2,4-二硝基苯肼与某些醛在阳离子表面活性剂胶束中的分析反应

Tatiana A. Sokolova, Anna A. Burmistrova, Sergey Yu. Doronin
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摘要

建立了一些芳香醛(AA)与2,4-二硝基苯肼(DNPH)反应中阳离子表面活性剂胶束的分析效应,并形成相应的酸型腙。已经确定,非离子和阴离子表面活性剂的胶束在所研究的体系中不会产生显著的分析影响。以苯甲醛及其硝基、亚基、氯基、二甲胺、甲氧基衍生物和对甲基甲胺醛(DMAC)为例,测定了DNPH-AA -阳离子表面活性剂体系的摩尔吸收系数(ε)、测定含量范围和检出限。多数醛类化合物的测定范围为0.2 ~ 2.1 μg/ml, ε值为2.10-4 ~ 1.10-5 l mol-1 cm-1。合成了由DNPH和DMAC合成的腙,并通过元素分析和红外光谱对其进行了鉴定。研究了合成的腙在水溶液(pH 13)和胶束(十六烷基氯吡啶,CPC)介质中的溶解度。结果表明,其在CPC胶束中的溶解度提高了约60倍,这使得所研究的体系DNPH - AA -阳离子表面活性剂在时间上(其各向同性)稳定,并且在没有挥发性和有毒有机溶剂的情况下,提高了相应醛的测定灵敏度,同时实现了“绿色化学”的原则。利用阳离子表面活性剂的作用,建立了一种非提取光度法测定药物制剂中链霉素(一种对结核病有效的广谱氨基糖苷类抗生素)含量的方法,测定范围为2.1 ~ 87.4 μg/ml。直接光度法测定链霉素的误差不超过5-9%。
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Analytical reactions of 2,4-dinitrophenylhydrazine with some aldehydes in micelles of cationic surfactants
The analytical effect of micelles of cationic surfactants in the reactions of some aromatic aldehydes (AA) with 2,4-dinitrophenylhydrazine (DNPH) with the formation of the corresponding aci-forms of hydrazones has been established. It has been established that micelles of nonionic and anionic surfactants do not cause analytically significant effects in the system under study. Analytical characteristics of systems DNPH–AA– cationic surfactant (molar absorption coefficients (ε), ranges of determined contents, limits of detection) were determined, using the example of benzaldehyde and its nitro-, sulfo-, chlorine-, dimethylamino- and methoxy derivatives, as well as p-dime thylaminocinnamic aldehyde (DMAC). For the majority of aldehydes ranges of determined contents are in the range from 0,2 to 2,1 μg/ml, ε from 2.10-4 to 1.10-5 L.mol-1.cm-1. The hydrazone formed by DNPH and DMAC was synthesized and identified by elemental analysis and IR spectroscopically. The solubility of the resulting hydrazone in aqueous (pH 13) and micellar (cetylpyridinium chloride, CPC) media was studied. It has been shown that its solubility in CPC micelles increases approximately 60 times, which leads to the stabilization of the studied system DNPH – AA – cationic surfactant in time (its isotropy) and an increase in the sensitivity of the determination of the corresponding aldehyde in the absence of volatile and toxic organic solvents, while the principle “green chemistry” has been implemented. The established effect of cationic surfactants was implemented to develop a method for the non-extraction photometric determination of streptomycin (a broad-spectrum aminoglycoside antibiotic effective against tuberculosis) in pharmaceutical preparations with ranges of determined contents from 2,1 to 87,4 μg/ml. The error of direct photometric determination of streptomycin did not exceed 5–9%.
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