目的 建立一種有效測定塞來昔布膠囊中有關物質的高效液相色譜法，并進行質量方法學研究。方法 采用Phenyl-2 Hypersil柱（250 mm×4.6 mm，5 μm）；流動相為甲醇–0.02 mol/L磷酸二氫鉀緩沖液（pH 3.0）（45∶55）；柱溫為40 ℃；檢測波長為215 nm；體積流量為1.3 mL/min；進樣量為80 μL。結果 4-[5-(2-甲基苯基)-3-(三氟甲基)-1H-吡唑-1-基]苯磺酰胺的質量濃度在1.0～3.0 μg/mL具有良好的線性關系（r=0.999 6）；檢測限（S/N=3）為0.4 ng。結論 本方法簡便準確、重現(xiàn)性好，精密度高，可有效地檢測塞來昔布膠囊中有關物質，并為塞來昔布的檢查和方法學研究提供了依據。

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.

國家重大新藥創(chuàng)制專項（2011ZX09-401-009，2011ZX09201-101-19，2012ZX09105102）；天津市科技支撐項目（09ZCKFSH01200）