混合型饲料添加剂中硫酸黏杆菌素的液相色谱检测方法研究
|
摘要
本研究建立了混合型饲料添加剂中硫酸黏杆菌素含量的液相色谱检测方法。混合型饲料添加剂样品用5%草酸提取,经离心和HLB小柱净化,用丹磺酰氯柱前衍生,以C_8柱(150 mm×4.6 mm×5μm)为分离柱,荧光检测器在激发波长344 nm,发射波长518 nm下进行检测。结果表明:在所选择的色谱条件和衍生条件下,硫酸黏杆菌素A在0.025～10.0μg/mL时线性关系良好,最低定量限为2 mg/kg;添加回收率为85.1%～108%,变异系数为0.84%～5.52%。本方法样品前处理简便、可靠,可用于混合型饲料添加剂中硫酸黏杆菌素的检测。
The study established a liquid phase chromatographic method for determination of colistin sulfate in mixed feed additives.Feed samples were firstly extracted by 5% oxalic acid,purification with HLB SPE cartridges,and derivatization with Dns-Clafter.The products were isolated by C8(150 mm×4.6 mm×5 μm)column,eventually detected by fluorescent detector at an excitation wavelength of 344 nm and an emission wavelength of 518 nm.The results showed that under the selected chromatographic and derivative conditions,colistin sulfate A was linear in the range of 0.025 ～ 10.0 μg/m L,and the lowest determination limit was 2 mg/kg.The relative standard deviation(RSD) was 0.84% ～ 5.52% when the recovery rate was 85.1% ～ 106%.The method was proved to be simple,rapid and resproducible for determination of colistin sulfate in mixed feed additives.
The study established a liquid phase chromatographic method for determination of colistin sulfate in mixed feed additives.Feed samples were firstly extracted by 5% oxalic acid,purification with HLB SPE cartridges,and derivatization with Dns-Clafter.The products were isolated by C8(150 mm×4.6 mm×5 μm)column,eventually detected by fluorescent detector at an excitation wavelength of 344 nm and an emission wavelength of 518 nm.The results showed that under the selected chromatographic and derivative conditions,colistin sulfate A was linear in the range of 0.025 ～ 10.0 μg/m L,and the lowest determination limit was 2 mg/kg.The relative standard deviation(RSD) was 0.84% ～ 5.52% when the recovery rate was 85.1% ～ 106%.The method was proved to be simple,rapid and resproducible for determination of colistin sulfate in mixed feed additives.
引文
[1]程古月,李俊,郝海红,等.黏杆菌素在动物中的研究与应用[J].中国兽医学报,2017,37(8):1617~1626.
[2]罗方方.水产品中硫酸粘菌素、杆菌肽、维吉尼霉素M_1残留量的检测方法研究:[硕士学位论文][D].福建:集美大学,2013.
[3]李延山.液相色谱-串联质谱法检测饲料中硫酸黏杆菌素[J].饲料工业,2017,38(14):56~58.
[4]林维宣,孙兴权,田苗,等.动物组织中粘杆菌素、杆菌肽及维吉尼霉素残留量的液相色谱-串联质谱检测[J].分析测试学报,2009,28(2):212~215.
[5]宋凯,郭远明.动物肌肉组织中粘杆菌素残留量的测定[J].食品与机械,2013,29(5):71~74.
[6]吴水华,尤洁,柯伙钊,等.多粘菌素E检测方法的研究新进展[J].海峡药学,2014,26(4):15~17.
[7]杨海峰,葛竹兴.硫酸黏杆菌素研究概况[J].饲料工业,2007,2:58~59.
[8]中华人民共和国农业部.农业部2086号公告-6-2014[S].中华人民共和国国家标准—饲料中硫酸黏杆菌素的测定液相色谱-串联质谱法.北京:2014-04-01.
[9]张玮,李会荣,宫玲玲.丹磺酰氯作为硫酸黏杆菌素柱前衍生试剂衍生化条件的研究[J].饲料研究,2017,23:46~49.
[10] LEGUA C M,FALCO P C,CABEZA A S,et al.Urine polyamines determinition using dansyl chloride derivatization in soilid-phase extraction cartridges and HPLC[J].Analyst,1999,124:477~501.
[11] Orwa J A,Govaerts C,Gevers K,et al.Study of the stability of polymyxins B1,E1and E2in aqueous solution using liquid chromatography and mass spectrometry[J].Journal of Pharmaceutical and Biomedical Analysis,2002,29:203~212.
[2]罗方方.水产品中硫酸粘菌素、杆菌肽、维吉尼霉素M_1残留量的检测方法研究:[硕士学位论文][D].福建:集美大学,2013.
[3]李延山.液相色谱-串联质谱法检测饲料中硫酸黏杆菌素[J].饲料工业,2017,38(14):56~58.
[4]林维宣,孙兴权,田苗,等.动物组织中粘杆菌素、杆菌肽及维吉尼霉素残留量的液相色谱-串联质谱检测[J].分析测试学报,2009,28(2):212~215.
[5]宋凯,郭远明.动物肌肉组织中粘杆菌素残留量的测定[J].食品与机械,2013,29(5):71~74.
[6]吴水华,尤洁,柯伙钊,等.多粘菌素E检测方法的研究新进展[J].海峡药学,2014,26(4):15~17.
[7]杨海峰,葛竹兴.硫酸黏杆菌素研究概况[J].饲料工业,2007,2:58~59.
[8]中华人民共和国农业部.农业部2086号公告-6-2014[S].中华人民共和国国家标准—饲料中硫酸黏杆菌素的测定液相色谱-串联质谱法.北京:2014-04-01.
[9]张玮,李会荣,宫玲玲.丹磺酰氯作为硫酸黏杆菌素柱前衍生试剂衍生化条件的研究[J].饲料研究,2017,23:46~49.
[10] LEGUA C M,FALCO P C,CABEZA A S,et al.Urine polyamines determinition using dansyl chloride derivatization in soilid-phase extraction cartridges and HPLC[J].Analyst,1999,124:477~501.
[11] Orwa J A,Govaerts C,Gevers K,et al.Study of the stability of polymyxins B1,E1and E2in aqueous solution using liquid chromatography and mass spectrometry[J].Journal of Pharmaceutical and Biomedical Analysis,2002,29:203~212.