宋更申, 徐艳梅, 周丽, 张兰桐. GC-MS法同时测定蛇床子中7种香豆素类活性成分J. 药学学报, 2016,51(4): 626-630. doi: 10.16438/j.0513-4870.2015-0649
引用本文: 宋更申, 徐艳梅, 周丽, 张兰桐. GC-MS法同时测定蛇床子中7种香豆素类活性成分J. 药学学报, 2016,51(4): 626-630. doi: 10.16438/j.0513-4870.2015-0649
SONG Geng-shen, XU Yan-mei, ZHOU Li, ZHANG Lan-tong. Simultaneous quantification of 7 coumarins in common cnidium fruit by GC-MSJ. Acta Pharmaceutica Sinica, 2016,51(4): 626-630. doi: 10.16438/j.0513-4870.2015-0649
Citation: SONG Geng-shen, XU Yan-mei, ZHOU Li, ZHANG Lan-tong. Simultaneous quantification of 7 coumarins in common cnidium fruit by GC-MSJ. Acta Pharmaceutica Sinica, 2016,51(4): 626-630. doi: 10.16438/j.0513-4870.2015-0649

GC-MS法同时测定蛇床子中7种香豆素类活性成分

Simultaneous quantification of 7 coumarins in common cnidium fruit by GC-MS

  • 摘要: 建立了同时测定蛇床子中7种香豆素类活性成分的GC-MS分析方法。采用DB-1毛细管柱(30 m×0.25 mm×0.25 μm),柱温采用程序升温,接口温度280℃,离子源温度250℃,四极杆温度150℃,采用电子轰击离子化(EI源)电离方式,电子能量70 eV,选择离子检测模式(SIM),扫描范围为50~350 amu。考察了方法的灵敏度、线性范围、回收率、日内和日间精密度。在本方法条件下, 7种香豆素类活性成分的线性关系良好(r2≥0.9986),检测限和定量限分别为1.06~10.11 ng·mL-1和3.21~29.88 ng·mL-1。日内(n=6)和日间(n=3)精密度分别为0.7%~2.5%和1.2%~3.3%。平均回收率范围为92.38%~100.50%。本方法简便、快速、灵敏度高、专属性好,可为蛇床子药材的质量控制提供参考依据。

     

    Abstract: A GC-MS-SIM method was developed for the simultaneous determination of the 7 coumarins in common cnidium fruit. The 7 bioactive constituents were separated on DB-1 capillary column (30 m×0.25 mm, 0.25 μm) using temperature programming. The interface temperature was set at 280℃; Ion source temperature:250℃; Quadrupole temperature:150℃; EI mode:70 eV; The mass spectrometer detector was in SIM mode; Scan range:50-350 amu. All the 7 marker substances showed good linearity (r2>0.9986) in the test ranges. The LODs and LOQs for the compounds ranged from 1.06 to 10.11 ng ·mL-1 and from 3.21 to 29.88 ng·mL-1, respectively. The overall intra-day (n=6) and inter-day (n=3) RSDs were 0.7%-2.5% and 1.2%-3.3%, respectively. The overall recoveries were between 92.38% and 100.50% for all compounds. This method was simple, rapid, sensitive, with good specificity, and it can provide a reference for the quality control of common cnidium fruit.

     

/

返回文章
返回