药用辅料蔗糖中亚硫酸盐检测方法的建立  

Establishment of Sulfite Detection Method for Pharmaceutical Excipient Sucrose

作　　者：李樾[1] 许凯 宋晓松[1] 杨锐[1] 肖新月[1] 孙会敏[1] Li Yue;Xu Kai;Song Xiaosong;Yang Rui;Xiao Xinyue;Sun Huimin(National Institutes for Food and Drug Control NMPA Key Laboratory for Quality Research and Evaluation of Pharmaceutical Excipients,Beijing 100050,China)

机构地区：[1]中国食品药品检定研究院药用辅料质量研究与评价重点实验室,北京100050

出　　处：《中国药事》2021年第9期1046-1051,共6页Chinese Pharmaceutical Affairs

基　　金：药典会质量标准提高课题(编号2020Y015)。

摘　　要：目的:建立适宜的蔗糖中亚硫酸盐测定法,提高现行药典标准。方法:采用IonPac AS11-HC阴离子分析柱并配加IonPac AG11-HC保护柱,柱温25℃,以10.0 mmol·L^(-1)的KOH作为淋洗液,流速1.0 mL·min^(-1),检测器为电导检测器,检测器温度30℃,抑制器为自动再生抑制模式,抑制电流40mA,进样量25μL。结果:离子色谱法测定亚硫酸钠质量浓度在1~20μg·mL^(-1)范围内线性良好,回归方程为Y=0.0434X-0.0211,r=0.9993,精密度RSD为0.5%,稳定性RSD为1.5%,回收率范围为93.5%~99.3%,检出限0.1μg·mL^(-1),定量限0.25μg·mL^(-1)。8批样品中1号、2号、3号及5号样品结果分别为8.1、9.8、12.0及10.4μg·g^(-1),其余各批样品均为未检出亚硫酸盐。结论:所建方法可行、准确,可用于测定蔗糖中亚硫酸盐的含量。Objective:To establish a suitable method for the determination of sulfite in sucrose and improve the standard of current pharmacopoeia.Methods:IonPac AS11-HC anion analysis column and IonPac AG11-HC protection column were used.The column temperature was 25℃,and 10.0 mmol·L^(-1)KOH was used as the eluent.The flow rate was 1.0 mL·min^(-1).The detector was a conductivity one and the detector temperature was 30℃.The suppressor was an automatic regeneration inhibition mode.The inhibition current was 40 mA,and the injection volume was 25μL.Results:The determination of sulfite concentration by ion chromatography showed good linearity in the range of 1-20μg·m L^(-1).The regression equation was Y=0.0434 X-0.0211,r=0.9993.The RSD of precision was 0.5%,and the RSD of stability was 1.5%,and the recovery was 93.5%-99.3%.The limit of detection was 0.1μg·m L^(-1)and the limit of quantitation was 0.25μg·m L^(-1).The results of No.1,No.2,No.3 and No.5 samples were 8.1,9.8,12.0 and 10.4μg·g-1,respectively.No sulfite was detected in the other batches of samples.Conclusion:This method is feasible and accurate,which can be used to determine sulfite content in sucrose.

关 键 词：药用辅料 蔗糖 亚硫酸盐 离子色谱 

分 类 号：R917[医药卫生—药物分析学]