实时直接分析-串联质谱法快速分析乳香中多种乳香酸

Fast detection of boswellic acids in Olibanum by direct analysis in real timetandem mass spectrometry

目的应用实时直接分析-串联质谱法(DART-MS/MS)在未经前处理和色谱分离的情况下快速鉴别乳香中乳香酸类成分。方法使用全扫描采集乳香的DART-MS特征图谱,并对乳香酸类成分进行二级质谱确证。结果药材和提取液的负模式全扫描质谱图中可见11-羰基-β-乙酰乳香酸(m/z 511)、11-羰基-β-乳香酸(m/z 469)、α及β-乳香酸(m/z 455)、α及β-乙酰乳香酸(m/z 497)等成分的[M-H]离子,正模式质谱图中可见11-羰基-β-乙酰乳香酸(m/z 513)和11-羰基-β-乳香酸(m/z 471)的[M+H]+离子,提取液中的正离子m/z 513和m/z 471的CID二级图谱分别与11-羰基-β-乙酰乳香酸和11-羰基-β-乳香酸对照品的一致。结论本法简便、专属性强,为药材、饮片的快速鉴别提供了新思路,具有实用价值。

Objective To establish a method for rapid detection ofboswellic acids in Olibanum without sample pretreatment and liquid chromatography separation by direct analysis in real time-tandem mass spectrometry （DART-MS/MS）. Methods The samples were analyzed using DART-MS with full scan. Results The full scan MS of both Olibanum and its extracting solution gave [M-H]^- signals at m/z 511, 469, 455, and 497 under negative ion mode, which were corresponding to acetyl-11-keto-β-boswellic acid, 11-keto-β-boswellic acid, β-boswellic acid （α-boswellic acid）, and acetyl-β-boswellic acid （acetyl-α-boswellic acid）. Under positive ion mode, the boswellic acids showed [M＋H]^＋ signals at m/z 513 and 471 which were corresponding to acetyl-11-keto-β-boswellic acid and 11-keto-β-boswellic acid. The CID secondary spectrum of acetyl-11-keto-β-boswellic acid and 11-keto-β-boswellic acid in positive ion mode of extract and references substances were the same. Conclusion The method is simple, specific, and can be used for rapid identification of Chinese materia medica and prepared slices of Olibanum.