Identification and quantification of atractylenolide I and atractylenolide III in Rhizoma Atractylodes Macrocephala by liquid chromatography–ion trap mass spectrometry
- 23 November 2012
- journal article
- research article
- Published by Wiley in Biomedical Chromatography
- Vol. 27 (6), 699-707
- https://doi.org/10.1002/bmc.2847
Abstract
Rhizoma Atractylodes Macrocephala (RAM) is an important traditional Chinese medicinal herb that is used for treatment of dyspepsia and anorexia. The active ingredients, atractylenolide I (AO-I) and atractylenolide III (AO-III), were identified by direct-injection ion trap-mass spectrometry (IT-MS) for collecting MSn spectra. The major fragment ions of AO-I and AO-III were confirmed by MSn both in negative ion mode and in positive ion mode. The possible main cleavage pathway of fragment ions was studied. The determinations of AO-I and AO-III were accomplished by liquid chromatography (LC) with UV and MS. The analytes provided good signals corresponding to the protonated molecular ions [M + H]+ and product ions. The precursor ions and product ions for quantification of AO-III and AO-I were m/z 249 → 231 and m/z 233 → 215, respectively, using selected ion monitoring by LC-IT-MS. Two methods were evaluated for a number of validation characteristics (repeatability, limit of detection, calibration range, and recovery). MS provides a high selectivity and sensitivity for determination of AO-III and AO-I in positive mode. After optimization of the methods, separation, identification and quantification of the two components in RAM were comprehensively tested by HPLC with UV and MS. Copyright © 2012 John Wiley & Sons, Ltd.Keywords
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