目的 建立一種同時測定唑來膦酸原料藥及其粉針劑中的磷酸鹽和亞磷酸鹽的離子色譜方法。方法 采用Dionex^TMIonPac^TMAS18Analytical（250 mm×4 mm）色譜柱，Dionex^TMIonPac^TMAG18Analytical（50 mm×4 mm）為保護柱，以碳酸鈉和碳酸氫鈉水溶液為淋洗液進行等度洗脫，體積流量為1.0 mL·min^-1，采用抑制型電導(dǎo)檢測器檢測。結(jié)果 亞磷酸根和磷酸根與相鄰峰的分離效果良好，分離度均大于1.5。亞磷酸根和磷酸根分別在2.075～20.750 μg·mL^-1和2.000～20.000 μg·mL^-1范圍內(nèi)線性關(guān)系良好，相關(guān)系數(shù)均大于0.998 9；原料藥中亞磷酸根和磷酸根的回收率分別在94.7%～108.0%和98.4%～106.3%，回收率RSD分別為3.6%和2.3%；粉針劑中亞磷酸根和磷酸根回收率分別在93.9%～100.4%和98.2%～104.4%，回收率RSD分別為2.5%和1.9%；重復(fù)性、精密度、耐用性、溶液穩(wěn)定性均符合要求。3批原料藥及粉針劑中均未檢出亞磷酸根和磷酸根雜質(zhì)。結(jié)論 該方法準確、靈敏、操作簡單，適用于唑來膦酸及其粉針劑中磷酸鹽和亞磷酸鹽雜質(zhì)的質(zhì)控研究。

Objective A method for simultaneous determination of phosphate and phosphite in zoledronic acid and its powderinjection by ion chromatography was developed. Methods A DionexTMIonPacTMAS18Analytical (250 mm × 4 mm) column and a DionexTMIonPacTMAG18Analytical (50 mm×4 mm) guard column were used for isocratic elution with aqueous sodium carbonate and sodium bicarbonate as the eluent. The flow rate was 1.0 mL·min^-1, and the detection was performed with a suppression type conductivity detector. Results The separation of phosphite and phosphate from the surrounding peaks was good, and the separation was greater than 1.5. The linear ranges of phosphite and phosphate were 2.075 to 20.750 μg·mL^-1 and 2.000 to 20.000 μg·mL^-1, respectively, with the correlation coefficients R² greater than 0.998 9. The recovery rates of phosphates and phosphates in the raw materials are 94.7% to 108.0% and 98.4% to 106.3%, respectively, with RSDs of 3.6% and 2.3%. The recovery rates of phosphates and phosphates in the powder injection were 93.9% to 100.4% and 98.2% to 104.4%, respectively, with RSDs of 2.5% and 1.9%; The repeatability, precision, durability, and solution stability all meet the requirements. No phosphite and phosphate impurity were detected in the 3 batches of raw materials and powder injection. Conclusion The method is accurate, sensitive,simple to operate, and is suitable for the quality control of phosphate and phosphite impurities in zoledronic acid and its powder injection.

R932

江蘇省產(chǎn)教融合一流課程《藥物分析》建設(shè)項目；江蘇海洋大學(xué)專業(yè)學(xué)位研究生課程案例庫建設(shè)項目（YJSZY202102）；江蘇海洋大學(xué)2023年一流課程《藥物儀器分析》建設(shè)項目；連云港市政策引導(dǎo)產(chǎn)學(xué)研項目（CYX2202）