発けい光性色素を用いる塩基性医薬品のけい光定量

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  • A fluorophotometric determination of basic drugs by using a fluorescent dye salt procedure
  • アバケ イヒカリセイ シキソ オ モチイル エンキセイ イヤクヒン ノ ケイコウ テイリョウ

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Several dye methods which are based on the formation of colored compounds with acid dyes, have been proposed for the determination of amines or quarternary ammonium salts. Although the sensitivity of the dye methods is quite sufficient for many purposes, situations often occur in biochemical field where a more sensitive method is necessary. Since fluorometry is known to be 10 to 100 times more sensitive than colorimetry, a fluorescent tetrabromosulfonfluorescein (TBSF) was used as the acid dye for the determination of long-chain secondary or tertiary amines, such as amitriptyline, nortriptyline, chlorpromazine, carbetapentane and tripelenamine.<BR>Fluorescent TBSF was synthesized by bromination of sulfonfluorescein. A TBSF standard solution (2 μg/ ml) and a TBSF solution (200 μg/ml) were prepared by dissolving the reagent in methanol and in water, respectively. An alkaline methanol was prepared by diluting 1 ml of 0.5 N NaOH to 100 ml with methanol. Chloroform was used as the extracting solvent.<BR>Determination of amitriptyline: To a 2 ml portion of amitriptyline hydrochloride (0.55.0 μg/ml in 0.1 N HCl), 1 ml of the TBSF solution and 3 ml of chloroform are added. The mixture is thoroughly stirred for 1 min by a mixer. After standing for a few minutes in order to separate the two phases, the upper aqueous phase is removed, and exactly 2 ml of the chloroform phase is transferred to another test tube containing 2 ml of the alkaline methanol. After mixing the two phases, the fluorescence intensity is measured with excitation maximum at 535 nm and with emission maximum at 550 nm. The fluorophotometer is calibrated by the TBSF standard solution. A linear relationship between the fluorescence intensity and the concentration of amitriptyline was obtained (1.6 16.0×10-9moles/ml).<BR>Fig. 1 shows that the optimum pH for the solvent extraction is 2.5, and Fig. 2 shows that the maximum relative fluorescence intensity is obtained by use of 0.02% TBSF solution. As shown in Fig. 3, the fluorescence intensity is very stable.<BR>The interference with various compounds in blood and urine was examined. Most of them caused no effect on the results. As expected, the proposed method is about 100 times more sensitive than the usual colorimetric method using acid dyes. This method could be applied to the determination of basic drugs in blood, urine or pharmaceutical preparations. For example, amitriptyline could be extracted from alkaline urine with n-hexane, back-extracted into 0.1 N HCl and then an appropriate portion of it was measured by the above determination procedure.

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  • 分析化学

    分析化学 22 (2), 163-167, 1973

    公益社団法人 日本分析化学会

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