喉舒宁片质量标准的提高  

Improvement of the quality standard for Houshuning tablets

作　　者：陈贵 夏稷子 徐作刚 CHEN Gui;XIA Ji-zi;XU Zuo-gang(Qiannan Inspection and Testing Institute,Duyun 558000,China)

机构地区：[1]黔南州检验检测院,都匀558000

出　　处：《药物分析杂志》2020年第7期1325-1333,共9页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:提高喉舒宁片的质量标准。方法:采用TLC法对白花蛇舌草、穿心莲和山芝麻进行定性鉴别;HPLC法测定去乙酰车叶草酸甲酯、穿心莲内酯、脱水穿心莲内酯的含量。白花蛇舌草的定性鉴别采用G型硅胶薄层板,以乙酸乙酯-甲醇-水(8∶2∶1)为展开剂,喷以10%硫酸乙醇溶液并在105℃加热显色,日光下检视;穿心莲的定性鉴别采用GF254型硅胶薄层板,以三氯甲烷-乙酸乙酯-甲醇(20∶15∶2)为展开剂,在紫外光254 nm下检视;山芝麻的定性鉴别采用G型硅胶薄层板,以甲苯-三氯甲烷-甲酸乙酯(3∶2∶4)为展开剂,喷以磷钼酸试液并在105℃加热至斑点显色,日光下检视。去乙酰车叶草酸甲酯、穿心莲内酯、脱水穿心莲内酯的HPLC法含量测定,采用C18色谱柱(250 mm×4.6 mm,5μm),以乙腈(A)-甲醇(B)-水(C)为流动相,梯度洗脱(0~10 min,0%A,4%B,96%C;10~60 min,0%A→66%A,4%B,96%C→30%C),流速1.0 mL·min^-1,柱温30℃,检测波长236nm,进样量10μL。结果:定性鉴别,TLC斑点清晰,阴性无干扰。定量测定,去乙酰车叶草酸甲酯、穿心莲内酯、脱水穿心莲内酯质量浓度分别在0.3320~16.60μg·mL^-1(r=0.9999)、5.144~257.2μg·mL^-1(r=1.0000)、4.214~210.7μg·mL^-1(r=1.0000)范围内线性关系良好;平均加样回收率分别为95.1%(RSD=2.6%)、103.0%(RSD=2.5%)、100.9%(RSD=1.7%);3批样品中去乙酰车叶草酸甲酯、穿心莲内酯、脱水穿心莲内酯的含量范围分别为0.238~0.311、4.960~5.581、4.541~5.548 mg·g^-1。结论:该方法提高了喉舒宁片质量标准,可用于其质量控制。Objective:To improve the quality standard of Houshuning tablets.Methods:The identification of Hedyotis Diffusa Herba,Andrographis Herba and Helicteris Radix were carried out by TLC.Contents of deacetyl asperulosidic acid methyl ester,andrographolide and dehydroandrographolide were determined by HPLC.The identification of Hedyotis Diffusa Herba was performed on silica gel G plate,with ethyl acetate-methanolwater(8∶2∶1)as developing solvent and 10%sulfuric acid in ethanol as spraying reagent.The plate was inspeced under daylight after heated at 105℃to the spots clear.The identification of Andrographis Herba was performed on silica gel GF254 plate,with chloroform-ethyl acetate-methanol(20∶15∶2)as developing solvent,and inspected under ultraviolet light at 254 nm.The identification of Helicteris Radix was performed on silica gel G plate,with toluene-chloroform-ethyl formate(3∶2∶4)as developing solvent and phosphomolybdic acid solution as spraying reagent.The thin-layer plate was inspeced under daylight after heated at 105℃to the spots clear.The quantitative analysis was performed on a thermostatic C18 column(250 mm×4.6 mm,5μm)at 30℃,with the mobile phase comprising of acetonitrile(A)-methanol(B)-water(C)at a flow rate of 1.0 mL·min^-1 in a gradient elution manner(0^-10 min,0%A,4%B,96%C;10-60 min,0%A→66%A,4%B,96%C→30%C).The detection wavelength was set at 236 nm,and the injection volume was 10μL.Results:The TLC spots were clear without negative interference.The linear ranges of deacetyl asperulosidic acid methyl ester,andrographolide and dehydroandrographolide were 0.3320^-16.60μg·mL^-1(r=0.9999),5.144-257.2μg·mL^-1(r=1.0000)and 4.214-210.7μg·mL^-1(r=1.0000),respectively.The average recoveries were 95.1%(RSD=2.6%),103.0%(RSD=2.5%)and 100.9%(RSD=1.7%),respectively.The contents of deacetyl asperulosidic acid methyl ester,andrographolide and dehydroandrographolide in 3 batches of samples were 0.238-0.311,4.960-5.581,4.541-5.548 mg·g^-1,respectively.Conclusion:The method impro ves the qual

关 键 词：喉舒宁片 白花蛇舌草 穿心莲 山芝麻 去乙酰车叶草酸甲酯 穿心莲内酯 脱水穿心莲内酯 定性定量 薄层色谱 高效液相色谱 

分 类 号：R917[医药卫生—药物分析学]