高效液相色谱-紫外光谱法建立3,5-二硝基苯甲酸工业品的色谱指纹图谱

Establishment of the Chromatographic Fingerprint of Industrial 3,5-Dinitrobenzoic Acid by High Performance Liquid Chromatography-Ultraviolet Spectrometry

建立了3,5-二硝基苯甲酸工业品的高效液相色谱-紫外光谱的指纹图谱。首先,在Kromasil C_(18)色谱柱上,以水-甲醇-0．10%高氯酸水溶液(体积比为25:45:30)为流动相,流动相流速1．0 mL/min,检测波长254 nm,对3,5-二硝基苯甲酸及其相关杂质进行了分离分析。在此基础上,通过运行大量样品,筛选共有组分,绘制具有共同特性的指纹图谱。根据待测样品色谱峰的保留时间、紫外光谱及其色谱峰面积,与色谱指纹图谱进行分析对比,建立了控制3,5-二硝基苯甲酸产品质量的新方法。该方法在产品含量测定方面结果准确、可靠,在产品质量控制方面直观、方便。阐述了“整体性”和“明确性”是精细化工中间体指纹图谱的基本属性和发展方向。

A reliable reversed-phase high performance liquid chromatography-ultraviolet spectrometric method has been developed for drawing chromatographic fingerprint of 3,5-dinitrobenzoic acid for industrial use. Separation of 3,5-dinitrobenzoic acid and its relative impurities were achieved on a Kromasil C18 column by using methanol-water-0. 10% perchloric acid （ V/V/V= 25/45/30） as a mobile phase at a flow rate of 1.0 mL/min. And the determination was carried out by UV spectrometry at wavelength of 254 nm. Accordingly, the chromatographic fingerprint of 3,5-dinitrobenzoic acid could be established by analyzing a lot of samples and extracting their common peaks which are of representative features for all samples involved. For a given sample, the retention time, UV spectrum and area of all peaks were compared with the proposed chromatographic fingerprint, and a new protocol was then developed, by which the quality of 3,5-dinitrobenzoic acid can be controlled. This method is accurate and credible in determination of every component in an industrial product. It is also visualized and convenient in quality control. In addition, it was expounded that ＂ integrity＂ and ＂ definitude＂ should be elementary attributes and developing direction of the chromatographic fingerprint of fine chemical intermediate.