College of Food Science, Sichuan Agricultural University, Ya'an 625014, China.
Deyang Food & Drug Safety Inspection and Testing Center, Deyang 618029, China.
Int J Mol Sci. 2023 Feb 5;24(4):3156. doi: 10.3390/ijms24043156.
Hydroxyl-α-sanshool is the main alkylamide produced by DC., and it is responsible for numbness after consuming -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 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.
羟基-α-山椒素是山葵产生的主要烷基酰胺，它是食用辛辣菜肴或食品后产生麻木感的原因。本研究涉及羟基-α-山椒素的分离、富集和纯化。结果表明，粉末用 70%乙醇提取，然后过滤；上清液浓缩得到糊状残渣。选择石油醚（60-90°C）和乙酸乙酯的比例为 3:2，Rf 值为 0.23，作为洗脱剂。石油醚提取物（PEE）和乙酸乙酯-石油醚提取物（E-PEE）被用作合适的富集方法。然后，将 PEE 和 E-PEE 加载到硅胶上进行硅胶柱层析。通过 TLC 和 UV 进行初步鉴定。含有主要羟基-α-山椒素的馏分合并并用旋转蒸发仪干燥。最后，所有样品均通过 HPLC 确定。p-E-PEE 中羟基-α-山椒素的产率和回收率分别为 12.42%和 121.65%，纯度为 98.34%。此外，与 E-PEE 相比，E-PEE 纯化（p-E-PEE）中羟基-α-山椒素的纯度提高了 88.30%。总之，本研究提供了一种简单、快速、经济、有效的方法来分离高纯度的羟基-α-山椒素。
