HPLC法测定二氢杨梅素含量的操作规程 |
发布时间:2022-12-17 信息来源:admin 发布人:admin 点击次数:313 |
HPLC法测定二氢杨梅素含量的操作规程 起草单位:长沙上禾生物科技有限公司 目 的:HPLC法测定二氢杨梅素含量的操作规程 责任人:QC员。 内 容: 1、 试剂 1.1 甲醇(HPLC级) 1.2 蒸馏水(AR级) 1.3冰醋酸(HPLC级) 2、 对照品 二氢杨梅素(购自中国药品生物制品检定所) 3、 仪器和用具 3.1 电子天平(1/100000) 3.2 玻璃仪器:100ml容量瓶 3.3 安捷伦1220 HPLC 4、液相条件 4.1流动相:甲醇:水:冰醋酸=50:50:1 4.2检测波长:292nm 4.3流速:1ml/min 4.4柱温:30℃ 5 、 操作步骤 5.1 对照品溶液的制备 精密称取在110℃干燥至恒重的二氢杨梅素对照品10mg,置50ml容量瓶中,加50%甲醇适量,超声处理10min使溶解,放冷,加50%甲醇至刻度,摇匀,备用。 5.2样品溶液制备 精密称取在110℃干燥至恒重的二氢杨梅素样品10mg,置50ml容量瓶中,加50%甲醇适量,超声处理10min使溶解,放冷,加50%甲醇至刻度,摇匀,备用。 6、检测 取对照品溶液和样品溶液0.22μm针孔过滤器过滤,进样20μl,根据峰面积计算样品含量。 含量按以下公式计算: A2 x C1 x T R=------------------------- x 100 A1 x C2 C1: 对照品的参考浓度,mg/ml C2: 样品的参考浓度,mg/ml A1: 对照品溶液的色谱主峰值面积 A2: 样品溶液的色谱主峰值面积 T: 对照品的含量 藤茶生产工艺流程 藤茶提取物-二氢杨梅素生产工艺流程: 原料→挑洗→去杂→粉碎→乙醇提取→浓缩→离心→上大孔树脂柱→20%,40%,60%,80%乙醇分别洗脱 →分段收集→脱色→结晶→干燥→混合、筛分、包装→检测合格后入库 参考文献: 1.Seymour RB, Deanin RD, editors. History of polymeric composites. Utrecht, The Netherlands: VNU Science Press; 1987. pp. 223. 2.Nedelcev T, Krupa I, Csomorova K, Janigova I, Rychly J. 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