柱后衍生离子色谱法测定氯膦酸二钠注射液的含量

Aanalysis of disodium clodronate injection by ion-exchange chromatography with post-column derivatization

目的建立氯膦酸二钠注射液的含量测定方法。方法采用阴离子交换色谱柱分离，用衍生溶液在线柱后衍生，再进行紫外检测。色谱柱为阴离子交换柱（DIONEX Ion Pac AS7分离柱，10μm，4mm×25cm；DIONEX Ion Pac AG7预柱）；流动相为40mmol／L硝酸溶液，流速0.5mL／min；柱后衍生溶液为含有高氯酸的硝酸铁溶液，流速为0．25mL／min；检测波长为300nm。结果氯膦酸二钠在100～300μg／mL的浓度范围内有良好的线性关系，回归方程为P=0．00013014A＋23．952，r=0．9999（n=7）；平均回收率为101．85％，RSD=1．2％（n=9）。结论该方法简捷、快速、准确度高，可用于氯膦酸二钠注射液的质量控制。

Objective To establish a method for the content determination of disodium clodronate in disodium clodronate injection. Methods The separation was performed on an anion-exchange column （DIONEX IonPac AS7 analytical column, 10μm,4 mm × 25 cm; DIONEX IonPac AG7 guard columns）. Derivatization solution was used for post-column derivatization online. A UV-detector was used for detection. The mobile phase consisted of 40 mmol/L HNO3 solution. The flow was 0.5 ml/min. The post-derivatization solution was ferric nitrate solution containing perchloric acid, and flow was 0.25 ml/min. The detective wavelength was 300 nm. Results Disocliu clodronate was linear in the range of 100 -300μg/ml（ r = 0. 9999,n = 7）. The average recovery was 101.85% with RSD of 1.2% （n =9）. Conclusion This method is simple,fast and reliable for the quality control of disodium clodronate injection.