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采用制备色谱对芒果苷原料药中的一种主要杂质进行分离纯化,利用HR-ESI(-)-MS/MS分析其结构。在芒果苷及其杂质的一级质谱中,其[M-H]-峰分别为m/z421.0775和435.0973;在HR-ESI(-)-MS/MS串联质谱分析中,芒果苷的主要碎片峰有m/z331.0436、301.0335、271.0237;而杂质的主要碎片峰有m/z345.0657、315.0486、287.0189、272.0308。经有机质谱分析,并经UV、1HNMR、13CNMR进一步确认,芒果苷原料药中微量杂质的结构为2-C-β-D-glucopyranosyl-1,6,7-trihydroxy-3-methoxy-xanthen-9-one。根据HR-ESI(-)-MS/MS分析,给出了芒果苷及其杂质主要碎片的ESI-MS质谱裂解途径。
A major impurity in mangiferin API was isolated and purified by preparative chromatography. The structure was analyzed by HR-ESI (-) - MS / MS. The [MH] - peaks in the first order MS of mangiferin and its impurities were m / z 421.0775 and 435.0973, respectively. The major fragment peaks of mangiferin in HR-ESI (-) MS / MS tandem mass spectrometry There are m / z 331.0436, 301.0335, 271.0237; while the major impurity peaks have m / z 345.0657, 315.0486, 287.0189, 272.0308. The structure of trace impurities in mangiferin APIs was confirmed by MS and UV, 1HNMR, 13CNMR. The structure of 2-C-β-D-glucopyranosyl-1,6,7-trihydroxy-3-methoxy-xanthen- -one. According to HR-ESI (-) - MS / MS analysis, the ESI-MS mass spectrometry cleavage pathway of mangiferin and its major impurities was given.