[关键词]
[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-2 Hypersil柱(250 mm×4.6 mm,5 μm);流动相为甲醇–0.02 mol/L磷酸二氢钾缓冲液(pH 3.0)(45∶55);柱温为40 ℃;检测波长为215 nm;体积流量为1.3 mL/min;进样量为80 μL。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1.0~3.0 μg/mL具有良好的线性关系(r=0.999 6);检测限(S/N=3)为0.4 ng。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。
[Key word]
[Abstract]
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.
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[基金项目]
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)