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.pdfVIP

中国药师　 　 2016年第19卷第10期　 　 China Pharmacist2016,Vol.19　 No.10 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 丁文静　 陆明　 厉延春　 顾颂青　 (上海市食品药品检验所,上海　 201203) 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IonPac AS11-HC -1 (25 mm×4.0 mm,5 μm)阴离子色谱柱,以12 mmol ·L 氢氧化钠溶液为淋洗液,采用电导检测器,抑制器电压30 mV。 结 -1 果:甲磺酸峰与其他离子色谱峰之间分离度良好,在 10 ~30 μg ·ml 浓度范围内线性关系良好(r =0.999 9),定量限为 -1 0.116 μg ·ml ,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。 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 中图分类号:R917　 文献标识码:A　 　 文章编号:1008-049X(2016)10-1969-04 Uncertainty EvaluationintheDeterminationofMethaneSulfonicAcidinBetahistineMesylatebyIonChro- matography Ding Wenjing,Lu Ming,Li Yanchun,Gu Songqing (Shanghai Institutefor Food and Drug Control,Shanghai201203,China) ABSTRACT　 Objective:Toestablishanionchromatographymethodforthedeterminationofmethanesulfonicacidinbetahistineme- sylate and evaluate the uncertainty in the measurement. Methods: An ion chromatographic column IonPac AS11-HC(25 mm × -1 4.0 mm,5 μm)wasusedwith 12 mmol ·L NaOHastheeluentandanelectricalconductivitydetectorwiththesuppressorof30 mV. Results:The results showed that methane sulfonic acid could be detected without any interference. The calibration curve was linear -1 -1 within the range of 10-30 μg ·ml (r =0.999 9)and the LOQ was0.116 μg ·ml . The average recovery was 100.8% (RSD = 1.2%,n=9). Based ontheresultsof experiments,theinfluencingfactorsofuncertainty inthemeasurementwerequantitatively eval- uated. The expanded uncertainty was obtained.Conclusion:The method is simple,accurate and selective. It can be usedfor the de- termination of methane sulfonic acid in betahistine mesylate. Based on the evalua