利福昔明子宫注入剂含量测定及方法耐用性试验研究
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摘要
建立了利福昔明子宫注入剂HPLC含量测定方法,并对色谱测定条件进行了不同检测波长、流速及柱温等条件的耐用性研究。乙腈提取,超声离心后,经流动相稀释上机检测。结果显示,研究建立的利福昔明子宫注入剂含量测定方法在40~150μg/mL浓度范围内线性关系良好(r=0.9995),检测限(LOD)为0.25μg/mL,定量限(LOQ)为0.6μg/mL。以80、100、120μg/mL三个浓度水平进行添加回收,回收率在98.26%~101.12%之间,日内变异系数在0.17%~1.13%之间,日间变异系数<0.73%。耐用性研究表明,在测试范围内,检测波长、流速、柱温对含量测定无明显影响(RSD<2.0%)。三批制剂样品经测定后,含量分别为102.0%、99.8%、100.6%。本研究建立的利福昔明子宫注入剂含量方法操作简便、方法可靠,可用作该制剂的质量控制。
This study was aimed to establish a method for the content determination of rifaximin uterine injections by high-performance liquid chromatography(HPLC),and the durability of different conditions such as detection wavelength,flow rate and column temperature were studied also.The preparation was extracted with acetonitrile,after sonicated and centrifuged,then diluted with mobile phase to detect.The results showed that the calibration curve of rifaximin was linear at the concentration range of from 40 to 150 μg/mL(r=0.9995),and the limit of detection(LOD) was 0.25 μg/mL,the limit of quantification(LOQ) was 0.6 μg/mL.The recovery rate was from98.26% to 101.12% at the concentration of 80,100,120 μg/mL,the intra-day coefficient of variation was from 0.17% to 1.13%,and the inter-day coefficient of variation was <0.73%.In the durability studies,the wavelength,flow rate and column temperature had no significant effect on the content determination within the test range(RSD<2.0%).The content of three batches of the samples were 102.0%,99.8% and 100.6% respectively.This method was shown to be simple and reliable,therefore it can be applied for the quality control of rifaximin uterine injections.
This study was aimed to establish a method for the content determination of rifaximin uterine injections by high-performance liquid chromatography(HPLC),and the durability of different conditions such as detection wavelength,flow rate and column temperature were studied also.The preparation was extracted with acetonitrile,after sonicated and centrifuged,then diluted with mobile phase to detect.The results showed that the calibration curve of rifaximin was linear at the concentration range of from 40 to 150 μg/mL(r=0.9995),and the limit of detection(LOD) was 0.25 μg/mL,the limit of quantification(LOQ) was 0.6 μg/mL.The recovery rate was from98.26% to 101.12% at the concentration of 80,100,120 μg/mL,the intra-day coefficient of variation was from 0.17% to 1.13%,and the inter-day coefficient of variation was <0.73%.In the durability studies,the wavelength,flow rate and column temperature had no significant effect on the content determination within the test range(RSD<2.0%).The content of three batches of the samples were 102.0%,99.8% and 100.6% respectively.This method was shown to be simple and reliable,therefore it can be applied for the quality control of rifaximin uterine injections.
引文
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[9]林红,张智德,郑莉,等.利福昔明在防治奶牛乳房炎中的研究进展[J].中国奶牛,2014,(18):21-23.Lin H,Zhang Z,Zheng L,et al.Research progress of rifaximin in preventing and curing cow mastitis[J].China Dairy Cattle,2014,(18):21-23.
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[11]孙雷,李丹,毕言锋,等.牛奶中利福昔明残留消除规律研究[J].中国兽药杂志,2013,47(9):27-30.Sun L,Li D,Bi Y F,et al.Study on the Depletion of Rifaximin Residue in Milk[J].Chinese Journal of Veterinary Drug,2013,47(9):27-30.
[2]李世宏,杨国林,杨锐乐,等.奶牛子宫内膜炎研究进展[J].中国奶牛,2007,(1):34-38.Li S H,Yang G L,Yang R L,et al.Research Progress of Cow Endometritis[J].China Dairy Cattle,2007,(1):34-38.
[3]Williams E J,Fischer D P,Noakes D E,et al.The relationship between uterine pathogen growth density and ovarian function in the postpartum dairy cow[J].Theriogenology,2007,68(4):549-559.
[4]赵红琼,黄燕,陈杖榴,等.新疆地区奶牛子宫内膜炎病原菌的分离鉴定及其对抗菌药的敏感性试验[J].中兽医医药杂志,2005,(2):16-19.Zhao H Q,Huang Y,Chen Z L,et al.Identification of endometritis pathogens from Xinjiang dairy cows and their susceptibilities to antibacterials[J].Journal of Traditional Chinese Veterinary Medicine,2005,(2):16-19.
[5]陈星,胡松华,张克春,等.奶牛子宫内膜炎病原菌的分离鉴定及药敏试验[J].中国兽医杂志,2010,(1):43-44.Chen X,Hu S H,Zhang K C,et al.Isolation and Identification of Pathogenic Bacteria of Cow Endometritis and Drug Susceptibility Test[J].Chinese Journal of Veterinary Medicine,2010,(1):43-44.
[6]王佩,李玉珍.利福昔明的药理作用和临床应用[J].药物不良反应杂志,2005,(5):382-385.Wang P,Li Y Z.Pharmacological actions and clinical applications of rifaximin[J].Adverse Drug Reactions Journal,2005,(5):382-385.
[7]Gillis J C,Brogden R N.Rifaximin.A review of its antibacterial activity,pharmacokinetic properties and therapeutic potential in conditions mediated by gastrointestinal bacteria[J].Drugs,1995,49(3):467-484.
[8]周智,凌宁,黄长武,等.利福昔明片多中心、随机、单盲对照治疗急性细菌感染性腹泻的临床疗效观察[J].中国抗生素杂志,2004,(5):307-310.Zhou Z,Ling N,Huang C W,et al.Rifaximin in treatment of acute bacterial diarrhea a randomized,single-blind and multicenter clinical trial[J].Chinese Journal of Antibiotics,2004,(5):307-310.
[9]林红,张智德,郑莉,等.利福昔明在防治奶牛乳房炎中的研究进展[J].中国奶牛,2014,(18):21-23.Lin H,Zhang Z,Zheng L,et al.Research progress of rifaximin in preventing and curing cow mastitis[J].China Dairy Cattle,2014,(18):21-23.
[10]齐利宁——利福昔明乳房注入剂[J].北方牧业,2014,(17):28.Qi Lining-Rifaximin Breast Implants[J].Northern animal husbandry,2014,(17):28.
[11]孙雷,李丹,毕言锋,等.牛奶中利福昔明残留消除规律研究[J].中国兽药杂志,2013,47(9):27-30.Sun L,Li D,Bi Y F,et al.Study on the Depletion of Rifaximin Residue in Milk[J].Chinese Journal of Veterinary Drug,2013,47(9):27-30.