甲磺酸倍他司汀中甲磺酸的离子色谱法测定不确定度评定  

Uncertainty Evaluation in the Determination of Methane Sulfonic Acid in Betahistine Mesylate by Ion Chromatography

作　　者：丁文静[1] 陆明[1] 厉延春 顾颂青[1] 

机构地区：[1]上海市食品药品检验所,上海201203

出　　处：《中国药师》2016年第10期1969-1972,共4页China Pharmacist

摘　　要：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 an ion chromatography method for the determination of methane sulfonic acid in betahistine me- sylate and evaluate the uncertainty in the measurement. Methods： An ion chromatographic column IonPac AS11-HC （25mm×4.0mm,5μm） was used with 12 mmol . L-1 NaOH as the eluent and an electrical conductivity detector with the suppressor of 30 mV. Results： The results showed that methane sulfonic acid could be detected without any interference. The calibration curve was linear within the range of 10-30 μg . ml-1（r =0.999 9）and the LOQ was 0. 116μg . ml-1. The average recovery was 100.8% （RSD = 1.2%, n = 9）. Based on the results of experiments, the influencing factors of uncertainty in the measurement were quantitatively eval- uated. The expanded uncertainty was obtained. Conclusion： The method is simple, accurate and selective. It can be used for the de- termination of methane sulfonic acid in betahistine mesylate. Based on the evaluation of uncertainty, the analysis can help reduce the uncertainty in the measurement and improve the accuracy and reliability of the determination.

关 键 词：离子色谱 甲磺酸倍他司汀 甲磺酸 测定 测量不确定度 

分 类 号：R917[医药卫生—药物分析学]