论文部分内容阅读
目的:建立离子色谱法测定枸橼酸氢钾钠颗粒中钠、钾和枸橼酸含量的方法。方法:钾和钠的色谱条件:采用Dionex Ion Pac CS12A色谱柱(250 mm×4.6 mm,5μm),流动相为0.02 mol·L~(-1)甲烷磺酸溶液,流速为1.0 ml·min~(-1),抑制器为CSRS 300,抑制电流为59 m A,采用抑制型电导检测器,进样量为25μl。枸橼酸的色谱条件:采用Dionex HPICE-AS1离子排斥色谱柱(250 mm×9.0 mm,7.5μm),流动相为0.015 mol·L~(-1)硫酸溶液,流速为0.6 ml·min~(-1),检测波长为220 nm,进样量为10μl。结果:钠的线性范围为0.82~82.49μg·ml~(-1)(r=0.999 9),平均回收率为98.9%,RSD为0.55%(n=9);钾的线性范围为1.38~137.89μg·ml~(-1)(r=1.000 0),平均回收率为100.5%,RSD为0.53%(n=9);枸橼酸的线性范围为0.021~10.600mg·ml~(-1)(r=1.000 0),平均回收率为99.1%,RSD为0.54%(n=9)。结论:本方法简便、快速、准确,可用于枸橼酸氢钾钠颗粒的质量控制。
Objective: To establish a method for the determination of sodium, potassium and citric acid in sodium hydrogen citrate granules by ion chromatography. Methods: The chromatographic conditions of potassium and sodium were as follows: Dionex Ion Pac CS12A (250 mm × 4.6 mm, 5 μm) was used as the mobile phase with 0.02 mol·L -1 methanesulfonic acid solution and the flow rate was 1.0 ml · min ~ (-1), suppressor CSRS 300, inhibit current 59 m A, using an inhibitory conductivity detector with an injection volume of 25 μl. The chromatographic conditions of citric acid were as follows: Dionex HPICE-AS1 ion-exclusion chromatography column (250 mm × 9.0 mm, 7.5 μm) was used. The mobile phase was 0.015 mol·L -1 sulfuric acid solution and the flow rate was 0.6 ml · min ~ -1), the detection wavelength was 220 nm, the injection volume was 10μl. Results: The linear range of sodium was 0.82-82.49 μg · ml -1 (r = 0.999 9) with an average recovery of 98.9% and a RSD of 0.55% (n = 9). The linear range of potassium was 1.38 ~ 137.89 The average recovery was 100.5% and the RSD was 0.53% (n = 9). The linear range of citric acid was 0.021-10.600 mg · ml -1, (r = 1.000 0) with an average recovery of 99.1% and a RSD of 0.54% (n = 9). Conclusion: The method is simple, rapid and accurate and can be used for the quality control of sodium hydrogen citrate granules.