固相萃取高效液相色谱内标法测定冬虫夏草中甘露醇的含量

SPE-HPLC study on internal standard method for determination of mannitol in Cordyceps sinensis(Berk.)Sacc.

目的:研究用固相萃取预分离,高效液相色谱内标法测定冬虫夏草中甘露醇的含量。方法:冬虫夏草样品中的甘露醇用水超声振荡浸取,浸取液用 Waters Sep-Pak-C_(18)固相萃取小柱预分离,以海藻糖为内标物,Waters Sugar-Pak-1(6.5 mm×300 mm)钙型阳离子交换柱为固定相,0.05 g·L^(-1)EDTA 钙钠水溶液为流动相,流速0.5 mL·min^(-1),示差折光仪为检测器测定冬虫夏草样品中的甘露醇含量。结果:最低检测限为2.0μg·mL^(-1);回收率在97%～102%之间,RSD 在0.86%～1.2%之间。结论:方法简便、灵敏、准确、适用于冬虫夏草样品的甘露醇测定。

Objective： Study on pre - separation with solid phase extraction, and HPLC method for the determination of mannitol in Cordyceps sinensis （ Berk. ） Sacc. Methods： The mannitol was extracted from Cordyceps sinensis sample with water, and purified by solid phase extraction with Sep - Pak - C18 cartridge. With fucose as internal standard, the mannitol was separated on a Waters Sugar - Pak - 1 （6. 5 mm × 300 mm） cations ion exchange column with 0. 05 g · L^-1 EDTA calcium disodium salt solution as mobile phase, and flow rate was 0. 5 mL · min^-1, and detected with refractive index detector system. Results：The limit of detection of mannitol was 2.0 μg · mL^-1. The mean recovery was between 97% and 102% with RSD between 0. 86% and 1.2%. Conclusion：This method is simple, convenient, sensitive, accurate and suitable for the determining of the different mannitol in Cordyceps sinensis.