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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。
In this experiment, the types of flavonoids contained in the raw materials of ginkgo diterpene lactone meglumine injection were screened by LC-MS. The flavonoids were identified by UV-Vis and HPLC-DAD ) Ginkgo diterpene lactone meglumine injection of flavonoids in the raw materials to limit the sensitivity of the test and found that HPLCDAD detection limit of about UV-Vis 1/100, that HPLC-DAD detection sensitivity higher. Based on the results of LC-MS screening, quercetin, kaempferol and isorhamnetin were selected as reference materials and analyzed by Agilent Eclipse plus C18 column (4.6 mm × 250 mm, 5 μm), 0.4% phosphoric acid-methanol (50:50) As mobile phase, isocratic elution; flow rate 1.0 m L · min-1; detection wavelength 360 nm. The results showed that the specificity, precision and reproducibility of this method were good. The detection limits of quercetin, kaempferol and isorhamnetin were 27.6, 22.3 and 29.5 μg · L-1, respectively. The average recoveries ranged from 88.3% to 91.7 %. Based on the results of 10 batches of samples and the sensitivity of the instrument, the total flavonol glycoside content of the diterpene lactone meglumine injection of ginkgo should not exceed 2 × 10 -5. The method is simple, rapid, and has good operability, and can be used for detecting the flavonoid components in the raw materials of diterpene lactone meglumine injection.