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Analysis of Reaction between α-Lipoic Acid and 2-Chloro-1-methylquinolinium Tetrafluoroborate Used as a Precolumn Derivatization Technique in Chromatographic Determination of α-Lipoic Acid

机译:α-硫辛酸与2-氟-1-甲基喹啉四氟硼酸盐的色谱柱测定中柱前衍生技术的反应分析

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摘要

The present study offers results of analysis concerning the course of reaction between reduced α-lipoic acid (LA) and 2-chloro-1-methylquinolinium tetrafluoroborate (CMQT). In water environments, the reaction between CMQT and hydrophilic thiols proceeds very rapidly and the resultant products are stable. For the described analysis, optimum reaction conditions, such as concentration of the reducing agent, environment pH, and concentration of the reagent were carefully selected. The spectrophotometric assay was carried out measuring absorbance at λ = 348 nm (i.e., the spectral band of the obtained reaction product). Furthermore, the calibration curve of lipoic acid was registered. It was concluded that the Lambert-Beer law was observed within the range 1–10 μmol L−1. Later, the reaction between LA and CMQT was used as precolumn derivatization in a chromatographic determination of the lipoic acid in the range 2.5–50 μmol L−1. Practical applicability of the designed methods was evaluated by determining lipoic acid in Revitanerv pharmaceutical preparation which contains 300 mg LA in a single capsule. The error of the determination did not exceed 0.5% in relation to the declared value.
机译:本研究提供了有关还原α-硫辛酸(LA)与2-氯-1-甲基喹啉四氟硼酸酯(CMQT)之间反应过程的分析结果。在水环境中,CMQT与亲水性硫醇之间的反应进行得非常迅速,并且生成的产物稳定。对于所述分析,仔细选择最佳反应条件,例如还原剂的浓度,环境pH和试剂的浓度。用分光光度法测定λ= 348nm的吸光度(即所得反应产物的光谱带)。此外,记录了硫辛酸的校准曲线。结论是,在1-10μmolL -1 范围内观察到了朗伯-比尔定律。后来,LA和CMQT之间的反应被用作色谱柱测定中的硫辛酸,色谱范围为2.5–50μmol·L -1 。通过测定Revitanerv药物制剂中的硫辛酸来评估设计方法的实际适用性,该制剂中的单个胶囊中含有300μmgLA。相对于声明值,测定误差不超过0.5%。

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