Abstract

A validated analytical method is reported for the analysis of chlorogenic and caffeic acids in Xu Duan (Dipsacus asperoides) in the dried raw herb. The ground samples were extracted by ultrasonication in water and the extract was analysed by LC-PDA with identity confirmation by (+)ESI-MS/MS. A C18 column was used with a 0.1% aqueous formic acid : methanol gradient mobile phase. The analytes were quantified 325 nm. With the MS detector, using the chlorogenic acid precursor ion with m/z 354, ions with m/z 191, and 85 were produced. For caffeic acid the precursor ion with m/z 181, ions with m/z 163, 135, and 89 were produced. The amount of chlorogenic and caffeic acids in the raw herb was found to be 4.46 and 0.63 mg/g, respectively, and the method LOD was 0.13 and 0.02 mg/g, respectively.

Highlights

  • Dipsacus asperoides or commonly known as Xu Duan is a perennial plant distributed in mountainous regions of southwestern China and has been used in Chinese traditional folk medicine for its antibacterial and anti-inflammatory properties [1]

  • Chromatograms obtained at 325 nm for chlorogenic acid and caffeic acid gave the best compromise between sensitivity and baseline noise

  • The limits of detection (LOD) for chlorogenic and caffeic acids are determined as three times the SD obtained from seven replicate extractions and analyses of the raw herb were 0.13 and 0.02 mg/g, respectively

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Summary

Introduction

Dipsacus asperoides or commonly known as Xu Duan is a perennial plant distributed in mountainous regions of southwestern China and has been used in Chinese traditional folk medicine for its antibacterial and anti-inflammatory properties [1]. The analysis of chlorogenic and caffeic acids in Xu Duan has only been reported in one paper [3]. Caffeic acid has antiprostaglandin properties which are a property of conventional drugs used to treat dysmenorrhoea [10] This ability could explain its frequent inclusion in herbal formulations for the treatment of the gynaecological ailment dysmenorrhoea. A mixed standard containing 8.7, 26.2, 43.6, 87.3, 130.9, and 174.5 μg/mL of chlorogenic acid and 3.3, 9.9, 16.5, 33, 49.4, and 65.9 μg/mL of caffeic acid by diluting 50, 150, 250, 500, 750, and 1000 μL of the mixed calibration stock standard solution to 1000 μL with methanol was prepared. This work reports a LC-PDA (liquid chromatographyphotodiode array detection) method for the determination of chlorogenic and caffeic acids in the Xu Duan raw herb, with MS identity confirmation of the analyte

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