摘要
目的 完善大黄碳酸氢钠片质量标准.方法 TLC法对大黄酸、大黄素、大黄酚、芦荟大黄素、大黄素甲醚、土大黄苷进行定性鉴别,建立UPLC指纹图谱,测定芦荟大黄素-8-O-β-D-葡萄糖苷、大黄酸-8-O-β-D-葡萄糖苷、大黄素-8-O-β-D-葡萄糖苷、大黄酚-8-O-β-D-葡萄糖苷、大黄素甲醚-8-O-β-D-葡萄糖苷、芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚的含量.结果 TLC斑点清晰,专属性强.8批样品指纹图谱中有20个共有峰,相似度均大于0.535.10种成分在各自范围内线性关系良好(r≥0.997 0),平均加样回收率98.7％～104.1％,RSD 0.59％～2.13％,含量范围分别为 0.274 1～2.005 9、0.547 8～5.192 2、1.209 2～3.936 3、1.039 3～3.330 2、0.307 0～1.248 1、0.118 2～0.674 7、0.115 1～0.970 3、0.224 5～1.789 3、0.881 4～4.882 6、0.801 4～5.099 1 mg/g.结论 该方法简便稳定,可有效控制大黄碳酸氢钠片中大黄质量.
Abstract
AIM To improve the quality standard for Dahuang Sodium Bicarbonate Tablets.METHODS TLC was adopted in the qualitative identification of rhein,emodin,chrysophanol,aloe-emodin,physcion and rhapontin,after which UPLC fingerprints were established,content determination of aloe emodin-8-O-β-D-glucoside,rhein-8-O-β-D-glucoside,emodin-8-O-β-D-glucoside,chrysophanol-8-O-β-D-glucoside,physcion-8-O-β-D-glucoside,aloe-emodin,rhein,emodin,chrysophanol,physcion were performed.RESULTS The clear TLC plots demonstrated good specificity.There were 20 common peaks in the fingerprints for 8 batches of samples with the similarities of more than 0.535.Ten constituents showed good linear relationships within their own ranges(r≥0.997 0),whose average recoveries were 98.7％-104.1％with the RSDs of 0.59％-2.13％,whose content ranges were 0.274 1-2.005 9,0.547 8-5.192 2,1.209 2-3.936 3,1.039 3-3.330 2,0.307 0-1.248 1,0.118 2-0.674 7,0.115 1-0.970 3,0.224 5-1.789 3,0.881 4-4.882 6,0.801 4-5.099 1 mg/g,respectively.CONCLUSION This simple and stable method can effectively control the quality of Rhei Radix et Rhizoma in Dahuang Sodium Bicarbonate Tablets.
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