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目的:建立离子色谱法测定甲磺酸倍他司汀中甲磺酸的含量,并进行不确定度评定。方法:采用Ion Pac AS11-HC(25 mm×4.0 mm,5μm)阴离子色谱柱,以12 mmol·L~(-1)氢氧化钠溶液为淋洗液,采用电导检测器,抑制器电压30 m V。结果:甲磺酸峰与其他离子色谱峰之间分离度良好,在10~30μg·ml~(-1)浓度范围内线性关系良好(r=0.999 9),定量限为0.116μg·ml~(-1),平均加样回收率为100.8%,RSD为1.2%(n=9)。根据试验结果,对离子色谱法测量中影响测量不确定度的因素进行了量化、评定与合成,给出扩展不确定度的结果报告。结论:建立的离子色谱方法简便、准确,专属性好,可用于测定甲磺酸倍他司汀中甲磺酸含量;通过不确定度评定中对各因素分量结果的分析,有助于减小测量不确定度,提高测定结果的准确可靠性。
OBJECTIVE: To establish a method for the determination of methanesulfonic acid in betahistine mesylate by ion chromatography and evaluate the uncertainty. Methods: Ion Pac AS11-HC (25 mm × 4.0 mm, 5 μm) anion chromatographic column was used with 12 mmol·L -1 sodium hydroxide solution as the eluent. The conductivity detector and the suppressor voltage of 30 m V. Results: The resolution of methanesulfonic acid peak was in good agreement with other ion chromatographic peaks. The linearity was good (r = 0.999 9) in the range of 10 ~ 30μg · ml ~ (-1) and the limit of quantification was 0.116μg · ml ~ (- 1) with an average recovery of 100.8% and a RSD of 1.2% (n = 9). According to the test results, the factors affecting the uncertainty of measurement in ion chromatography were quantified, evaluated and synthesized, and the results of the extended uncertainty were reported. Conclusion: The established ion chromatography method is simple, accurate and specific, and can be used to determine the content of mesylate in betahistine mesylate. The analysis of the results of the component factors in uncertainty assessment helps to reduce Measurement uncertainty, improve the accuracy and reliability of measurement results.