摘要
目的:建立测定磷酸西他列汀含量的高效液相色谱法。方法:采用SymmetryC18柱(150mm×4.6mm,5μm);流动相为甲醇-0.1%高氯酸水溶液(32∶68),流速:1.0mL·min-1,检测波长:268nm,柱温:30℃。结果:磷酸西他列汀的浓度在0.5～500μg·mL-1范围内线性良好(r=0.9996);方法的最低检测限为1ng(S/N=3);高、中、低3个浓度的平均回收率(n=5)分别为99.4%(RSD=0.22%),98.9%(RSD=0.34%),99.3%(RSD=0.10%);各杂质峰与主峰达到基线分离。结论:此方法操作简便、灵敏、准确,重复性好,适用于磷酸西他列汀的含量测定,可作为该药质量控制的检测方法。
Objective： To establish an RP-HPLC method for determination of the content of sitagliptin phosphate. Methods： The column was Symmetry C18 （150mm×4.6mm, 5μm）, the mobile phase consisted of methanol - 0.1% perchloric acid solution （32：68） with a flow rate of 1.0mL·min-1, the UV detection wavelength was set at 268nm. Results： The calibration curve was linear within the range of 0.5 to 500 μg/mL （r= 0.9996）; the lowest limit determination was 1ng （S/N=3）. The mean recoveries （n=3） of high, middle and low concentration were 99.4% （RSD=0.22%）, 98.9% （RSD=0.34%）, 99.3% （RSD=0.10%）; the chromatographic peaks of sitagliptin phosphate and its related substances were well isolated. Conclusion： The method is simple, selective, accurate, reproducible. It is suitable for determination of the content of sitagliptin phosphate.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2009年第8期1370-1372,共3页
Chinese Journal of Pharmaceutical Analysis
