离子色谱法测定雷尼替丁原料药及制剂中亚硝酸根含量

Content Determination of Nitrite Ion in Ranitidine Raw Materials and Preparations by Ion Chromatography

目的建立测定雷尼替丁原料药及制剂中亚硝酸根(NO_(2)^(-))含量的离子色谱法。方法色谱柱为IonPac AS19柱(250 mm×4 mm,7.5μm),流动相为5~35 mmol/L氢氧化钾溶液(梯度洗脱),流速为1.2 m L/min,柱温为30℃,进样量为100μL。结果亚硝酸盐标准溶液的质量浓度在6.25~1 000.00 ng/m L范围内与峰面积线性关系良好(R^(2)=1.000 0,n=8);精密度、重复性试验结果的RSD均小于2.0%(n=6);盐酸雷尼替丁原料药、盐酸雷尼替丁胶囊、枸橼酸铋雷尼替丁片的平均回收率分别为95.50%,97.69%,98.20%,RSD分别为1.52%,0.83%,1.14%(n=6)。结论该方法结果准确,稳定性和重复性均较好,可用于雷尼替丁原料药及制剂中NO2-含量的测定。

Objective To establish an ion chromatography method for the content determination of nitrite ion(NO_(2)^(-))in ranitidine raw materials and preparations.Methods The chromatographic column was IonPac AS19 column(250 mm×4 mm,7.5μm),the mobile phase was 5-35 mmol/L potassium hydroxide solution(gradient elution),the flow rate was 1.2 mL/min,the column temperature was 30℃,and the injection volume was 100μL.Results The linear range of nitrite standard solution was 6.25-1000.00 ng/mL(R^(2)=1.0000,n=8).The RSDs of precision and repeatability tests were less than 2.0%(n=6).The average recoveries of nitrite in ranitidine hydrochloride raw materials,Ranitidine Hydrochloride Capsules and Ranitidine Bismuth Citrate Tablets were 95.50%,97.69%,98.20%with RSDs of 1.52%,0.83%and 1.14%(n=6),respectively.Conclusion The method is accurate,stable and reproducible,which can be used for the content determination of NO_(2)^(-)in ranitidine raw materials and preparations.