储俊民, 俞永祥. Pellagri氏反应的改进及其在吗啡类化合物比色定量上的应用J. 药学学报, 1958, 6(4): 179-183.
引用本文: 储俊民, 俞永祥. Pellagri氏反应的改进及其在吗啡类化合物比色定量上的应用J. 药学学报, 1958, 6(4): 179-183.
CHU JAIN-MING YU YUN-HSIAN, . THE MODIFICATION OF PELLAGRI'S REACTION AND ITS APPLICATION TO THE COLORIMETRIC DETERMINATION OF MORPHINEJ. Acta Pharmaceutica Sinica, 1958, 6(4): 179-183.
Citation: CHU JAIN-MING YU YUN-HSIAN, . THE MODIFICATION OF PELLAGRI'S REACTION AND ITS APPLICATION TO THE COLORIMETRIC DETERMINATION OF MORPHINEJ. Acta Pharmaceutica Sinica, 1958, 6(4): 179-183.

Pellagri氏反应的改进及其在吗啡类化合物比色定量上的应用

THE MODIFICATION OF PELLAGRI'S REACTION AND ITS APPLICATION TO THE COLORIMETRIC DETERMINATION OF MORPHINE

  • 摘要: 本文对Pellagri氏反应作了較全面的探討与改进,得出: 1.最合适的脱水剂是HCl-H2SO4(1ml:2滴),加酸后在水浴上蒸發半小时脫水,然后用KH2PO4-NaOH緩冲溶液及NaHCO3溶液中和到PH7左右时所得結果最好,氧化剂以碘酸溶液为最佳。2.反应产物可用有机溶剂抽出,其中正丁醇的抽出力最强,使反应的鑑识限度提高为1γ嗎啡鹽基. 3.依照本文条件試驗,反应产物的水溶液,正丁醇抽出液及苯抽出液都符合Beor氏定律(圖2),可用作嗎啡类化合物的比色定量(表1)。

     

    Abstract: The Pellagri's reaction has been known to be a specific and sensitive color reaction for morphine and its derivatives. However, because of the lack of mastering the proper experimental conditions, this reaction always fails to give consistent results and consequently can only be applied as a qualitative but not a quantitative method. According to the following experimental condition, we have succeeded to determine morphine colorimetrically with good reproducibility and to raise up the identification limit to 1 γ morphine base. After evaporating the aqueous solution of morphine hydrochloride or chloroform extract to dryness on a water bath, add 3 drops of HCI-H2SO4 (10:1) and heat for 30 minutes. Remove it from the water bath and add 6 drops of pH 7 buffer solution (KH2PO4-NaOH), 8 drops of 10% NaHCO3 solution and 3 drops of 2% HIO3 solution. Heat for 1/2 minute over water bath, then add 5 ml of water and heat for another 1/2 minute. Extract with 5 ml of n-butyl alcohol, and use the organic layer for the quantitative determination by measuring its extinction at 595 mμ or using a red brown filter instead. For the qualitative purpose, the solution to which HIO3 has been added, is heated for 1 minute on the water bath, transferred to a test tube (5×70 mm), and is shaken with 1-2 drops of n-butyl alcohol. In the presence of morphine and its derivatives the alcoholic layer should be bluish green.

     

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