利福昔明子宫注入剂含量测定及方法耐用性试验研究

The Content Determination of Rifaximin Uterine Injection and Durability Test

关键词:  利福昔明子宫注入剂  含量测定  耐用性试验  高效液相色谱

Key words:  rifaximin uterine injections  content determination  durability test  HPLC

摘要:

本研究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。制剂采用乙腈提取，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-1浓度范围内线性关系良好(r=0.9995)，检测限（LOD）为0.25μg?mL-1，定量限（LOQ）为0.6μg?mL-1。以80、100、120μg?mL-1三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%。结论：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，可以用作该制剂的质量控制。

Abstract:

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 show that:The calibration curve of rifaximin was linear at the concentration range of 40-150μg?mL-1(r=0.9995),and the limit of detection (LOD) was 0.25μg?mL-1,the limit of quantification (LOQ) was 0.6μg?mL-1.The recovery rate was 98.26%-101.12% at the concentration of 80,100,120μg?mL-1 ,the intra-day coefficient of variation was 0.17%-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.Conclusion: This method was shown to be simple and reliable, therefore it can be applied for the quality control of rifaximin uterine injections.