Simultaneous determination of ten constituents in the Chinese medicinal preparation Fufangxingxiangtu’erfeng capsules by ultra performance liquid chromatography with tandem mass spectrometry

doi:10.3724/SP.J.1123.2013.11008

Abstract

Abstract:

Using caffeic acid and icariin as internal standards, a method for the simultaneous determination of protocatechuic acid, protocatechuic aldehyde, chlorogenic acid, scutellarin, isochlorogenic acid C, baicalin, luteolin, apigenin, atractylenolide Ⅲ and atractylenolide I in Fufangxingxiangtu'erfeng capsules were established by ultra performance liquid chromatography with tandem mass spectrometry (UPLC-MS/MS). The separation was performed on a ZORBAX RRHD Eclipse Plus C₁₈ column (50 mm×2.1 mm, 1.8 μm) by using water containing 0.3% formic acid and methanol as mobile phases with the gradient elution at a flow rate of 0.3 mL/min. The analytes were detected by a tandem mass spectrometer in the multiple reaction monitoring (MRM) mode via the switching of positive electrospray ionization (ESI⁺) and negative electrospray ionization (ESI^-). Under optimum conditions, the calibration curves were linear in the range of 0.00300-24.0 mg/L for protocatechuic acid, 0.0170-2.00 mg/L for protocatechuic aldehyde, 0.0150-30.0 mg/L for chlorogenic acid, 0.00400-30.0 mg/L for scutellarin, 0.0105-24.0 mg/L for isochlorogenic acid C, 0.00300-30.0 mg/L for baicalin, 0.00300-5.0 mg/L for luteolin, 0.00600-1.50 mg/L for apigenin, 0.00150-4.00 mg/L for atractylenolide Ⅲ, and 0.000600-0.900 mg/L for atractylenolide I with the detection limits of 1.0, 11, 5.0, 1.5, 3.5, 1.0, 1.0, 2.0, 0.50, 0.20 μg/L, respectively. The average recoveries of the ten effective components were between 92.5% and 106% with all relative standard deviations not more than 3.2%. The developed method was rapid, simple, accurate, reproducible, and suitable for the quality control of the Fufangxingxiangtu'erfeng capsules.

Key words: effective components, Fufangxingxiangtu’erfeng capsules, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

CLC Number:

O658

FAN Xiaosu, PANG Qian, XU Yuanjin. Simultaneous determination of ten constituents in the Chinese medicinal preparation Fufangxingxiangtu’erfeng capsules by ultra performance liquid chromatography with tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2014, 32(3): 216-223.

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