吸附-发光法测定药品中山茱萸酸

S. Beltyukova, O. Teslyuk, E. Liventsova
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引用次数: 0

摘要

本研究对已知生物活性物质山茱萸酸(维生素B13)的发光特性进行了评价。研究表明,在香浓酸与铽(III)的配位配合物内,发生了从配体到镧系离子的分子间激发能转移,引起铽(III)离子发光的敏化。在阴离子和阳离子表面活性剂的存在下,由于水分子从配合物的配位球中位移,铽离子发光(ILum)的强度增加。作为这一过程的结果,激发能的非辐射失活减少和更有效的激发能转移从配体到镧系离子发生。研究表明,在所研究的配合物的发光强度(ILum)提高后,所研究的分析物在固相萃取吸附剂的聚合物基体上吸收后,其分子刚度随之增加,激发能转移更有效。山梨酸与山梨酸盐形式的铽(III)配位配合物的发光强度已被估计涉及不同类型的吸附剂(Phosphalugel, SFG-75, Calflo E, Celite 545, silagel Merck)。使用默克硅胶作为固相基质(吸附剂)获得了最合适的结果。在这种情况下,络合物的去除率可达97%。确定了测定山茱萸酸的最有效条件。用5ml溶液和100mg吸附剂进行吸附时,发光强度达到最高值。在吸收过程中,以山梨酸盐形式的配合物的发光强度在阳离子二聚体表面活性剂乙铵的存在下增加。在其他表面活性剂存在下,山梨酸盐形式的配合物的发光强度降低可能是由于配合物在溶液中的增溶,从而降低了其吸附水平。在上述研究工作的基础上,建立了一种固相发光法测定药物中山茱萸酸及山茱萸酸盐的分析方法。本文对药用药物“磁黄酮”(角化酸镁)和“角化酸钾”中的角化酸盐进行了测定。所建立的分析方法具有良好的计量特性和相对简单的性能。相对标准偏差Sr为3,6 ~ 4,3%。
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SORPTION-LUMINESCENT DETERMINATION OF OROTIC ACID IN MEDICINAL DRUGS
Luminescent properties of orotic acid (vitamin B13), known bioactive substance, have been evaluated in this research. It has been shown that inside a coordination complex of orotic acid with terbium (III) an intermollecular excitation energy transfer from a ligand to a lanthanide ion occurs which causes sensitization of terbium (III) ion luminescence. Intensity of the terbium (III) ion luminescence (ILum) increases in the presence of anionic and cationic surfaceactive agents as a result of displacement of water molecules from coordination sphere of the complex. As a consequence of this process, a non-radiative deactivation of excitation energy decreases and more efficient excitation energy transfer from a ligand to a lanthanide ion occurs. It has been established that after absorption of analyte of interest onto a polymer matrix of a solid phase extraction sorbent with subsequent increasing of its molecular rigidity more efficient excitation energy transfer is observed followed by elevation of luminescence (ILum) intensity of the coordination complex being studied. Intensity of luminescence of coordination complex of orotic acid with terbium (III) in the form of a sorbate salt has been estimated involving different types of sorbents (Phosphalugel, SFG-75, Calflo E, Celite 545, Silicagel Merck). Most suitable results have been achieved by the use of Silica gel Merck as a solid-phase matrix (sorbent). The removal rate of the complex from the solution in this case reaches to 97%. The most effective conditions for determination of orotic acid have been specified. The highest values of luminescence intensity is obtained by conducting of sorption using 5 mL of solution and 100 mg of sorbent. Luminescence intensity of the complex in the form of a sorbate salt, during a sorption process, increases in presence of ethonium, cationic dimeric surface-active agent. Decrease in luminescence intensity of the complexes in the form of a sorbate salt in presence of other surface-active agents may be caused by solubilization of the complex in the solution and thereby reduced level of its sorption. On the basis of presented research work a new analytical procedure has been developed for the solid-phase luminescence determination of orotic acid and orotic acid salts in pharmaceutical drugs. Determination of orotic acid salts has been performed in pharmaceutical drugs ‘Magnerot’ (magnesium orotate) and ‘Potassium orotate’. The proposed analytical procedure for determination of orotic acid salts is remarkable by good metrological characteristics and relative simplicity of performance. The relative standard deviation, Sr, is 3,6 - 4,3%.
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