离子色谱法测定盐酸法舒地尔药物中高哌嗪含量

目的: 建立高效离子色谱法测定药物盐酸法舒地尔中高哌嗪含量的方法。 方法: 采用阳离子色谱柱IonPac CS17(4 mm×250 mm),以17 mmol·L^-1甲烷磺酸溶液-乙腈(85∶15)作为淋洗液,进样量25 μL,在流速1.0 mL·min^-1的条件下,测定盐酸法舒地尔样品中残留药物中间体高哌嗪的含量。 结果: 在0.05~10 μg·mL^-1范围内线性关系良好,线性相关系数为0.9996,加样回收率在97.8%~101.2%之间。 结论: 该方法具有灵敏度高,操作简单,重复性好等特点,能够快速准确测定药物中的痕量高哌嗪。

Objective: To establish a new method for the determination of homopiperazine in fasudil hydrochloride based on high-performance ion chromatography. Methods: Fasudil hydrochloride was first dissolved in methane sulfonic acid, and then the solution was filtered through a 0.45 μm syringe membrane filter and Guard RP cleanup column before injection. The IC separation was performed on an IonPac CS17 (4 mm×250 mm) column with 17 mmol·L^-1 methanesulfonic acid and acetonitrile(85∶15)as the elution and a Cation MicroMembrane Suppressor(CMMS 300,4 mm)as the suppression. Results: The background was much reduced and the sensitivities of homopiperazine were greatly improved.Calibration curves of peak area versus concentration showed a linear correlation coefficient of 0.9996 for homopiperazine in the range of 0.05-10 μg·mL^-1.Average recoveries were between 98.0%-102.0%. Conclusion: The established Ion chromatography method has the advantages of high sensitivity,specificity and reproductivity, which can be applied to the limit amount determination of drug homopiperazine.

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