HPLC法测定喹乙醇预混剂中喹乙醇的含量
|
摘要
建立并验证了喹乙醇预混剂中喹乙醇含量的高效液相色谱测定法。试验采用十八烷基硅烷键合硅胶色谱柱(250 mm×4.6 mm,5μm),以0.02 mol/L磷酸二氢钾溶液(用三乙胺调节pH值为6.0)-乙腈(92∶8,V∶V)为流动相,流速为1.0 mL/min,柱温为30℃,检测波长为262 nm。试验结果表明喹乙醇在5~100μg/mL范围内线性良好,R~2=1.0000,平均回收率100.2%(n=6),RSD为0.2%。建立的方法简便、准确、可靠,可更好地控制喹乙醇预混剂的质量。
The method for determination of olaquindox in olaquindox premix by HPLC was developed and validated. Analysis was performed on a C18 column( 250 mm × 4. 6 mm,5 μm) with a mode of 0. 02 mol/L monopotassium phosphateaqueous solution( pH value was adjusted to 6.0 by triethylamine)-acetonitrile(92 ∶ 8)at a flow rate of 1.0 mL/min and a column temperature of 30 ℃. The determination wave length was 262 nm. The results showed that a good linear relationship was accepted in the range of 5 ~ 100 μg/mL( R~2= 1.0000),and the average recovery was 100.2%( n = 6) with RSD of 0.2%. This method was convenient,accurate,reliable and was suitable to control the quality of olaquindox premix.
The method for determination of olaquindox in olaquindox premix by HPLC was developed and validated. Analysis was performed on a C18 column( 250 mm × 4. 6 mm,5 μm) with a mode of 0. 02 mol/L monopotassium phosphateaqueous solution( pH value was adjusted to 6.0 by triethylamine)-acetonitrile(92 ∶ 8)at a flow rate of 1.0 mL/min and a column temperature of 30 ℃. The determination wave length was 262 nm. The results showed that a good linear relationship was accepted in the range of 5 ~ 100 μg/mL( R~2= 1.0000),and the average recovery was 100.2%( n = 6) with RSD of 0.2%. This method was convenient,accurate,reliable and was suitable to control the quality of olaquindox premix.
引文
[1]Linton A H,Hedges A J,Bennett P M.Monitoring for the development of antimicrobial resistance during the use of olaquindox as a feed additive on commercial pig farms[J].The Journal of Applied Bacteriology,1988,64(4):311-327.
[2]Chen Q,Tang S,Jin X,Zou J,et al.Investigation of the genotoxicity of guinocetone,carbadox and olaquindox in vitro using vero cells[J].Food and Chemical Toxicology.2009,47(2):328-334.
[3]Zou J J,Chen Q,Jin X,et al.Olaquindox induces apoptosis through the mitochondrial pathway in Hep G2 cells[J].Toxicology,2011,285(3):104-113.
[4]中国兽药典委员会.中华人民共和国兽药典兽药使用指南2010年版化学药品卷[S].Commission of Chineses Veterinary Pharmacopoeia.Guide to Utilization of Veterinary Drug in Veterinary Pharmacopoeia of People's Republic of China,2010,Chemical Medicine Volume.
[5]农业部.农业部第168号公告[S].Ministry of Agriculture.No.168 Bulletin of The Ministry of Agriculture of The Pepole's Republic of China[S].
[6]何方洋,郗日沫,冯才伟,等.喹乙醇药物ELISA检测方法的建立[J].畜牧与兽医,2011,43(6):56-60.He F Y,Xi R M,Feng C W,et al.Determination of olaquindox by ELISA[J].Animal Busbandry&Veterinary Medicine,2011,43(6):56-60.
[7]刘淳.超高效液相色谱测定猪肉中喹乙醇的残留量[J].分析仪器,2015,(2):44-47.Liu C.Determination of olaqunindox residue in pork by ultra high performance liquid chromatography[J].Analytical Instrumentation,2015,(2):44-47.
[8]易锡斌,裘立群,刘世琦,等.液相色谱-串联质谱同时测定禽肉组织中盐酸金刚烷胺、盐酸金刚乙胺、地塞米松、替米考星及喹乙醇代谢物的残留量[J].分析测试学报,2015,34(3):346-351.Yi X B,Qiu L Q,Liu S Q,et al.Simultaneous determination of amantadine hydrochloride,rimantadine hydrochloride,dexamethasone,tilmicosin and olaquindox metabolite residues in poultry tissues by high performance liquid chromatography coupled with tandem mass spectrometry[J].Journal of Instrumental Analysis,2015,34(3):346-351.
[9]吴宁鹏,王丽景,李慧素,等.五种兽药中非法添加喹乙醇和乙酰甲喹的HPLC-PDA:检测方法的建立[J].中国兽药杂志,2014,48(12):43-49.Wu N P,Wang L J,Li H S,et al.Determination of olaquindox and mequindox illegally added in five kinds of veterinary drug by HPLC-PDA[J].Chinese Journal of Veterinary Drug,2014,48(12):43-49.
[10]中国兽药典委员会.中华人民共和国兽药典2010年版一部[S].Commission of Chineses Veterinary Pharmacopoeia.Veterinary Pharmacopoeia of People's Republic of China,2010 edition,Part1[S].
[11]陆春波,高三玉,罗成江,等.HPLC-DAD法检测喹乙醇预混剂中违规添加喹烯酮的研究[J].中国兽药杂志,2017,51(3):61-64.Lu C B,Gao S Y,Luo C J,et al.Determination of quinocetone into olaquindox premix by HPLC-DAD[J].Chinese Journal of Veterinary Drug,2017,51(3):61-64.
[2]Chen Q,Tang S,Jin X,Zou J,et al.Investigation of the genotoxicity of guinocetone,carbadox and olaquindox in vitro using vero cells[J].Food and Chemical Toxicology.2009,47(2):328-334.
[3]Zou J J,Chen Q,Jin X,et al.Olaquindox induces apoptosis through the mitochondrial pathway in Hep G2 cells[J].Toxicology,2011,285(3):104-113.
[4]中国兽药典委员会.中华人民共和国兽药典兽药使用指南2010年版化学药品卷[S].Commission of Chineses Veterinary Pharmacopoeia.Guide to Utilization of Veterinary Drug in Veterinary Pharmacopoeia of People's Republic of China,2010,Chemical Medicine Volume.
[5]农业部.农业部第168号公告[S].Ministry of Agriculture.No.168 Bulletin of The Ministry of Agriculture of The Pepole's Republic of China[S].
[6]何方洋,郗日沫,冯才伟,等.喹乙醇药物ELISA检测方法的建立[J].畜牧与兽医,2011,43(6):56-60.He F Y,Xi R M,Feng C W,et al.Determination of olaquindox by ELISA[J].Animal Busbandry&Veterinary Medicine,2011,43(6):56-60.
[7]刘淳.超高效液相色谱测定猪肉中喹乙醇的残留量[J].分析仪器,2015,(2):44-47.Liu C.Determination of olaqunindox residue in pork by ultra high performance liquid chromatography[J].Analytical Instrumentation,2015,(2):44-47.
[8]易锡斌,裘立群,刘世琦,等.液相色谱-串联质谱同时测定禽肉组织中盐酸金刚烷胺、盐酸金刚乙胺、地塞米松、替米考星及喹乙醇代谢物的残留量[J].分析测试学报,2015,34(3):346-351.Yi X B,Qiu L Q,Liu S Q,et al.Simultaneous determination of amantadine hydrochloride,rimantadine hydrochloride,dexamethasone,tilmicosin and olaquindox metabolite residues in poultry tissues by high performance liquid chromatography coupled with tandem mass spectrometry[J].Journal of Instrumental Analysis,2015,34(3):346-351.
[9]吴宁鹏,王丽景,李慧素,等.五种兽药中非法添加喹乙醇和乙酰甲喹的HPLC-PDA:检测方法的建立[J].中国兽药杂志,2014,48(12):43-49.Wu N P,Wang L J,Li H S,et al.Determination of olaquindox and mequindox illegally added in five kinds of veterinary drug by HPLC-PDA[J].Chinese Journal of Veterinary Drug,2014,48(12):43-49.
[10]中国兽药典委员会.中华人民共和国兽药典2010年版一部[S].Commission of Chineses Veterinary Pharmacopoeia.Veterinary Pharmacopoeia of People's Republic of China,2010 edition,Part1[S].
[11]陆春波,高三玉,罗成江,等.HPLC-DAD法检测喹乙醇预混剂中违规添加喹烯酮的研究[J].中国兽药杂志,2017,51(3):61-64.Lu C B,Gao S Y,Luo C J,et al.Determination of quinocetone into olaquindox premix by HPLC-DAD[J].Chinese Journal of Veterinary Drug,2017,51(3):61-64.