Study On Impurities In Gastrodin

Objective(s):Enrich and separate the related impurities of gastrodin from the stock solution of gastrodin in industrial production,determine the structure of the impurities by spectrum analysis,and then explore the law of gastrodin impurity production by acid-base hydrolysis method to stably obtain gastrodin impurities,which is the quality study of gastrodin provide impurity reference products for future control of impurities in gastrodin products.Methods:(1)Explore the method of separating the impurities of gastrodin stock solution by column chromatography.The method of column chromatography separation of gastrodin stock solution is:methanol/dichloromethane for impurities with Rf value of 0.5 to 0.7,0%-10%,0-20 min;10%-10%,20-50 min;10%-15%,50-60 min;15%-15%,60-100 min.For ethyl acetate/petroleum ether system with Rf value of 0.7 to 0.9,0%-40%,0-20 min;40%,20-40 min;40%-60%,40-80 min.Obtained gastrodin impurities with a purity of more than 95%.(2)Determine the structure of impurities by infrared spectroscopy,mass spectrometry,nuclear magnetic hydrogen spectroscopy,and nuclear magnetic carbon spectroscopy.(3)Explore the acquisition method of gastrodin impurities by acid-base hydrolysis of pentaacetyl gastrodin.Results:(1)Impurity 1,Impurity 2,Impurity 3,Impurity 4,Impurity 5,were obtained from industrial gastrodin enriched stock solution.(2)Spectral analysis confirmed the structure of impurity 1 as:4-acetylmethylphenyl-?-D-glucopyranoside;impurity 2:4-acetylmethylphenyl-6'-O-acetyl-?-D-Glucopyranoside;impurity 3:4-hydroxymethylphenyl-2 ',3 ',4 ',6'-tetra-O-acetyl-?-D-glucopyranoside;impurity 4:4-aldehyde methylphenyl-?-D-glucopyranoside;impurity 5:p-hydroxybenzyl alcohol.(3)Screening and exploration found that using 30 mg of sodium methoxide and 10 g of pentaacetyl gastrodin in 40 ml of methanol can be obtained stably,impurity 1,impurity 2,and impurity 3.Impurity 4 was found through forced degradation experiments,and Impurity 5 was gastrodin degradation impurities.Conclusion(s):Five impurities were obtained from the gastrodin industrial stock solution,and the structure of gastrodin related impurities was determined by spectrum analysis.Impurity 1,impurity 2,and impurity 3 are process impurities in the production of gastrodin,impurity 4,and impurity 5 are gastrodin Degradation impurities in production.Impurity 1 and Impurity 2 are the first compounds reported as impurities in the gastrodin process.Finally,through the acid-base hydrolysis of pentaacetyl gastrodin to explore the method to obtain gastrodin impurities.