[在线固相萃取-高效液相色谱法同时测定虫草属中虫草素和2'-脱氧腺苷的含量]

[Simultaneous determination of cordycepin and 2'-deoxyadenosine in Cordyceps genus by online SPE-HPLC].

作者信息

Tian Ye, Wang Chuan-Xi, Qian Zheng-Ming, Li Zhou, Zhou Miao-Xia, Sun Wan-Yang, Yao Xin-Sheng, Li Wen-Jia, Gao Hao

机构信息

Key Laboratory of State Administration of Traditional Chinese Medicine, Sunshine Lake Pharma Co., Ltd., Dongguan 523850, China.

Institute of Traditional Chinese Medicine and Natural Products, College of Pharmacy, Jinan University, Guangzhou 510632, China.

出版信息

Zhongguo Zhong Yao Za Zhi. 2017 May;42(10):1932-1938. doi: 10.19540/j.cnki.cjcmm.20170223.025.

DOI:10.19540/j.cnki.cjcmm.20170223.025

PMID:29090553

Abstract

An online SPE-HPLC method for simultaneous determination of cordycepin (3'-deoxyadenosine) and 2'-deoxyadenosine in Cordyceps genus (C. sinensis,C. militaris,Hirsutella sinensis and C. sobolifera) was developed. The samples were enriched on a ZORBAX SB-AQ (4.6 mm×12.5 mm,5 μm) column with isocratic elution by 9% methanol solution. The separation of analytes was performed on a ZORBAX SB-AQ (4.6 mm×150 mm,5 μm) column with gradient elution by 0.1% formic acid solution and methanol (91∶9). The flow rate was 1.0 mL•min⁻¹. Column temperature was 40 ℃ and detection wavelength was 260 nm. This method has been applied for analysis of different Cordyceps genus. The 2'-deoxyadenosine was detected in C. sinensis,Hirsutella sinensis and C. sobolifera. The cordycepin was detected in C. militaris. In summary,the cordycepin chromatographic peak from C. sinensis in some past reports may be the 2'-deoxyadenosine chromatographic peak or the mixture peak of 2'-deoxyadenosine and cordycepin in which 2'-deoxyadenosine content was higher than cordycepin. The developed method is suitable for analysis of cordycepin and 2'-deoxyadenosine in Cordyceps genus.

摘要

建立了一种在线固相萃取-高效液相色谱法同时测定虫草属（中华虫草、蛹虫草、中华被毛孢和古尼虫草）中的虫草素（3'-脱氧腺苷）和2'-脱氧腺苷。样品在ZORBAX SB-AQ（4.6 mm×12.5 mm，5μm）柱上用9%甲醇溶液等度洗脱进行富集。分析物在ZORBAX SB-AQ（4.6 mm×150 mm，5μm）柱上用0.1%甲酸溶液和甲醇（91∶9）梯度洗脱进行分离。流速为1.0 mL•min⁻¹。柱温为40℃，检测波长为260 nm。该方法已应用于不同虫草属的分析。在中华虫草、中华被毛孢和古尼虫草中检测到了2'-脱氧腺苷。在蛹虫草中检测到了虫草素。综上所述，以往一些报道中中华虫草的虫草素色谱峰可能是2'-脱氧腺苷色谱峰或2'-脱氧腺苷含量高于虫草素的2'-脱氧腺苷与虫草素的混合峰。所建立的方法适用于虫草属中虫草素和2'-脱氧腺苷的分析。