离子色谱法同时测定低分子量肝素钠注射液中的有机酸和无机阴离子  

Determination of organic acids and inorganic anions in low molecular weight heparin sodium injection by ion chromatography

作　　者：肖菁 王蓉蓉 张俊 谢莹莹 李子珊 黄舒 姚静[3] XIAO Jing;WANG Rong-rong;ZHANG Jun;XIE Ying-ying;LI Zi-shan;HUANG Shu;YAO Jing(Hunan Institute for Drug Control,Changsha 410001;Hunan Drug Inspection Center,Changsha 410001;National Institutes for Food and Drug Control,Beijing 102629)

机构地区：[1]湖南省药品检验检测研究院,长沙410001 [2]湖南省药品审核查验中心,长沙410001 [3]中国食品药品检定研究院,北京102629

出　　处：《中南药学》2024年第8期2187-2190,共4页Central South Pharmacy

基　　金：湖南省自然科学基金部门(省药监局)联合基金(No.2022JJ80071)。

摘　　要：目的建立同时测定低分子量肝素钠注射液中醋酸根离子、氯离子、亚硫酸根离子、硫酸根离子和草酸根离子含量的离子色谱法。方法色谱柱为Dionex IonPac AS11(250 mm×4 mm),保护柱为Dionex IonPac AG11(50 mm×4 mm),用淋洗液自动发生器,采用氢氧化钾梯度洗脱,流速为1.0 mL·min^(-1),检测器为配有化学抑制器的电导检测器。结果醋酸根离子、氯离子、亚硫酸根离子、硫酸根离子和草酸根离子分别在0.12~24μg·mL^(-1)、0.24~48μg·mL^(-1)、0.4~80μg·mL^(-1)、0.04~8μg·mL^(-1)、0.3~60μg·mL^(-1)与测定值线性关系良好,r分别为0.9991、0.9999、0.9999、0.9995、0.9995;加样回收率分别为105.3%、101.0%、102.3%、96.8%和108.3%(n=6),RSD分别为2.2%、1.8%、1.6%、2.6%和1.6%。结论该方法操作简便,灵敏,高效,可用于同时测定低分子量肝素钠注射液中醋酸根、亚硫酸根、硫酸根、草酸根和氯离子的含量,为其质量提供保证。Objective To establish an ion chromatography to simultaneously determine acetate ion,chloride ion,sulfurous acid ion,sulfate ion and oxalate ion in low molecular weight heparin sodium injection.Methods The chromatographic column was Dionex IonPack AS11(250 mm×4 mm),and the protective column was Dionex IonPack AG11(50 mm×4 mm).The automatic eluent generator and the gradient elution of potassium hydroxide were used.The flow rate was 1.0 mL·min^(-1).A conductivity detector was used with a chemical inhibitor.Results The method showed good linearity at 0.12~24μg·mL^(-1)for acetate ion(r=0.9991),0.24~48μg·mL^(-1)for chloride ion(r=0.9999),0.4~80μg·mL^(-1)for sulfurous acid ion(r=0.9999),0.04~8μg·mL^(-1)for sulfate ion(r=0.9995),and 0.3~60μg·mL^(-1)for oxalate ion(r=0.9995),respectively.The average recoveries(n=6)were 105.3%(RSD=2.2%),101.0%(RSD=1.8%),102.3%(RSD=1.6%),96.8%(RSD=2.6%),and 108.3%(RSD=1.6%)for acetate ion,chloride ion,sulfurous acid ion,sulfate ion and oxalate ion,respectively.Conclusion The method is simple,sensitive and efficient,which can be used to simultaneously determine the content of acetate,sulfurous acid,sulfate,oxalate and chloride ions in low molecular weight heparin sodium injection,and to control its quality.

关 键 词：离子色谱法 低分子量肝素钠注射液 醋酸根离子 氯离子 亚硫酸根离子 硫酸根离子 草酸根离子 

分 类 号：R927[医药卫生—药学]