摘要
目的建立HPLC测定赛利司他有关物质的方法。方法采用Agilent Phenyl色谱柱(250 mm×4.6 mm,5μm),以5 mmol·L^(-1)磷酸二氢钾(用10%磷酸调pH值至4.0)-乙腈为流动相进行梯度洗脱,流速为1.0 m L·min^(-1),检测波长为226nm。结果各杂质与主峰之间的分离度良好。开环杂质(杂质A)、2-十七烷基氧-6-甲基-4氢-3,1-苯并噁嗪-4-酮(杂质B)、2-十八烷基氧-6-甲基-4氢-3,1-苯并噁嗪-4-酮(杂质C)浓度分别在0.049 5~1.981μg·m L^(-1),0.059 9~0.399 1μg·m L-1,0.059 6~0.397 5μg·m L^(-1)内与峰面积呈良好的线性关系,r均为0.999 9;杂质A、B、C加样回收率的平均值分别为104.2%,107.0%和107.8%,RSD分别为2.09%,1.77%和2.18%。结论本方法简便、准确可靠,适用于赛利司他中有关物质的控制。
OBJECTIVE To establish an HPLC method for determining the contents of the related substances of cetilistat. METHODS The condition of detection were as follows： Agilent Phenyl column（250 mm×4.6 mm, 5 μm）, the gradient mobile phase consisted of 5 mmol·L^-1 potassium dihydrogen phosphate（adjust with 10% phosphoric acid to p H 4.0） and acetonitrile with a flow rate of 1.0 m L·min^-1, the UV detection wavelength was 226 nm. RESULTS The resolution of cetilistat and relate substances was good. The calibration curves were linear in the range of 0.049 5-1.981 0 μg·m L^-1 for impurity A（r=0.999 9）; the calibration curves were linear in the range of 0.059 9-0.399 1 μg·m L^-1 for impurity B（r=0.999 9）; the calibration curves were linear in the range of 0.059 6-0.397 5 μg·m L^-1 for impurity C（r=0.999 9）. The average recoveries of impurity A, impurity B and impurity C were 104.2%, 107.0% and 107.8% respectively; the RSDs were 2.09%, 1.77% and 2.18%, respectively. CONCLUSION The method is simple, accurate, reliable and can be used for the quality control of the related substances of cetilistat.
出处
《中国现代应用药学》
CAS
CSCD
2017年第3期399-402,共4页
Chinese Journal of Modern Applied Pharmacy
