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该文建立一种同时测定4种虫草类药材(冬虫夏草、蛹虫草、虫草菌丝体和蝉花)中虫草素(3’-脱氧腺苷)和2’-脱氧腺苷含量的在线固相萃取-高效液相色谱分析方法。供试品经ZORBAX SB-AQ(4.6 mm×12.5 mm,5μm)色谱柱富集,水-甲醇(91∶9)洗脱;ZORBAX SB-AQ(4.6 mm×150 mm,5μm)色谱柱分离,流动相为0.1%甲酸水溶液-甲醇(91∶9),检测波长260nm,柱温40℃,流速1.0 m L·min~(-1),分别对4种虫草类药材中虫草素和2’-脱氧腺苷含量进行检测。结果表明冬虫夏草、虫草菌丝体和蝉花样品中仅检测到2’-脱氧腺苷,蛹虫草样品中仅检测到虫草素,早期报道的在冬虫夏草中检测到的虫草素色谱峰可能是其同分异构体2’-脱氧腺苷色谱峰或以2’-脱氧腺苷为主的与虫草素的共洗脱色谱峰。该方法重复性好,准确度高,分析时间短,可用于虫草类药材中虫草素和2’-脱氧腺苷的分析。
This article established an online solid-phase extraction method for the simultaneous determination of cordycepin (3’-deoxyadenosine) and 2’-deoxyadenosine in four Cordyceps species (Cordyceps sinensis, Cordyceps militaris, mycelium of Cordyceps and cicadas) - High performance liquid chromatography method. The samples were separated on a ZORBAX SB-AQ (4.6 mm × 150 mm, 5 μm) column and eluted with water-methanol (91: 9) The mobile phase consisted of 0.1% formic acid in methanol (91:9), the detection wavelength was 260 nm, the column temperature was 40 ℃ and the flow rate was 1.0 mL · min -1. Cordyceps and 2’- Deoxyadenosine content were tested. The results showed that only 2’-deoxyadenosine was detected in Cordyceps sinensis, Cordyceps mycelium and cicada flowers samples, and only cordycepin was detected in Cordyceps militaris samples. Earlier reported cordycepin peaks detected in Cordyceps sinensis may be the same The isomer 2’-deoxyadenosine peak or 2’-deoxyadenosine-based co-eluted peak with cordycepin. The method has good repeatability, high accuracy and short analysis time, and can be used for the analysis of cordycepin and 2’-deoxyadenosine in Cordyceps species.