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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

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【作者】 宋更申徐艳梅周丽张兰桐

【Author】 SONG Geng-shen;XU Yan-mei;ZHOU Li;ZHANG Lan-tong;Hebei Medical University;Hebei Institute for Drug Control;CSPC Zhongqi Pharmaceutical Technology (Shijiazhuang) Co.Ltd.;

【机构】 河北医科大学河北省药品检验研究院石药集团中奇制药技术(石家庄)有限公司

【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×0.25μm),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 e V,选择离子检测模式(SIM),扫描范围为50350 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≥0.998 6),检测限和定量限分别为1.0610.11 ng·m L-1和3.2129.88 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 e V; The mass spectrometer detector was in SIM mode; Scan range: 50-350 amu. All the 7 marker substances showed good linearity(r2 > 0.998 6) 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·m L-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.

【关键词】 蛇床子香豆素含量测定GC-MS-SIM
【Key words】 common cnidium fruitcoumarinquantificationGC-MS-SIM
【基金】 河北省自然科学基金资助项目(H2012206079)
  • 【文献出处】 药学学报 ,Acta Pharmaceutica Sinica , 编辑部邮箱 ,2016年04期
  • 【分类号】R284.1;O657.63
  • 【被引频次】10
  • 【下载频次】434
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