大黄碳酸氢钠片质量标准研究  

Quality Standard of Rhubarb and Sodium Bicarbonate Tablets

作　　者：王昆鹏[1] 张月娴 钟玮 邓晓锶 魏志雄[1] WANG Kunpeng;ZHANG Yuexian;ZHONG Wei;DENG Xiaosi;WEI Zhixiong(Dongguan Institute for Food and Drug Control,Dongguan,Guangdong,China 523808)

机构地区：[1]广东省东莞市食品药品检验所,广东东莞523808

出　　处：《中国药业》2025年第5期84-87,共4页China Pharmaceuticals

基　　金：广东省东莞市社会发展科技项目[20211800904842]。

摘　　要：目的完善大黄碳酸氢钠片的质量标准。方法采用薄层色谱(TLC)法对制剂中伪品大黄指标性成分土大黄苷进行定性鉴别;采用高效液相色谱法测定大黄中5种游离蒽醌芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚的含量,色谱柱为Shiseido Capcell PAK C_(18)柱(250 mm×4.6 mm,5μm),流动相为甲醇-0.2%磷酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长为254 nm,柱温为35℃,进样量为10μL。结果土大黄苷的TLC图斑点清晰,分离度好,且制剂中未检出土大黄苷。芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚的质量浓度分别在0.2472~39.5460μg/mL、0.2463~39.4022μg/mL、0.2393~38.2848μg/mL、0.2624~41.9866μg/mL、0.2076~8.3030μg/mL范围内与峰面积线性关系良好(r≥0.9997,n=7);精密度、稳定性、重复性试验结果的RSD均小于1.5%;平均加样回收率分别为100.36%,102.26%,102.17%,103.20%,103.38%,RSD分别为1.64%,1.35%,1.50%,1.62%,1.88%(n=6)。8批大黄碳酸氢钠片按处方折算,大黄粉中5种游离蒽醌总含量分别为0.18%,0.23%,0.37%,0.76%,0.36%,0.08%,0.12%,0.75%,大黄的质量差异较大。结论所建立的方法操作简便、结果准确可靠,可用于大黄碳酸氢钠片的质量控制。Objective To improve the quality standards of Rhubarb and Sodium Bicarbonate Tablets.Methods Thin-layer chromatography(TLC)method was used to qualitatively identify the indicator component of rhaponiticin.High-performance liquid chromatography(HPLC)method was used to determine the content of five free anthraquinones of rhubarb(aloe-emodin,rhein,emodin,chrysophanol and physcion)in Rhei Radix et Rhizoma.The chromatographic column was Shiseido Capcell PAK C_(18) column(250 mm×4.6 mm,5μm),the mobile phase was methanol-0.2%phosphoric acid solution(gradient elution),the flow rate was 1.0 mL/min,the detection wavelength was 254 nm,the column temperature was 35℃,and the injection volume was 10μL.Results The TLC spot of rhaponiticin was clear with good separation,and no rhaponiticin was detected in the preparation.The linear ranges of aloe-emodin,rhein,emodin,chrysophanol and physcion were 0.2472-39.5460μg/mL,0.2463-39.4022μg/mL,0.2393-38.2848μg/mL,0.2624-41.9866μg/mL,and 0.2076-8.3030μg/mL,respectively(r≥0.9997,n=7).The RSDs of precision,stability,and repeatability test results were all lower than 1.5%.The average recoveries of aloe-emodin,rhein,emodin,chrysophanol and physcion were 100.36%,102.26%,102.17%,103.20%,and 103.38%,with RSDs of 1.64%,1.35%,1.50%,1.62%,and 1.88%,respectively(n=6).According to the prescription,the total contents of five free anthraquinones in Rhei Radix et Rhizoma powder in eight batches of Rhubarb and Sodium Bicarbonate Tablets were 0.18%,0.23%,0.37%,0.76%,0.36%,0.08%,0.12%,and 0.75%,respectively,with a significant difference in the quality of Rhei Radix et Rhizoma.Conclusion The established method is simple,accurate and reliable,which can be used for quality control of Rhubard and Sodium Bicarbonate Tablets.

关 键 词：薄层色谱法 高效液相色谱法 大黄碳酸氢钠片 游离蒽醌 土大黄苷 质量标准 

分 类 号：R917[医药卫生—药物分析学] R975[医药卫生—药学]