Separation and Purification of Hydroxyl-α-Sanshool from Zanthoxylum armatum DC. by Silica Gel Column Chromatography

Abstract

Hydroxyl-α-sanshool is the main alkylamide produced by Zanthoxylum armatum DC., and it is responsible for numbness after consuming Z. armatum-flavored dishes or food products. The present study deals with the isolation, enrichment, and purification of hydroxyl-α-sanshool. The results indicated that the powder of Z. armatum was extracted with 70% ethanol and then filtrated; the supernatant was concentrated to get pasty residue. Petroleum ether (60–90 °C) and ethyl acetate at a 3:2 ratio, with an Rf value of 0.23, were chosen as the eluent. Petroleum ether extract (PEE) and ethyl acetate–petroleum ether extract (E-PEE) were used as the suitable enriched method. Afterward, the PEE and E-PEE were loaded onto silica gel for silica gel column chromatography. Preliminary identification was carried out by TLC and UV. The fractions containing mainly hydroxyl-α-sanshool were pooled and dried by rotary evaporation. Lastly, all of the samples were determined by HPLC. The yield and recovery rates of hydroxyl-α-sanshool in the p-E-PEE were 12.42% and 121.65%, respectively, and the purity was 98.34%. Additionally, compared with E-PEE, the purity of hydroxyl-α-sanshool in the purification of E-PEE (p-E-PEE) increased by 88.30%. In summary, this study provides a simple, rapid, economical, and effective approach to the separation of high-purity hydroxyl-α-sanshool.

Rapid purification of alkylamides from Zanthoxylum bungeanum by medium-pressure liquid chromatography and the establishment of a numbness prediction model using an electronic tongue

“…Cheng et al 22 used silica gel column chromatography to separate prickly ash amides extract and obtained high-purity hydroxyl-α-sanshool, but with a low loading capacity and yield. Wang et al 23 used high-speed counter-current chromatography to fractionate typical prickly ash amides, but obtained only a mixture of alkylamides.…”

The Identification and Role of the Key Mycotoxin of Pestalotiopsis kenyana Causing Leaf Spot Disease of Zanthoxylum schinifolium

“…Elution was carried out using a large volume of eluent, and the eluted components were collected and evaporated to dryness. Water was added to prepare a solution with a specific concentration suitable for bioassay [43][44][45][46].…”