Determination of Related Substances in Ibandronate Sodium Raw Materials by Ion Suppression Chromatography / 中国药房

ABSTRACT

OBJECTIVE:To adopt ion suppression chromatography to determine related substance in ibandronate sodium raw materials.METHODS:The separation was performed on a Dionex IonPac AS11-HC column with mobile phase consisted of potassium hydroxide (gradient elution) at the flow rate of 1.1 mL/min.The column temperature was set at 45 ℃,and sample size was 20 μL.Suppressed conductivity detector was adopted with temperature of 35 ℃.RESULTS:The linear ranges of phosphite,impurity Ⅰ and phosphate were 3.08-30.83 μg/mL(r=0.999 9),2.84-28.43 μg/mL(r=0.999 1),2.95-29.52 μg/mL(r=0.999 9),respectively.The limits of quantitation were 2.47,56.7,3.31 ng,and the limits of detection were 0.75,17.2,1.0 ng.RSDs of precision,stability and reproducibility tests were all lower than 4.0％.The recoveries were 101.49％-103.57％ (RSD=0.7％,n=9),100.00％-104.85％ (RSD=1.8％,n=9),101.35％-104.08％ (RSD=0.9％,n=9),respectively.CONCLUSIONS:The method is simple,accurate and sensitive,and is suitable for the determination of related substance in ibandronate sodium raw materials.