Abstract

Detection of sulfur-fumigated Paeoniae Alba Radix (PAR) in different complex preparations is challenging due to the relatively lower content of PAR and interference from more complicated components in complex preparations with different multiple constituent herbs. In this study, a high performance liquid chromatography- triple-quadrupole tandem mass spectrometry method was developed for detecting sulfur-fumigated PAR in different complex preparations. Paeoniflorin, the major component of PAR, and paeoniflorin sulfonate, the characteristic artifact transformed from paeoniflorin during sulfur-fumigation of PAR, were used as chemical markers. Multiple reaction monitoring (MRM) scan was employed to maximize sensitivity and selectivity. Through optimizing full mass scan and daughter ion scan conditions, two mass transitions were selected and employed respectively for unequivocal identification of paeoniflorin and paeoniflorin sulfonate. The detection limits for paeoniflorin and paeoniflorin sulfonate using MRM were much lower than those detected with UV 270 nm. Paeoniflorin and paeoniflorin sulfonate could be simultaneously detected in different commercial PAR-containing complex preparations without interference of other components using the established method, indicating that the newly established method was selective and sensitive enough for screening sulfur-fumigated PAR in commercial complex preparations.

Highlights

  • Paeoniae Alba Radix (PAR), derived from the root of Paeonia lactiflora, is a commonly used medicinal herb with claims of antispasmodic, tonic, astringent and analgesic properties [1]

  • Non-fumigated and sulfur-fumigated PAR samples were comparatively analyzed by HPLC-photo-diode array (PDA)-TQ-MS/MS

  • To extensively optimize the conditions for fragmentation of paeoniflorin and paeoniflorin sulfonate, the samples were further analyzed with daughter ion scan, with ion m/z 449 and m/z 543 selected as parent ions of paeoniflorin and paeoniflorin sulfonate respectively

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Summary

Introduction

Paeoniae Alba Radix (PAR), derived from the root of Paeonia lactiflora, is a commonly used medicinal herb with claims of antispasmodic, tonic, astringent and analgesic properties [1]. In. Traditional Chinese Medicine, this herb is prescribed as the major constituent material of many complex preparations [2,3,4,5]. To the best of our knowledge, no study on screening for sulfur-fumigated PAR in complex preparations was reported. When LC-UV was used to identify sulfur-fumigated PAR in complex preparations, the more complicated constituents of different complex preparations may interfere with the separation of target analytes due to the poor selectivity of the UV detector, and it is difficult to develop a universal LC-UV method for the identification of sulfur-fumigated PAR in different complex preparations. In this study, using HPLC-TQ-MS/MS with two mass transitions MRM scan, a sensitive and selective method to screen sulfur-fumigated PAR in complex preparations was developed, and was successfully applied for analysis of commercial PAR-containing complex preparations with different constituent herbs

Results and Discussion
1: Scan ESTIC
Fragmentation of Paeoniflorin and Paeoniflorin Sulfonate by Daughter Ion Scan
Selectivity and Sensitivity by MRM Scan
Analysis of Commercial PAR Samples and PAR-containing Complex Preparations
Result
Chemicals and Reagents
Plant Materials
Sulfur-Fumigation of PAR
Water decoction of PAR
Liquid Chromatography
Mass Spectrometry
Sensitivity Test
Conclusions

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