg/kg)測(cè)定批次回收率(%)平均回(%)批內(nèi)RSD(%)批間RSD(%)Ⅰ76.0271.0572.9774.0973.1673.462.465.67Ⅱ83.3780.6879.3686.9180.4882.163.69Ⅲ80.2074.7174.2175.9678.8876.793.430.2Ⅰ69.2172.5376.9667.6274.7372.215.324.98Ⅱ71.8269.4178.0273.5575.3073.624.46Ⅲ82.4866.3371.8967.1374.4682.064.81Ⅰ75.0569.7978.8477.0473.975.866.54Ⅱ81.7673.3881.3080.5079.8279.354.31Ⅲ73.9269.0282.5268.2371.7382.683.19Ⅰ81.3981.4076.3478.4781.5479.832.935.46Ⅱ74.6378.6475.4974.3879.2776.483.01Ⅲ71.4172.6068.9971.9471.0371.19表13精料補(bǔ)充料中慶大霉素添加回收率、批內(nèi)和批間精密度(mg/kg)測(cè)定批次回收率(%)平均回(%)批內(nèi)RSD(%)批間RSD(%)Ⅰ83.280.467.879.292.280.68.745.26Ⅱ78.577.985.478.077.279.43.38Ⅲ79.182.084.979.877.980.72.750.2Ⅰ79.885.267.867.681.48Ⅱ81.582.582.486.085.983.7Ⅲ83.291.979.491.277.884.76.57Ⅰ81.579.985.285.892.885.04.983.74Ⅱ80.878.083.585.482.582.02.81Ⅲ78.180.885.585.384.082.83.19200Ⅰ81.580.280.967.965.58Ⅱ79.279.377.981.079.279.3Ⅲ91.380.381.877.678.381.95.53圖13豬配合飼料添加樣品特征離子色譜圖圖14豬濃縮飼料空白樣品特征離子色譜圖圖15豬濃縮飼料添加樣品特征離子色譜圖圖16豬豬預(yù)混料空白樣品特征離子色譜圖圖17豬豬預(yù)混料添加樣品特征離子色譜圖圖18雞配合飼料空白樣品特征離子色譜圖圖19雞配合飼料添加樣品特征離子色譜圖圖20雞預(yù)混料空白樣品特征離子色譜圖圖21雞預(yù)混料添加樣品特征離子色譜圖圖22魚(yú)配合飼料空白樣品特征離子色譜圖圖23魚(yú)配合飼料肪添加樣品特征離子色譜圖圖24魚(yú)濃縮飼料空白樣品特征離子色譜圖圖25魚(yú)濃縮飼料添加樣品特征離子色譜圖圖26精料補(bǔ)充料空白樣品特征離子色譜圖圖27精料補(bǔ)充料添加樣品特征離子色譜圖條件下獲得的三次獨(dú)立結(jié)果的相對(duì)偏差值均不超過(guò)20%，符合本標(biāo)準(zhǔn)研究需以上結(jié)果表明，本標(biāo)準(zhǔn)建立的飼料中慶大霉素的超高效液相色譜-串聯(lián)質(zhì)還是慶大霉素總含量，該方法都能夠滿足飼三、試驗(yàn)驗(yàn)證的分析、綜述報(bào)告，技術(shù)經(jīng)濟(jì)論證，預(yù)期的經(jīng)濟(jì)效果外樣品、樣機(jī)的有關(guān)數(shù)據(jù)對(duì)比情況五、采標(biāo)情況，以及是否合規(guī)引用或采用國(guó)際國(guó)外標(biāo)準(zhǔn)七、重大分歧意見(jiàn)的處理經(jīng)過(guò)和依據(jù)八、涉及專利的有關(guān)說(shuō)明（1）首先應(yīng)在實(shí)施前保證文本的充足供應(yīng)，讓每個(gè)使用者都能及時(shí)得到（2）發(fā)布后、實(shí)施前應(yīng)將信息在媒體上廣為宣傳，建議全國(guó)飼料工業(yè)標(biāo)[1]Gentamicin.(WHOFoodAdditivesSeries41).[2]JaoRL,JacksonGG.GentamicinSulfate,NewAntibioticagainstGram-NegativeBacilli[J].JAMA,1964,189:817–822.[3]McKellarQ1Antimicrobialresistance:Aveterinaryperspective[J].BMJ,1998,317:610–611.[4]RosenkrantzBE,GrecoJR,HoogerheideJG,etal.GentamicinSulfate[J].AnalyticalProfilesofDrugSubstances,1981,9:295–340.[5]謝桂芬.慶大霉素在豬病防治中的使用[J].現(xiàn)代農(nóng)業(yè)科技,2008(19):302-304.XieGF.Applicationofgentamicininpreventionandtreatmentofpigdisease[J].ModernAgriculturalScienceandTechnology,2008(19)：302-304.(inChinese)[6]羅文柳.慶大霉素在獸醫(yī)臨床中的應(yīng)用[J].獸醫(yī)導(dǎo)刊,2020(13):106.LuoWL.Applicationofgentamicininveterinaryclinic[J].VeterinaryGuide,2020(13):106.(inChinese)[7]田強(qiáng)兵,巨歡,任惠麗,等.高效液相色譜-質(zhì)譜法測(cè)定魚(yú)肉中慶大霉素主要組分C1、C1a、C2[J].理化檢驗(yàn)(化學(xué)分冊(cè)),2019,55(01):97-100.TianQB,JuH,RenHL,etal.DeterminationofgentamicincomponentsC1,C1aandC2infishmeatbyhighperformanceliquidchromatography-massspectrometry[J].PhysicalandChemicalExamination(ChemistryBranch),2019,55(01):97-100.(inChinese)[8]PourfeiziHH,SalehP,AbbasalizadehS,etal.Gentamicin-mediatedototoxicityandnephrotoxicity:Aclinicaltrialstudy[J].NigerianMedicalJournal,2016,57(6):347–352.[9]李福剛,袁玉國(guó).致病性大腸桿菌對(duì)慶大霉素的耐藥性研究[J].江西畜牧獸醫(yī)雜志,2002(01)：6-8.LiFG,YuanYG.StudyonresistanceofpathogenicEscherichiacolitogentamicin[J].JiangxiJournalofAnimalHusbandryandVeterinaryMedicine,2002(01):6-8.(inChinese)[10]王秀英.禽大腸桿菌對(duì)慶大霉素的耐藥性誘導(dǎo)試驗(yàn)[J].中國(guó)畜禽種業(yè),2019,15(09):191.WangXY.InductionofresistancetogentamicininavianEscherichiacoli[J].ChineseJournalofLivestockandPoultryBreeding,2019,15(09):191.(inChinese)[11]中華人民共和國(guó)農(nóng)業(yè)部公告第1519號(hào),禁止在飼料和動(dòng)物飲水中使用的物質(zhì)[EB/OL].2010.中華人民共和國(guó)農(nóng)業(yè)部公告第1519號(hào)()AnnouncementNo.1519oftheMinistryofAgricultureofthePeople'sRepublicofChina,Substancesprohibitedinfeedandanimaldrinkingwater[EB/OL].2010.AnnouncementNo.1519oftheMinistryofAgricultureofthePeople'sRepublicofChina().(inChinese)[12]中華人民共和國(guó)農(nóng)業(yè)農(nóng)村部公告第194號(hào),發(fā)布藥物飼料添加劑退出計(jì)劃和相關(guān)管理政策[EB/OL].2019.中華人民共和國(guó)農(nóng)業(yè)農(nóng)村部公告第194號(hào)()MinistryofAgricultureandRuralAffairsofthePeople'sRepublicofChinaAnnouncementNo.194,Releaseofdrugfeedadditiveswithdrawalplanandrelatedmanagementpolicies[EB/OL].2019.AnnouncementNo.194oftheMinistryofAgricultureandRuralAffairsofthePeople'sRepublicofChina().(inChinese)[13]農(nóng)業(yè)農(nóng)村部畜牧獸醫(yī)局，農(nóng)業(yè)農(nóng)村部畜牧獸醫(yī)局關(guān)于2020年全國(guó)飼料質(zhì)量安全監(jiān)督抽查結(jié)果的通報(bào)[EB/OL].中華人民共和國(guó)農(nóng)業(yè)農(nóng)村部公報(bào),2021(02)：122-123./nybgb/2021/202102/202110/t20211008_6378916.htmMinistryofAgricultureandRuralAffairsAnimalHusbandryandVeterinaryBureau,MinistryofAgricultureandRuralAffairsAnimalHusbandryandVeterinaryBureauon2020nationalfeedqualityandsafetysupervisionresultsNotice[EB/OL].TheagriculturalNongCunBucommuniqueofthePeople'sRepublicofChina,2021(02)：122-123./nybgb/2021/202102/202110/t20211008_6378916.htm.(inChinese)[14]TangSP,CanfarottaF,Smolinska-KempistyK,etal.Apseudo-ELISAbasedonmolecularlyimprintednanoparticlesfordetectionofgentamicininrealsamples[J].AnalyticalMethods,2017,9(19)：2853-285[15]XiaY,SuR,HuangR,etal.Designofelutionstrategyforsimultaneousdetectionofchloramphenicolandgentamicinincomplexsamplesusingsurfaceplasmonresonance[J].BiosensorsandBioelectronics,2017,92：266–272.[16]WuSM,YanCX,FanXH,etal.Developmentofenzyme-linkedimmunosorbentassayandcolloidalgold-basedimmunochromatographicassayfortherapiddetectionofgentamicininchickenmuscleandmilk[J].ChineseJournalofAnalyticalChemistry,2022,50(10).[17]RadhakumaryC,SreenivasanK.Gentamicininducedformationofgoldnanoparticlesasanassayprotocolforitsdetection[J].ColloidsandSurfacesA:PhysicochemicalandEngineeringAspects,2014,443:326–330.[18]LiC,ZhangY,EreminSA,etal.Detectionofkanamycinandgentamicinresiduesinanimal-derivedfoodusingIgYantibodybasedic-ELISAandFPIA[J].FoodChemistry,2017,277：48–54.[19]GukowskyJC,TanC,HanZ,etal.Cysteamine-ModifiedGoldNanoparticlesasaColorimetricSensorfortheRapidDetectionofGentamicin[J].JournalofFoodScience,2018,83(6)：1631–1638.[20]AdamsE,RoelantsW,DePaepeR,etal.Analysisofgentamicinbyliquidchromatographywithpulsedelectrochemicaldetection[J].JournalofPharmaceuticalandBiomedicalAnalysis,1999,18(4–5):689–698.[21]MahonWA,EzerJ,WilsonTW.RadioimmunoassayforMeasurementofGentamicininBlood[J].AntimicrobialAgentsandChemotherapy,1973,3(5):585–589.[22]HellerDN,PegginsJO,NochettoCB,etal.LC/MS/MSmeasurementofgentamicininbovineplasma,urine,milk,andbiopsysamplestakenfromkidneysofstandinganimals[J].JournalofChromatographyB,2005,821(1):22–30.[23]劉雪紅,張秀芹,侯穎,等.超高效液相色譜-串聯(lián)質(zhì)譜法檢測(cè)牛奶中7種氨基糖苷類藥物殘留[J].中國(guó)獸藥雜志,2015(3):48-52.LiuXH,ZhangXQ,HouY,etal.Determinationof7aminoglycosidesresiduesinmilkbyultra-highperformanceliquidchromatography-tandemmassspectrometry[J].ChineseJournalofVeterinaryMedicine,2015(3):48-52.(inChinese)[24]呂芳,李英,沈媛,等.超高效液相色譜-串聯(lián)質(zhì)譜法測(cè)定鱘魚(yú)中慶大霉素和新霉素殘留量[J].食品安全質(zhì)量檢測(cè)學(xué)報(bào),2019,10(01):234-239.LvF,LiY,ShenY,etal.DeterminationofgentamicinandneomycinresiduesinSturgeonbyultra-highperformanceliquidchromatography-tandemmassspectrometry[J].JournalofFoodSafetyandQualityInspection,2019,10(01):234-239.(inChinese)[25]馬凱,蔡芳葉,黃永橋,等.超高效液相色譜-串聯(lián)質(zhì)譜法檢測(cè)蜂蜜中九種氨基糖苷類藥物殘留[J].食品與發(fā)酵工業(yè),2020,46(18):203-208.MaK,CaiFY,HuangYQ,etal.Determinationofnineaminoglycosidesresiduesinhoneybyultra-highperformanceliquidchromatography-tandemmassspectrometry[J].FoodandFermentationIndustry,2019,46(18):203-208.(inChinese)[26]王美麗,李敦毅.QuEChERS法提取-液相色譜-質(zhì)譜法檢測(cè)分析制藥園區(qū)污水中青霉素、潔霉素、土霉素、四環(huán)素和慶大霉素殘留方法的建立[J].分析儀器,2021(04):150-154.WangML,LiDY.EstablishmentofQuEChERSextraction-liquidchromatography-massspectrometrymethodfordetectionandanalysisofpenicillin,lincomycin,oxytetracyclineandgentamicinresiduesinwastewaterofpharmaceuticalpark[J].AnalyticalInstruments,2021(04)：150-154.(inChinese)[27]趙國(guó)寶,羅飛,臧勇軍.超高效液相色譜-串聯(lián)質(zhì)譜法測(cè)定豬肉中慶大霉素殘留量[J].肉類工業(yè),2019(07):40-42+51