摘要
目的:建立离子色谱法同时测定无水磷酸氢二钠中的氟离子、氯离子、硝酸根和硫酸根离子的含量,并评价不同级别无水磷酸氢二钠的质量状况。方法:采用Dionex Ion Pac AS18(4 mm×250 mm)色谱柱,以10,40 mmol·L^-1氢氧化钾淋洗液梯度洗脱,流速为1.0 ml·min^-1,进样量为25μl。结果:氟离子、氯离子、硝酸根和硫酸根离子质量浓度分别在0.02~0.40,0.01~0.80,0.06~1.00和0.10~5.00μg·ml^-1范围内与峰面积均呈良好线性关系,r分别为0.9995,0.9997,0.9999和0.9995,平均回收率分别为92.26%,93.17%,99.80%,91.81%,RSD分别为0.87%,2.32%,3.07%,1.49%(n=6),供试品溶液在30 h内稳定。结论:本方法准确度高、重复性好,可用于测定无水磷酸氢二钠中的氟离子、氯离子、硝酸根和硫酸根离子的含量,为建立无水磷酸氢二钠的质量标准提供参考。
Objective:To establish a method for the content determination of fluoride ion,chloride ion,nitrate ion and sulfate ion in anhydrous sodium hydrogen phosphate by ion chromatography,and evaluate the quality of different grades of anhydrous sodium hydrogen phosphate.Methods:The column was a Dionex Ion Pac AS18(4 mm×250 mm)using 10 and 40 mmol·L^-1 potassium hydroxide as the mobile phase with gradient elution,the flow rate was 1.0 ml·min^-1,and the injection volume was 25μl.Results:The concentration of fluoride ion,chloride ion,nitrate ion and sulfate ion in disodium hydrogen phosphate and anhydrous sodium hydrogen phosphate was within the range of 0.02-0.40,0.01-0.80,0.06^-1.00 and 0.10-5.00μg·ml^-1,respectively,and all showed good linear relationship with the correlation coefficient of 0.9995,0.9997,0.9999 and 0.9995,respectively.The average recovery was 92.26%,93.17%,99.80%and 91.81%,and the RSDs were 0.87%,2.32%,3.07%and 1.49%(n=6),respectively.The test solution was stable within 24 h.Conclusion:The method has high accuracy and good reproducibility,and can be used for determining the contents of fluoride ion,chloride ion,nitrate ion and sulfate ion in anhydrous sodium hydrogen phosphate,which provides reference for establishing the quality standard of anhydrous sodium hydrogen phosphate.
作者
李颖
刘雁鸣
Li Ying;Liu-Yanming(Hunan Institute for Drug Control,Changsha 410001,China)
出处
《中国药师》
CAS
2019年第12期2328-2331,共4页
China Pharmacist
关键词
无水磷酸氢二钠
离子色谱法
氟离子
氯离子
硝酸根
硫酸根离子
Anhydrous disodium hydrogen phosphate
Ion chromatography
Fluoride ion
Chloride ion
Nitrate ion
Sulfate ion