离子色谱法分析微晶纤维素的离子分布及与其电导率的相关性研究  

Study of ion distribution in microcrystalline cellulose and its correlation with conductivity using ion chromatography

作　　者：刘静兰 王珏[2] 陈惠玲 郑淑凤 杨锐[2] 赵霞[2] LIU Jing-lan;WANG Jue;CHEN Hui-lin;ZHENG Shu-feng;YANG Rui;ZHAO Xia(Xiamen Institute for Food and Drug Control,Xiamen 361012,China;National Medical Products Administration Key Laboratory for Quality Research and Evaluation of Pharmaceutical Excipients,National Institutes for Food and Drug Control,Beijing 100050,China)

机构地区：[1]厦门市食品药品质量检验研究院,厦门361012 [2]国家药品监督管理局药用辅料质量研究与评价重点实验室/中国食品药品检定研究院,北京100050

出　　处：《中国新药杂志》2025年第3期304-311,共8页Chinese Journal of New Drugs

摘　　要：目的:建立离子色谱法分别测定微晶纤维素中5种阴离子(CH 3COO^(-),HCOO^(-),Cl^(-),NO_(3)^(-),SO 4^(2-))和5种阳离子(Na^(+),NH_(4)^(+),K^(+),Mg^(2+),Ca^(2+))的含量,探究微晶纤维素电导率变化与其离子浓度变化之间的关系,并为其质量控制方法提供建议。方法:阴离子测定采用Dionex IonPac AS19色谱柱(250 mm×4.0 mm,5μm),ASRS 300(4 mm)型抑制器,以15 mmol·L^(-1)氢氧化钾为淋洗液;阳离子测定采用Dionex IonPac CS12A色谱柱(250 mm×4.0 mm,5μm),CSRS 300(4 mm)型抑制器,以15 mmol·L^(-1)甲基磺酸为淋洗液;流速为1.0 mL·min^(-1),检测方式为抑制电导检测(抑制电流:44 mA),检测池温度为35℃,柱温为30℃,进样量为25μL,按标准曲线法定量10种离子浓度。基于微晶纤维素稳定性实验不同时间点测得的电导率,通过灰色关联模型分析其与各离子浓度之间的灰色关联度。结果:10种离子的质量浓度与其峰面积呈良好的线性关系,相关系数r均>0.999,定量限为0.02~2.81 ng,检测限为0.01~0.89 ng,平均回收率为92.8%~101.3%(n=6)。微晶纤维素电导率变化与Na^(+)和Cl^(-)的关联系数最大。结论:该方法简便快速、专属性和通用性强,适用于微晶纤维素多种阴阳离子的测定,对电导率与离子分布的灰色关联度分析为其质量控制提供数据参考。Objective:To develop ion chromatography methods for the determination of five anions(CH 3COO^(-),HCOO^(-),Cl^(-),NO_(3)^(-),SO 4^(2-))and five cations(Na^(+),NH_(4)^(+),K^(+),Mg^(2+),Ca^(2+))in microcrystalline cellulose,to investigate the relationship between changes in conductivity and ion concentrations,and to provide suggestions for its quality control measures.Methods:The determination of anions was performed using a Dionex IonPac AS19 column(250 mm×4.0 mm,5μm)equipped with an ASRS 300 suppressor(4 mm)and utilizing 15 mmol·L^(-1)potassium hydroxide as the eluent.For cation ayalysis,a Dionex IonPac CS19 column(250 mm×4.0 mm,5μm)was used with a CSRS 300 suppressor(4 mm)and 15 mmol·L^(-1)methane sulfonic acid serving as the eluent.The flow rate was maintained at 1.0 mL·min^(-1),the suppression conductivity detection(current of suppressor was 44 mA)was used,the conductivity cell temperature was 35℃,the column temperature was kept at 30℃,the injection volume was 25μL,and the quantitative concentrations of 10 ions were determined using standard curve methodology.Based on the conductivity values at different time points in the stability test of microcrystalline cellulose,grey correlation analysis between conductivity and ion concentration was performed using a grey correlation model.Results:The mass concentration of 10 ions showed a good linear relationship with their respective peak areas,with all correlation coefficients above 0.999.The limits of quantitation ranged 0.02~2.81 ng,while the limits of detection ranged 0.01~0.89 ng,and the average recoveries were 92.8%~101.3%(n=6).The changes in conductivity of microcrystalline cellulose has a significant correlation coefficient with both Na^(+)and Cl^(-).Conclusion:This method is simple,rapid,specific and universally applicable,making it suitable for the determination of multiple anions and cations in microcrystalline cellulose,while grey correlation analysis between conductivity and ion distribution provides data reference for its quality control.

关 键 词：微晶纤维素 电导率 离子色谱法 灰色关联度 

分 类 号：R927.2[医药卫生—药学]