以三氟乙丙酮（TRIFLUOROACETYLACETONE）為衍生試劑，運用毛細管氣相層析法對藥品製劑及血液中之異菸鹼酸胺（ISONIZIDE）檢測方法之建立   全文下載

Capillary Gas Chromatographic Determination of Isoniazid in Pharmaceutical Preparations and Blood by Precolumn Derivatization with Trifluoroacetylacetone

異菸鹼酸胺（Isoniazid, INH）及聯胺（Hydrazine, HZ）2種抗結核藥物經三氟乙丙酮trifluoroacetylacetone（FAA）做通過層析管柱前之衍生化（Precolumn derivatization）後，以毛細管管柱-氣相層析儀完成分析檢驗。以型號HP-5（30m長 × 0.32mm 內徑）毛細管柱及火焰離子偵檢器（FID）之層析條件來分析苯聯胺Phenylhydrazine（PHZ）與INH及HZ時，3者都能同時的完全分離開來，因此以PHZ做為內部標準品。對於INH及HZ所做的檢量線性範圍分別是2.5-25 μg/mL及2.5-21.2 μg/mL，儀器之最低偵測的範圍可以達到62.5 pg（訊號/雜訊, S/N）的靈敏度。本檢驗方法可以用於檢驗藥品製劑中之INH與HZ，也可以應用肺結核病患之血液中INH之檢驗。在接受以INH為主的化學治療之結核病患者血清中所INH的檢測濃度範圍為0.82-4.8 μg/mL，試驗之相對標準差（RSD）為2.0-5.8%。INH在血液樣本中之回收率為98%，試驗之相對標準差（RSD）為2.5%。"

Antituberculosis drug isoniazid (INH) and hydrazine (HZ) have been determined by capillary column gas chromatography after precolumn derivatization with trifluoroacetylacetone (FAA). Phenylhydrazine (PHZ) when present together with INH and HZ also separated completely from the column HP-5 (30 mm × 0.32 mm I.D) connected with flame ionization detection (FID), and thus was used as an internal standard. The linear calibration ranges for INH and HZ were determined to be 2.5-25 μg/mL and 2.5- 21.2 μg/mL respectively, with detection limit (S/N = 3) corresponding 62.5 pg reaching to the detector. The method was applied for the determination of INH and HZ from pharmaceutical preparations. The method was also used for determination of INH from blood of tuberculosis patient. The amount of INH found in the blood serum of tuberculosis patients on chemotherapy with INH based drugs was within 0.82-4.8 μg/mL with relative standard deviation (RSD) of 2-5.8%. The recovery percentage of INH from blood samples was found 98% with RSD 2.5%.