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1 Acta Chromatographica

1 2016

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Comprehensive characterization and quantification of phillyrin in the fruits of Forsythia suspensa and its medicinal preparations by liquid chromatography-ion trap mass spectrometry

Chen J., Chen Q., Yu F., Huang H., Li P., Zhu J., He X.

Acta Chromatographica

2016

Vol. 28, no. 1

145--157

A rapid and sensitive method for the identification and quantification of phillyrin (POG) in Forsythia suspense is described. The phillyrin standard solution was directly infused into the ion trap mass spectrometers (IT-MS) for collecting the MSn spectra. The electrospray ionization (ESI) mass spectral fragmentation pathway of phillyrin was proposed, and the ESI-MSn fragmentation behavior of phillyrin was deduced in detail. The major product ion at m/z 355 belongs to furofuran, which was formed by loss the glucopyranoside (180 Da), and the characteristic fragment ions m/z 473, 395, 337, 309, and 249 were observed. The loss of 18 Da could arise from two different fragmentation pathways, and the observed ion was composed of a mixture of two different structural ions. Quantification of phillyrin was assigned in positive-ion mode at a product ion at m/z 557 → 355 by liquid chromatography-mass spectrometry (LC-MS). The LC-MS method was validated for linearity, sensitivity, accuracy, and precision and then used to determine the content of the phillyrin. Lastly, the LC-MS method was successfully applied to determine phillyrin in real sample F. suspense and three of its medicinal preparations in the positive mode at the first time.