胶束电动毛细管色谱法测定冬虫夏草中核苷及核苷碱基的含量

目的:测定冬虫夏草、虫体和子座部分核苷及核苷碱基的含量,为质量评定提供检测方法。方法:用胶束电动毛细管色谱法(MECC)测定,以黄嘌呤核苷为内标,电泳缓冲液为V(20mmol·L~(-1)硼砂,25mmol·L~(-1)十二烷基硫酸钠即SDS):V(乙腈)=95:5,电压25KV,柱温30℃,检测波长260nm,进样量5mmHg·S。结果:可同时测定出腺嘌呤(Ⅰ)、腺苷(Ⅱ)、次黄嘌呤(Ⅲ)、鸟苷(Ⅳ)、尿苷(Ⅴ)和次黄嘌呤核苷(Ⅵ)的含量,回收率分别为102.5％,102.7％,98.83％,101.1％,100.8％和101.4％,RSD小于2％。结论:正品虫草中都含有1～Ⅵ6个化合物,子座中Ⅰ～Ⅴ5个化合物的含量均明显高于虫体,虫草中Ⅱ、Ⅳ、Ⅴ、Ⅵ4种核苷的含量较高且相对稳定。

STUDIES ON DETERMINATION OF NUCLEOSIDES AND SOME THEIR BASES IN CORDYCEPS SINENSIS BY MICELLAR ELECTROKINETIC CAPILLARY CHRO-MATOGRAPHY

AIM To determine the nucleosides and their bases existing in the Cordyceps, caterpillar body and stroma of Cordyceps sinensis, and provide the inspection method for eval- uation quality. METHODS: Micellar electrokinetic capillary chromatography (MECC) was used with xanthosine as an internal standard. Separations were performed in an uncoated sili- ca capillary (72cm×50μm. id., 52 cm to window) and electrophoretic buffer V (20mmol L~(-1)borate, 25mmol · L~(-1)sodium dodecyl sulphate) V (acetonitrile) =95:5. Optimum condi- tions were 30 C, 25KV and 5mmHg Sload and detection at 260nm. RESULT: The contents of adenine, adenosine, cypoxanthine, guanosine, uridine and hypoxanthosine have been simul- taneously determined. The recoveries were 102.5%, 102.7%, 98.83%, 101.1%, 100.8% and 101.4% and RSD was less than 2%. CONCLUSION: Ⅰ~Ⅴ5 compounds all exists in the caterpillar body and stroma of true Cordyceps sinensis. The contents of Ⅰ~Ⅴ5 com- pounds in stroma were obviously higher than in caterpillar body. The contents of Ⅱ, Ⅳ,Ⅴ, Ⅵ 4 nudeosides in Cordyceps sinensis were much higher and relatively invariable.