| 引用本文: | 张立波,陈蓓,汤谷平.HPLC测定赛利司他有关物质及降解产物[J].中国现代应用药学,2017,34(3):399-402. |
| ZHANG libo,CHEN bei,TANG guping.Determination of the Related Substances of Cetilistat by HPLC[J].Chin J Mod Appl Pharm(中国现代应用药学),2017,34(3):399-402. |
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| HPLC测定赛利司他有关物质及降解产物 |
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张立波1,2, 陈蓓1,2, 汤谷平3
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1.浙江大学药学院, 药学院, 杭州 310000;2.杭州华东医药集团新药研究院有限公司, 杭州 310000;3.浙江大学药学院, 化学生物和药物研究所, 杭州 310000
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| 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，5 μm），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 mL·min-1，检测波长为226 nm。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 5~1.981 μg·mL-1，0.059 9~0.399 1 μg·mL-1，0.059 6~0.397 5 μg·mL-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。 |
| 关键词: 赛利司他 高效液相色谱法 有关物质 |
| DOI：10.13748/j.cnki.issn1007-7693.2017.03.021 |
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| Determination of the Related Substances of Cetilistat by HPLC |
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ZHANG libo1,2, CHEN bei1,2, TANG guping3
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1.Zhejiang University, School of Pharmaceutical Sciences, Hangzhou 310000, China;2.East China Pharmaceutical Group New Grug Institute Limited Co., Ltd., Hangzhou 310000, China;3.Zhejiang University, Institute of Chemical Biology and Pharmaceutical Chemistry, Hangzhou 310000, China
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| Abstract: |
| 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 pH 4.0) and acetonitrile with a flow rate of 1.0 mL·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·mL-1 for impurity A (r=0.999 9); the calibration curves were linear in the range of 0.059 9-0.399 1 μg·mL-1 for impurity B (r=0.999 9); the calibration curves were linear in the range of 0.059 6-0.397 5 μg·mL-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. |
| Key words: cetilistat HPLC related substances |
