风湿骨痛胶囊定性与定量质量控制方法研究

目的完善风湿骨痛胶囊的质量标准,提高其质量控制水平。方法以正己烷-三氯甲烷-乙酸乙酯-甲醇(4:7:6:2)为展开剂,碘蒸汽为显色剂,对麻黄、制川乌和制草乌进行薄层色谱鉴别;以乙酸乙酯-甲酸-冰醋酸-水(15:1:1:2)为展开剂,10%硫酸乙醇溶液为显色剂,对甘草进行薄层色谱鉴别;以三氯甲烷-乙酸乙酯-丙酮-甲酸(8:2:2:0.4)为展开剂,2,2-联苯基-1-苦基肼基(DPPH)无水乙醇溶液为显色剂,采用薄层-生物自显影技术对木瓜进行鉴别;建立同时测定苯甲酰新乌头原碱、苯甲酰乌头原碱和苯甲酰次乌头原碱含量的HPLC方法;建立测定甘草酸含量的HPLC方法。结果所建立的2个TLC方法,各斑点清晰,Rf值适中,分离度良好。薄层-生物自显影实现了鉴别木瓜的表征抗氧活性成分的目的。含量测定中苯甲酰新乌头原碱、苯甲酰乌头原碱和苯甲酰次乌头原碱的线性范围分别为2.200~280.0μg/mL、2.370~75.76μg/mL、3.180~101.6μg/mL,线性关系良好;各指标成分的相关系数均>0.9999,平均加样回收率为92%~107%,RSD为2.85%~5.62%。21批样品中3个指标成分含量分别为35.00~80.15μg/粒、6.92~13.57μg/粒、9.94~17.99μg/粒;甘草酸的线性范围为6.100~97.58μg/mL,线性关系良好;平均加样回收率为100.9%,RSD为1.95,21批样品中甘草酸含量为1.70~2.21 mg/粒。结论建立的相关的定性与定量方法准确灵敏,专属性强,重复性好,可用于风湿骨痛胶囊的质量控制。

Study on qualitative and quantitative quality control methods of Fengshigutong Capsules

Objective identification of Ephedra herba,Aconiti Radix Cocta(ARC) and Aconiti Kusnezoffii Radix Cocta(AKC) was conducted by using n-hexanechloroform-ethyl acetate-methanol(4:7:6:2)as the developing agent and iodine vapor as the developer. The TLC identification of Glycyrrhizae Radix Et Rhizoma(GRER)was conducted by using ethyl acetate-formic acid-glacial acetic acid-water(15:1:1:2)as the developing agent,and 10%sulfuric acid ethanol solution as the developer. The TLC-bioautography identification of Chaenomelis Fructus was conducted by using chloroform-ethyl acetate-acetone-formic acid(8:2:2:0.4)as the developing agent,2,2-biphenyl-1-picrylhydrazino(DPPH)anhydrous ethanol solution as the developer. The HPLC method was established for the simultaneous determination of benzoylmesaconine(BMA),benzoylaconine(BAC) and benzoylhypaconine(BHA) and their contents were determined. The HPLC method was established for glycyrrhizic acid and its content was determined.Results purpose of identifying and characterizing antioxidant active ingredients in Chaenomelis Fructus. The linear ranges of BMA,BAC and BHA in the content determination were 2.200~280.0 μg/mL,2.370~75.76 μg/mL,3.180~101.6 μg/mL,respectively. The inner linear relationship was good,correlation coefficient of each index component was greater than0.9999. The average recovery rates were between 92% and 107% with RSD between 2.85% and 5.62% for BMA,BAC and BHA. The contents of BMA,BAC and BHA in 21 batches of samples were 35.00~80.15 μg,6.92~13.57 μg,9.94~17.99 μg per capsule. The linear range of glycyrrhizic acid was 6.100~97.58 μg/m L. The inner linear relationship was good,and the average recovery rate was 100.9% with RSD of 1.95%. The content of glycyrrhizic acid in 21 samples was between 1.70 and 2.21 mg per capsule.ConclusionThe method is accurate,sensitive,specific,and reproducible and it can be used for the qualitycontrol of Fengshigutong Capsules.