摘要
目的：建立同时测定蛹虫草中腺苷、胞苷、鸟苷、甘露醇、腺嘌呤、虫草素含量的方法。方法：液质联用技术,以甲醇-0.1%甲酸溶液为流动相等度洗脱,采用Agilent ZORBAX SB-C18色谱柱,通过电喷雾离子源,选择正离子模式多反应监测方式检测。结果：腺苷、胞苷、鸟苷、甘露醇、腺嘌呤、虫草素的线性范围分别为37.5~1 200μg·L-1（r=0.998 5）,20~640μg·L-1（r=0.996 4）,40~1 280μg·L-1（r=0.999 1）,77.5~2 480μg·L-1（r=0.993 5）,27.5~880μg·L-1（r=0.992 4）,90~2 880μg·L-1（r=0.9937）,加样回收率在92.1%~102.6%,RSD均〈8.1%。腺苷、胞苷、鸟苷、甘露醇、腺嘌呤、虫草素在蛹虫草中的平均质量分数分别为268.33,11.28,185.66,1 421.44,10.67,812.21μg·g-1。结论：该法专属性强、快速灵敏,可用于蛹虫草中腺苷、胞苷、鸟苷、甘露醇、腺嘌呤、虫草素的含量测定。
Objective： To develop a UPLC-MS /MS method for the determination of adenosine,cytidine,guanosine,mannitol,adenine and cordycepin in Chinese Caterpillar Fungus. Method： Isocratic elution was carried out with methanol-0. 1% formic acid as the mobile phase using liquid chromatography-mass spectrometry technology. The separation was performed on Agilent ZORBAX SB-C18,and the mass spectrometer was operated in the positive ionization electrospray（ ESI） mode using multiple monitoring（ MRM） for analysis of six components. Result： The linear ranges of adenosine,cytidine,guanosine,mannitol,adenine and cordycepin were 37. 5-1 200 μg·L- 1（ r = 0. 998 5）,20-640 μg·L- 1（ r = 0. 996 4）,40-1 280 μg·L- 1（ r = 0. 999 1）,77. 5-2 480 μg·L- 1（ r = 0. 993 5）,27. 5-880 μg·L- 1（ r = 0. 992 4）,90-2 880 μg·L- 1（ r = 0. 993 7）respectively. The recoveries of six analytes ranged from 92. 1% to 102. 6% and the relative standard deviations were all below 8. 1%. The average contents of adenosine,cytidine,guanosine,mannitol,adenine and cordycepin were 268. 33,11. 28,185. 66,1 421. 44,10. 67,812. 21 μg ·g- 1,respectively. Conclusion： A sensitive,accuracy and suitable UPLC-MS / MS method has been developed,and the method could be applied for the determination of adenosine,cytidine,guanosine,mannitol,adenine and cordycepin in Chinese Caterpillar Fungus.
出处
《中国实验方剂学杂志》
CAS
CSCD
北大核心
2015年第21期43-46,共4页
Chinese Journal of Experimental Traditional Medical Formulae
基金
国家"重大新药创制"科技重大专项(2012ZX09303009-002)
江苏省中医药领军人才项目(LJ200906)
江苏高校优势学科建设工程项目(2010)
