HPLC法测定塞来昔布胶囊中有关物质  

Determination of related substances in Celecoxib Capsule by HPLC

作　　者：高洁[1] 曹光[2] 张晓东[2] 任晓文[2] 

机构地区：[1]天津中医药大学研究生院,天津300193 [2]天津药物研究院,天津300193

出　　处：《现代药物与临床》2013年第2期182-184,共3页Drugs & Clinic

基　　金：国家重大新药创制专项(2011ZX09-401-009;2011ZX09201-101-19;2012ZX09105102);天津市科技支撑项目(09ZCKFSH01200)

摘　　要：目的建立一种有效测定塞来昔布胶囊中有关物质的高效液相色谱法,并进行质量方法学研究。方法采用Phenyl-2Hypersil柱(250mm×4.6mm,5μm);流动相为甲醇-0.02mol/L磷酸二氢钾缓冲液(pH3.0)(45:55);柱温为40℃;检测波长为215nm;体积流量为1.3mL/min;进样量为80μL。结果 4-[5-(2-甲基苯基)-3-(三氟甲基)-1H-吡唑-1-基]苯磺酰胺的质量浓度在1.0～3.0μg/mL具有良好的线性关系(r=0.9996);检测限(S/N=3)为0.4ng。结论本方法简便准确、重现性好,精密度高,可有效地检测塞来昔布胶囊中有关物质,并为塞来昔布的检查和方法学研究提供了依据。Objective To establish an HPLC method for the determination of related substances in Celecoxib Capsule and to study on quality by methodology.Methods The separation was performed on a Phenyl-2 Hypersil column（250 mm × 4.6 mm,5 μm）;The mobile phase was methanol-0.02 mol/L monobasic potassium phosphate buffer（45：55,adjusted to pH 3.0 with phosphoric acid） at a flow rate of 1.3 mL/min;The detection wavelength was 215 nm.The column temperature was 40 ℃,and the injection volume was 80 μL.Results The linear range of 4-[5-（2-methyl phenyl）-3-（triflorine methyl）-1H-pyrazole-1-based] benzene sulfonamide was 1.0—3.0 μg/mL（r = 0.999 6）.The detection limit（S/N = 3） was 0.4 ng.Conclusion This method is simple,accurate,reproducible,and suitable for the determination of related substances in Celecoxib Capsule,which provides a reliable method for the sample examination and methodological study on celecoxib.

关 键 词：塞来昔布胶囊 4-[5-(2-甲基苯基)-3-(三氟甲基)-1H-吡唑-1-基]苯磺酰胺 有关物质 高效液相色谱 

分 类 号：R927.2[医药卫生—药学]