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离子色谱法测定无水磷酸氢二钠中阴离子及不同级别产品质量比较 被引量:1

Quality Comparison of Different Grades of Anhydrous Sodium Hydrogen Phosphate through the Determination of Anions by Ion Chromatography
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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
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