反相高效液相色谱法测定唑来膦酸及其制剂含量

Determination of zoledronic acid and its preparations by RP-HPLC

目的建立高效液相色谱测定唑来膦酸及其制剂含量。方法采用离子对反相高效液相色谱-蒸发光散射检测器检测法。固定相为BDSC8色谱柱(4.6mm×150mm,5μm),以甲醇-5mmol·L-1醋酸铵缓冲液配制的10mmol·L-1正戊胺溶液(醋酸调pH=7.0)(3:97)为流动相,流速1.0mL·min-1,柱温室温。结果唑来膦酸的浓度为99.04-891.4μg·mL-1时,线性关系良好(r=0.9999);注射用唑来膦酸的平均回收率为100.4%,RSD为0.76%(n=9);唑来膦酸注射液的平均回收率为100.2%,RSD为0.69%(n=9)。结论方法准确,操作简便,分析快速,适用于唑来膦酸原料药及制剂的含量测定。

OBJECTIVE: To establish a HPLC method for the determination of zoledronic acid and its preparations. METHODS: Ion-pair RP-HPLC coupled with evaporative light-scattering detection was performed on a BDS C8 column (4.6 mm × 150 mm, 5 μm) at room temperature. The mobile phase consisted of methanol-buffer solution (5 mmol&middotL-1 ammonium acetate and 10 mmol&middotL-1 amylamine, adjusted to pH 7.0 with acetic acid) (3:97), at a flow rate of 1.0 mL&middotmin-1. RESULTS: The calibration curve was linear in the range of 99.04-891.4 μg&middotmL -1 (r = 0.999 9). For zoledronic acid for injection, the average recovery was 100.4% with RSD of 0.76% (n = 9); for zoledronic acid injection, the average recovery was 100.2% with RSD of 0.69% (n = 9). CONCLUSION: The method is rapid, simple and accurate for the determination of zoledronic acid in material and in its preparations.