| 英文摘要 |
An HPLC assay method for determining the degradation of zomepirac was developed and validated under acidic, basic, and photoirradiated conditions. The HPLC system consisted of an Inertsil 5 ODS-3V column (4.6 ¥ 250 mm i.d.), and a guard column of Inertsil 7 ODS-3V (4.6 ¥ 50 mm i.d.) using a mobile phase of CH3CN: CH3OH: 1%HOAc (2:64:34, v/v/v) with UV detection at 254 nm. The developed method satisfies the system suitability criteria, peak integrity, and resolution for the parent drug and its degradants. The results indicate that the established assay method shows good selectivity and specificity suitable for stability measurements of zomepirac. From the intra- and interday tests of 6 replicates, the coefficients of variations (CVs) were between 0.12% and 2.24% for the former and 0.15% and 3.93% for the latter. Recoveries were found to be between 97.14% and 101.58%. From the stress treatments, zomepirac was determined to be more sensitive to the light and acidic conditions, but it was stable in basic medium. A preliminary kinetic study of the photodegradation of zomepirac in methanol showed that it followed an apparent first-order reaction.
本研究已發展出在酸、檢和照光條件下，以安定性指標的高壓液相層析法來定量佐美酸（Zomepirac）的降解情況並予確效。本高壓液相層析法系統使用Inertsil 50DS-3V 管柱（4.6公釐內徑×250公釐）及另一Inertsil 7ODS-3V保護管柱（4.6公釐內徑×50公釐）。移動相組成為乙腈：甲醇：1%醋酸（2: 64: 34，v／v／v），UV偵測器設定為254 mn。本法合乎光解產物和原料藥之系統合適規範，波峰純度完整性及高解析度。本分析結果顯示新建立之定量法具良好選擇性和專一性，適合用以測定佐美酸的安定性。從日內及日間各六重複之差異分析：前者標準誤差介於0.111及0.272之間，而變異係數介於0.12%及2.24%；後者標準誤差介於0.152及0.387之間，而變異係數介於0.15%及3.93%。佐美酸回收率亦在97.14%及101.58%之間。從虐待試驗結果可發現佐美酸對照光及在酸性溶液中較敏感，但對鹼性溶液較安定。佐美酸在甲醇溶媒的光降解初步動力學結果遵守一階次反應模式。 |
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