中国中药杂志

2015, v.40(16) 3209-3213

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LC-MS结合HPLC-DAD对银杏二萜内酯葡胺注射液原料中黄酮类成分的限度检测方法研究
Study on limit detection of flavones in diterpene ginkgolides meglumine injection materials by LC-MS and HPLC-DAD

毕森;李艳静;黄文哲;康丹瑜;丁岗;萧伟;
BI Sen;LI Yan-jing;HUANG Wen-zhe;KANG Dan-yu;DING Gang;XIAO Wei;Jiangsu Kanion Pharmaceutical Co.,Ltd.;State Key Laboratory of New-Tech for Chinese Medicine Pharmaceutical Process;

摘要(Abstract):

该实验采用LC-MS对银杏二萜内酯葡胺注射液原料中所含黄酮类成分的种类进行筛选,通过紫外-可见分光光度法(UV-Vis)和高效液相色谱法(HPLC-DAD)对银杏二萜内酯葡胺注射液原料中黄酮类成分限量检查灵敏度比较,发现HPLCDAD的检测限约为UV-Vis的1/100,即HPLC-DAD检测灵敏度更高。基于LC-MS筛选结果选用槲皮素、山柰素和异鼠李素为对照品,采用Agilent Eclipse plus C18色谱柱(4.6 mm×250 mm,5μm);0.4%磷酸-甲醇(50∶50)为流动相,等度洗脱;流速1.0 m L·min-1;检测波长360 nm。结果显示,此法专属性、精密度、重复性良好;槲皮素、山柰素和异鼠李素检测限分别为27.6,22.3,29.5μg·L-1;平均回收率在88.3%~91.7%;基于10批次样品检测结果和仪器灵敏度,最终确定银杏二萜内酯葡胺注射液原料中总黄酮醇苷的含量不得过2×10-5。该方法简便、快捷,可操作性好,可用于银杏二萜内酯葡胺注射液原料中黄酮类成分的限度检测。
Limit test of flavones in diterpene ginkgolides meglumine injection materials by UV-Vis and HPLC-DAD method was studied in this essay. The HPLC-DAD method has lower LOD( about 1% of the UV-Vis),that is,the sensitivity is higher than UVVis method. Through the analysis of the kinds of flavonoids ingredients in the samples by LC-MS,the three compounds with highest contents are kaempferol,quercetin and isorhamnetin. Kaempferol,quercetin and isorhamnetin were chosen as reference compounds for HPLC analysis,and the HPLC separation analysis was carried on an Agilent Eclipse plus C18column( 4. 6 mm × 250 mm,5 μm) with methanol and water containing 0. 4% phosphoric acid( 50∶ 50) as mobile phase,and the flow rate was 1. 0 m L·min- 1. The detection wavelength was set at 360 nm. This method has good specificity,precision and reproducibility. The LODs of quercetin,kaempferide and isorhamnetin were 27. 6,22. 3,29. 5 μg · L- 1. The average recovery was 87. 9%( RSD 3. 3%),91. 7%( RSD 3. 1%),88. 3( RSD 1. 3%) for quercetin,kaempferide and isorhamnetin,respectively. Based on the 10 batches of sample results and sensitivity of different HPLC,the content of total flavonoids ingredients of diterpene ginkgolides meglumine injection materials was limited no more than 2 × 10- 5. This method is simple,quick and has good maneuverability,and could be used to the limit test of flavonoids in the diterpene ginkgolides meglumine injection materials.

关键词(KeyWords): LC-MS;HPLC-DAD;UV-Vis;银杏二萜内酯葡胺注射液原料;黄酮;限度检测
LC-MS;HPLC-DAD;UV-Vis;diterpene ginkgolides meglumine injection materials;flavonoids;limit detection

Abstract:

Keywords:

基金项目(Foundation): 国家“重大新药创制”科技重大专项(2013ZX09402203)

作者(Author): 毕森;李艳静;黄文哲;康丹瑜;丁岗;萧伟;
BI Sen;LI Yan-jing;HUANG Wen-zhe;KANG Dan-yu;DING Gang;XIAO Wei;Jiangsu Kanion Pharmaceutical Co.,Ltd.;State Key Laboratory of New-Tech for Chinese Medicine Pharmaceutical Process;

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