5-硝基间苯二甲酸甲酯工业品的高效液相色谱指纹图谱的建立

Establishment of the chromatographic fingerprints of industrial product methyl 5-nitro-iso-phthalates

建立了5-硝基间苯二甲酸单甲酯和5-硝基间苯二甲酸二甲酯共享的高效液相色谱-紫外光谱的指纹图谱。在反相C18色谱柱上,以甲醇-水-0.1%高氯酸水溶液为流动相,对5-硝基间苯二甲酸单甲酯和5-硝基间苯二甲酸二甲酯及其相关杂质进行分离测定。通过运行大量样品,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、紫外光谱及其峰面积,与色谱指纹图谱进行分析对比,建立了工业品5-硝基间苯二甲酸单甲酯和5-硝基间苯二甲酸二甲酯质量控制的新方法。

A reliable reversed-phase high performance liquid chromatographic method has been developed for drawing shared chromatographic fingerprints of mono-methyl 5-nitro-iso-phthalate （MM-NIP） and di-methyl 5-nitro-isophthalate （DM-NIP） for industrial use. Separation and determination of MM-NIP and DM-NIP as well as their relative substances were achieved on a Kromasil C18 column by using methanol-water-perchloric acid （1%o） （V/V/V = 60/20/ 20） at a flow rate of 1.0 mL/min as the mobile phase. The temperature of the column was 30 ℃ and the detection was operated by UV absorption at a wavelength of 254 nm. Accordingly, the chromatographic fingerprints could be established by analyzing a lot of samples and extracting their common peaks in chromatograms, which are of representative feature for all samples involved. If given a sample, we can compare retention time, UV spectrum and area of all peaks with the proposed chromatographic fingerprint, and then develop a new protocol by which the quality of MM-NIP and DM-NIP can be controlled.