HPLC法测定塞来昔布原料药中有关物质
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摘要
目的建立测定塞来昔布原料药中有关物质的高效液相色谱(HPLC)法。方法建立HPLC法,采用Century SIL C30色谱柱(250mm×4.6mm,5μm),流动相:水(A)–乙腈(B)–甲醇(C),梯度洗脱;体积流量:1.0mL/min;检测波长:215 nm;柱温:25℃;进样量:20μL。结果塞来昔布与各杂质的分离度良好,且在一定浓度范围内线性关系良好。塞来昔布和杂质A、B、C、D、F的定量限分别为198.0、161.2、240.0、239.4、203.5、156.8 ng/mL,检测限分别为40.3、50.0、39.9、61.0、39.2、24.8ng/mL。结论本法操作简单,准确度、灵敏度高,可用于塞来昔布原料药中有关物质的分离检测。
Objective To establish an HPLC method for determination of the related substances in celecoxib active pharmaceutical ingredients. Methods HPLC method was established. The determination was carried out on Century SIL C30 column(250 mm × 4.6 mm, 5 μm). The mobile phase consisted of water-acetonitrile-methanol with gradient elution. The flow rate was 1.0 mL/min. The detective wavelength was set at 215 nm, column temperature was 25 ℃, and the injection volume was 20 μL. Results Celecoxib and its related impurities had good separation, and there were good linear relationship within a certain concentration ranges. The quantitative limits of cecoxib and impurity A, B, C, D, and F were 198.0, 161.2, 240.0, 239.4, 203.5, and 156.8 ng/mL, respectively.The detection limits were 40.3, 50.0, 39.9, 61.0, 39.2, and 24.8 ng/mL. Conclusion The method is simple, accurate, sensitive, and suitable for the determination of related substances in celecoxib active pharmaceutical ingredients.
Objective To establish an HPLC method for determination of the related substances in celecoxib active pharmaceutical ingredients. Methods HPLC method was established. The determination was carried out on Century SIL C30 column(250 mm × 4.6 mm, 5 μm). The mobile phase consisted of water-acetonitrile-methanol with gradient elution. The flow rate was 1.0 mL/min. The detective wavelength was set at 215 nm, column temperature was 25 ℃, and the injection volume was 20 μL. Results Celecoxib and its related impurities had good separation, and there were good linear relationship within a certain concentration ranges. The quantitative limits of cecoxib and impurity A, B, C, D, and F were 198.0, 161.2, 240.0, 239.4, 203.5, and 156.8 ng/mL, respectively.The detection limits were 40.3, 50.0, 39.9, 61.0, 39.2, and 24.8 ng/mL. Conclusion The method is simple, accurate, sensitive, and suitable for the determination of related substances in celecoxib active pharmaceutical ingredients.
引文
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[6]杨佳,岳金波,孙菊杰,等.塞来昔布对Fa Du人咽鳞癌裸鼠移植瘤放疗过程中肿瘤再增殖抑制效应[J].中华肿瘤防治杂志,2017,24(19):1349-1356.
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[8]吕苗苗,陈华宝,李海泉等.塞来昔布的合成[J].北京化工大学学报,2005,32(6):97-98.
[9]蒋振东,杨琳,卢巍.塞来昔布有关物质的HPLC法测定[J].中国医药工业杂志,2018,49(9):1295-1299.
[2]梅之南,施震,汪细和,等.COX-2抑制剂Celecoxib的合成[J].中国医药工业杂志,2000,31(10):433-434.
[3]董亚琳,罗秦英,姚鸿萍,等.塞来昔布的药理作用、药代动力学及临床评价[J].中国医院用药评价与分析,2002,2(5):274-276.
[4]吕双丛,曹瑞丽.塞来昔布治疗风湿性关节炎和骨关节炎的疗效观察[J].中国医院用药评价与分析,2015,15(10):1296-1299.
[5]Lu Y,Liu X F,Liu T R,et al.Celecoxib exerts antitumor effects in HL-60 acute leukemia cells and inhibits autophagy by affecting lysosome function[J].Biomed Pharmacother,2016(84):1551-1557.
[6]杨佳,岳金波,孙菊杰,等.塞来昔布对Fa Du人咽鳞癌裸鼠移植瘤放疗过程中肿瘤再增殖抑制效应[J].中华肿瘤防治杂志,2017,24(19):1349-1356.
[7]崔志艳.塞来昔布合成方法与杂质研究[D].石家庄:河北科技大学,2013.
[8]吕苗苗,陈华宝,李海泉等.塞来昔布的合成[J].北京化工大学学报,2005,32(6):97-98.
[9]蒋振东,杨琳,卢巍.塞来昔布有关物质的HPLC法测定[J].中国医药工业杂志,2018,49(9):1295-1299.