title: [Study on limit detection of flavones in diterpene ginkgolides meglumine injection materials by LC-MS and HPLC-DAD].
abstract: 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 UV-Vis 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 C18 column (4.6 mm x 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 mL x 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 x 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 x 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.
authors.forename: Sen
authors.initials: S
authors.lastname: Bi
authors.forename: Yan-jing
authors.initials: YJ
authors.lastname: Li
authors.forename: Wen-zhe
authors.initials: WZ
authors.lastname: Huang
authors.forename: Dan-yu
authors.initials: DY
authors.lastname: Kang
authors.forename: Gang
authors.initials: G
authors.lastname: Ding
authors.forename: Wei
authors.initials: W
authors.lastname: Xiao
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004224:Diterpenes / Q000032:analysis*; D004365:Drugs, Chinese Herbal / Q000032:analysis*; D047309:Flavones / Q000032:analysis*; D046934:Ginkgolides / Q000032:analysis*; D057230:Limit of Detection; D013058:Mass Spectrometry / Q000379:methods*
chemical_list: D004224:Diterpenes; D004365:Drugs, Chinese Herbal; D047309:Flavones; D046934:Ginkgolides