超高效液相色谱-串联质谱法同时测定饲料中林可霉素和克林霉素残留
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摘要
建立UPLC-MSMS法同时测定饲料中林可霉素和克林霉素残留量。样品处理采用乙腈提取,正己烷去除脂肪净化。分析采用"HSS T3色谱柱";流动相为0.1%(v/v)甲酸-水/乙腈溶液,梯度洗脱;正离子多反应监测模式;外标法进行定量。林可霉素的检出限为5.0μg/kg,定量限为20.0μg/kg,线性范围为20.0～400.0μg/L;克林霉素的检出限为1.0μg/kg,定量限为10.0μg/kg,线性范围分别为5.0～200.0μg/L。该方法专属性强、灵敏度高,分离度好,适用于饲料中林可霉素和克林霉素残留量的测定。
This is to set up a method to determine resides of lincomycin and clindamycin in animal feed by ultra-performance liquid chromatography-tandem mass speftometry method. After the samples were extracted by acetonitrile and removed fat and other impurities by hexane,"HSS T3 chromatographic column"with 0.1%(v/v) formic acid water/acetonitrile as mobile phase, liquid chromatography was separated by gradient elution, with positive ion multiple reaction monitoring and external standard quantitative method. The detection limit of lincomycin was 5.0 μg/kg, the limit of quantitation was 20.0 μg/kg and the linear range was 20.0～400.0 μg/L. The detection limit of clindamycin was 1.0 μg/kg, the limit of quantitation was 10.0 μg/kg and the linear range was 5.0～200.0 μg/L. This method is highly specific, sensitive and separative, applicable to the determination of the resides of lincomycin and clindamycin in animal feed.
This is to set up a method to determine resides of lincomycin and clindamycin in animal feed by ultra-performance liquid chromatography-tandem mass speftometry method. After the samples were extracted by acetonitrile and removed fat and other impurities by hexane,"HSS T3 chromatographic column"with 0.1%(v/v) formic acid water/acetonitrile as mobile phase, liquid chromatography was separated by gradient elution, with positive ion multiple reaction monitoring and external standard quantitative method. The detection limit of lincomycin was 5.0 μg/kg, the limit of quantitation was 20.0 μg/kg and the linear range was 20.0～400.0 μg/L. The detection limit of clindamycin was 1.0 μg/kg, the limit of quantitation was 10.0 μg/kg and the linear range was 5.0～200.0 μg/L. This method is highly specific, sensitive and separative, applicable to the determination of the resides of lincomycin and clindamycin in animal feed.
引文
[1]Tenson T,Lovmar M,Ehrenberg M.The Mecha‐nism of Action of Macrolides,Lincosamides and Streptogramin B Reveals the Nascent Pep‐tide Exit Path in the Ribosome[J].Journal of Molecular Biology,2003,330(5):1005-1014.
[2]牛长群,刘进怀,祝仕清.林可霉素相关物质的LC-ESI-MS研究[J].中国抗生素杂志,2003,28(2):76-78.
[3]孙秋实,李悦,王慧敏,等.LC-MS法研究盐酸克林霉素中的有关物质[J].药物分析杂志,2011(6):1059-1063.
[4]Poucke C V,Keyser K D,Baltusnikiene A,et al.Liquid chromatographic-tandem mass spectrometric detection of banned antibacte‐rial growth promoters in animal feed[J].An‐alytica Chimica Acta,2003,483(1):99-109.
[5]The European Medicines Agency(EMEA):Commit‐tee for Medicinal Products for Veterinary Use(CMVP).Reflection paper on the use of mac‐rolides,lincosamides and streptogramins(MLS)in food-producing animals in the European Union:development of resistance and impact on human and animal health Adoption by CVMP on12 October 2011.http://www.ema.europa.eu/docs/en_GB/document_library/Scientif‐ic_guideline/2011/11/WC500118230.pdf,Ac‐cessed:22.07.2013.
[6]DB/T 1032-2009.饲料中林可霉素的测定-高效液相色谱法[S].安徽省地方标准,2009.
[7]Michal Dou?a,Zdeněk Sika,Michal Halama,et al.HPLC determination of lincomycin in pre‐mixes and feedstuffs with solid-phase ex‐traction on HLB OASIS and LC-MS/MS confir‐mation[J].J Pharm Biomed Anal,2006,40(4):981-986.
[8]GB/T 20762-2006.畜禽肉中林可霉素、竹桃霉素、红霉素、替米考星、泰乐菌素、克林霉素、吉它霉素、交沙霉素残留量的测定液相色谱-串联质谱法[S].中华人民共和国国家标准,2006.
[9]GB/T 22941-2008.蜂蜜中林可霉素、红霉素、螺旋霉素、替米考星、泰乐菌素、交沙霉素、吉它霉素、竹桃霉素残留量的测定液相色谱-串联质谱法[S].中华人民共和国国家标准,2008.
[10]GB/T 22946-2008.蜂王浆和蜂王浆冻干粉中林可霉素、红霉素、替米考星、泰乐菌素、螺旋霉素、克林霉素、吉它霉素、交沙霉素残留量的测定液相色谱-串联质谱法[S].中华人民共和国国家标准,2008.
[11]Spisso B F,Ferreira R G,Pereira M U,et al.Simultaneous determination of polyether ionophores,macrolides and lincosamides in hen eggs by liquid chromatography-electro‐spray ionization tandem mass spectrometry using a simple solvent extraction[J].Ana‐lytica Chimica Acta,2010,682(1-2):82-92.
[12]孙雷,张骊,王树槐,等.超高效液相色谱-串联质谱法对动物源食品中13种林可胺类及大环内酯类药物残留的检测[J].分析测试学报,2009,28(9):1058-1061.
[13]刘正才,杨方,林永辉,等.超高效液相色谱串联质谱法测定鳗鱼中大环内酯类和林可酰胺类抗生素残留量的研究[J].福建分析测试,2010(3):1-5.
[14]严丽娟,储晓刚,周昱,等超高效液相色谱-电喷雾串联质谱法测定动物饲料中的大环内酯类和林可胺类抗生素[J].色谱,2010,28(11):1038-1042.
[15]刘瑜,赵颖,张鹏远,等.超高效液相色谱-串联质谱法同时检测复合预混饲料中29种兽药[J].分析试验室,2012,31(10):77-81.
[2]牛长群,刘进怀,祝仕清.林可霉素相关物质的LC-ESI-MS研究[J].中国抗生素杂志,2003,28(2):76-78.
[3]孙秋实,李悦,王慧敏,等.LC-MS法研究盐酸克林霉素中的有关物质[J].药物分析杂志,2011(6):1059-1063.
[4]Poucke C V,Keyser K D,Baltusnikiene A,et al.Liquid chromatographic-tandem mass spectrometric detection of banned antibacte‐rial growth promoters in animal feed[J].An‐alytica Chimica Acta,2003,483(1):99-109.
[5]The European Medicines Agency(EMEA):Commit‐tee for Medicinal Products for Veterinary Use(CMVP).Reflection paper on the use of mac‐rolides,lincosamides and streptogramins(MLS)in food-producing animals in the European Union:development of resistance and impact on human and animal health Adoption by CVMP on12 October 2011.http://www.ema.europa.eu/docs/en_GB/document_library/Scientif‐ic_guideline/2011/11/WC500118230.pdf,Ac‐cessed:22.07.2013.
[6]DB/T 1032-2009.饲料中林可霉素的测定-高效液相色谱法[S].安徽省地方标准,2009.
[7]Michal Dou?a,Zdeněk Sika,Michal Halama,et al.HPLC determination of lincomycin in pre‐mixes and feedstuffs with solid-phase ex‐traction on HLB OASIS and LC-MS/MS confir‐mation[J].J Pharm Biomed Anal,2006,40(4):981-986.
[8]GB/T 20762-2006.畜禽肉中林可霉素、竹桃霉素、红霉素、替米考星、泰乐菌素、克林霉素、吉它霉素、交沙霉素残留量的测定液相色谱-串联质谱法[S].中华人民共和国国家标准,2006.
[9]GB/T 22941-2008.蜂蜜中林可霉素、红霉素、螺旋霉素、替米考星、泰乐菌素、交沙霉素、吉它霉素、竹桃霉素残留量的测定液相色谱-串联质谱法[S].中华人民共和国国家标准,2008.
[10]GB/T 22946-2008.蜂王浆和蜂王浆冻干粉中林可霉素、红霉素、替米考星、泰乐菌素、螺旋霉素、克林霉素、吉它霉素、交沙霉素残留量的测定液相色谱-串联质谱法[S].中华人民共和国国家标准,2008.
[11]Spisso B F,Ferreira R G,Pereira M U,et al.Simultaneous determination of polyether ionophores,macrolides and lincosamides in hen eggs by liquid chromatography-electro‐spray ionization tandem mass spectrometry using a simple solvent extraction[J].Ana‐lytica Chimica Acta,2010,682(1-2):82-92.
[12]孙雷,张骊,王树槐,等.超高效液相色谱-串联质谱法对动物源食品中13种林可胺类及大环内酯类药物残留的检测[J].分析测试学报,2009,28(9):1058-1061.
[13]刘正才,杨方,林永辉,等.超高效液相色谱串联质谱法测定鳗鱼中大环内酯类和林可酰胺类抗生素残留量的研究[J].福建分析测试,2010(3):1-5.
[14]严丽娟,储晓刚,周昱,等超高效液相色谱-电喷雾串联质谱法测定动物饲料中的大环内酯类和林可胺类抗生素[J].色谱,2010,28(11):1038-1042.
[15]刘瑜,赵颖,张鹏远,等.超高效液相色谱-串联质谱法同时检测复合预混饲料中29种兽药[J].分析试验室,2012,31(10):77-81.