HPLC法测定猪血浆中帕托珠利的方法学建立
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摘要
建立了HPLC法测定猪血浆中帕托珠利含量的方法。色谱柱为安捷伦ZORBAX Eclipse XDB-C18柱(250 mm×4.6 mm,5μm),流动相0.2%乙酸水溶液-乙腈(47∶53),柱温35℃,流速为1 m L/min,检测波长为250 nm。在本方法条件下,帕托珠利在0.1～10μg/m L浓度范围内线性关系良好(r>0.999),检测限(LOD)为0.04μg/m L,定量限(LOQ)为0.1μg/m L,批内和批间回收率均大于90%,批内和批间精密度RSD均小于9%。本方法简单、准确、快速,可用于测定猪血浆中帕托珠利的含量。
The paper established an HPLC method for the determination of ponazuril in pig plasma. The column was Agilent ZORBAX Eclipse XDB-C18( 250 mm×4.6 mm,5 μm); the mobile phase consisted of water( 0.2%acetic acid)-acetonitrile( 47: 53); the column temperature was 35 ℃; the flow rate was 1 mL/min; the detection wavelength was 250 nm.Under the condition of this method,ponazuril has a good linear relationship in the range of 0.1 ～ 10 μg/m L( r > 0. 999); the detection limit( LOD) is 0. 04 μg/m L; the limit of quantitation( LOQ) is0.1 μg/m L; the intraland inter-assay recovery rates were both greater than 90%; the internal and inter-assay precision RSD were less than 9%. The method is simple,accurate and rapid. It can be used to determine the content of ponazuril in pig plasma.
The paper established an HPLC method for the determination of ponazuril in pig plasma. The column was Agilent ZORBAX Eclipse XDB-C18( 250 mm×4.6 mm,5 μm); the mobile phase consisted of water( 0.2%acetic acid)-acetonitrile( 47: 53); the column temperature was 35 ℃; the flow rate was 1 mL/min; the detection wavelength was 250 nm.Under the condition of this method,ponazuril has a good linear relationship in the range of 0.1 ～ 10 μg/m L( r > 0. 999); the detection limit( LOD) is 0. 04 μg/m L; the limit of quantitation( LOQ) is0.1 μg/m L; the intraland inter-assay recovery rates were both greater than 90%; the internal and inter-assay precision RSD were less than 9%. The method is simple,accurate and rapid. It can be used to determine the content of ponazuril in pig plasma.
引文
[1]邱小兵.妥曲珠利砜对猪球虫病的药效学及安全药理学研究[D].江西农业大学,2013.Qiu X B. Pharmacodynamics and safety pharmacology of toltrazuril on porcine coccidiosis[D]. Jiangxi Agricultural University,2013.
[2]王翔林,王冠楠,钱琛,等. HPLC法测定帕那珠利含量[J].中国兽药杂志,2012,46(8):35-38.Wang X L,Wang G N,Qian S,et al. Determination of Panazuril by HPLC[J]. Chinese Journal of Veterinary Medicine,2012,46(8):35-38.
[3] Zou M,Guo G,Zhao Y,et al. Detection,quantifications,and pharmacokinetics of ponazuril in healthy swine[J]. Journal of Veterinary Pharmacology and Therapeutics,2014,37(6):598-602.
[4] Dirkolu L,Yohn R,Garrett E F,et al. Quantifications and pharmacokinetics of toltrazuril sulfone(ponzuril)in cattle[J]. Journal of Veterinary Pharmacology and Therapeutics,2009,32(3):280-288.
[5] Kim M S,Lim J H,Hwang Y H,et al. Plasma disposition of toltrazuril and its metabolites,toltrazuril sulfoxide and toltrazuril sulfone,in rabbits after oral administration.[J]. Veterinary Parasitology,2010,169(1):51-56.
[6] Love D,Gibbons P,Fajt V,et al. Pharmacokinetics of singledose oral ponazuril in weanling goats[J]. Journal of Veterinary Pharmacology and Therapeutics,2016,39(3):4.
[7] Victor H,Magne Y,Oyvin O. Determination of flunixin and tiamulin hydrogen fumarate in meat and toltrazuril and the metabolite toletazurilsulfon in meat and eggs using LC/MS[J]. Journal of Liquid Chromatography&Related Technologies,2003,26(5):791-801.
[8]徐颖洁,韩航如,郭永刚,等.液质联用方法测定鸡血浆中妥曲珠利及其代谢产物[J].南京农业大学学报,2006,29(1):127-130.Chen Y J,Han H R,Guo Y G,et al. Determination of toltrazuril and its metabolites in chicken plasma by liquid chromatographymass spectrometry[J]. Journal of Nanjing Agricultural University,2006,29(1):127-130.
[9]宫小明,孙军,董静,等.高效液相色谱-串联质谱法测定猪肉中的阿维菌素类、地克珠利、妥曲珠利及其代谢物残留[J].色谱,2011,29(3):217-222.Gong X M,Sun J,Dong J,et al. Determination of avermectins,diclazuril,toltrazuril and their metabolite residues in pork by high performance liquid chromatography-tandem mass spectrometry[J]. Chromatography,2011,29(3):217-222.
[10]卢朝成,符华林,张伟,等.妥曲珠利微晶体的制备及其在家兔体内的药动学[J].中国兽医学报,2014,34(7):149-153.Lu C C,Fu H L,Zhang W,et al. Preparation of toltrazuril microcrystals and pharmacokinetics in rabbits[J]. Chinese Veterinary Journal,2014,34(7):149-153.
[2]王翔林,王冠楠,钱琛,等. HPLC法测定帕那珠利含量[J].中国兽药杂志,2012,46(8):35-38.Wang X L,Wang G N,Qian S,et al. Determination of Panazuril by HPLC[J]. Chinese Journal of Veterinary Medicine,2012,46(8):35-38.
[3] Zou M,Guo G,Zhao Y,et al. Detection,quantifications,and pharmacokinetics of ponazuril in healthy swine[J]. Journal of Veterinary Pharmacology and Therapeutics,2014,37(6):598-602.
[4] Dirkolu L,Yohn R,Garrett E F,et al. Quantifications and pharmacokinetics of toltrazuril sulfone(ponzuril)in cattle[J]. Journal of Veterinary Pharmacology and Therapeutics,2009,32(3):280-288.
[5] Kim M S,Lim J H,Hwang Y H,et al. Plasma disposition of toltrazuril and its metabolites,toltrazuril sulfoxide and toltrazuril sulfone,in rabbits after oral administration.[J]. Veterinary Parasitology,2010,169(1):51-56.
[6] Love D,Gibbons P,Fajt V,et al. Pharmacokinetics of singledose oral ponazuril in weanling goats[J]. Journal of Veterinary Pharmacology and Therapeutics,2016,39(3):4.
[7] Victor H,Magne Y,Oyvin O. Determination of flunixin and tiamulin hydrogen fumarate in meat and toltrazuril and the metabolite toletazurilsulfon in meat and eggs using LC/MS[J]. Journal of Liquid Chromatography&Related Technologies,2003,26(5):791-801.
[8]徐颖洁,韩航如,郭永刚,等.液质联用方法测定鸡血浆中妥曲珠利及其代谢产物[J].南京农业大学学报,2006,29(1):127-130.Chen Y J,Han H R,Guo Y G,et al. Determination of toltrazuril and its metabolites in chicken plasma by liquid chromatographymass spectrometry[J]. Journal of Nanjing Agricultural University,2006,29(1):127-130.
[9]宫小明,孙军,董静,等.高效液相色谱-串联质谱法测定猪肉中的阿维菌素类、地克珠利、妥曲珠利及其代谢物残留[J].色谱,2011,29(3):217-222.Gong X M,Sun J,Dong J,et al. Determination of avermectins,diclazuril,toltrazuril and their metabolite residues in pork by high performance liquid chromatography-tandem mass spectrometry[J]. Chromatography,2011,29(3):217-222.
[10]卢朝成,符华林,张伟,等.妥曲珠利微晶体的制备及其在家兔体内的药动学[J].中国兽医学报,2014,34(7):149-153.Lu C C,Fu H L,Zhang W,et al. Preparation of toltrazuril microcrystals and pharmacokinetics in rabbits[J]. Chinese Veterinary Journal,2014,34(7):149-153.