Study On Quality Of Tangerine Seed And Purification Of Limonoids

Tangerine Seed is dry mature seed of Citrus reticulata Blanco and the variation of it. The efficacy of Tangerine Seed are regulating qi, eliminating the lump and relieving pain, for the treatment of acute mastitis,mammary gland hyperplasia,the effect of Tangerine Seed is significant, have great medicinal value, But at present,the quality standard of Tangerine Seed is not perfect;Studies have shown that the limonoids are active ingredients of Tangerine Seed, These compounds pharmacological effects is clear, with good development prospects.However, few studies on the the limonoids purification process, and the extract purity is too low. The purpose of this subject is to improve the quality standards and obtain high purity of limonoids, mainly on the following aspects were studied:1. Study on Quality of Tangerine Seed:(1)Establish the HPLC examination method, determine the content of Limonin and Nomilin.(2)Doing the content determination of18batch of Tangerine Seed:Suggesting Limonin and Nomilin to Tangerine Seed posted under item as "the content determination" index component, according to the Tangerine Seed dry product calculation, Tangerine Seed medicine contain the content of limonin can not less than0.49%, the content of nomilin must not be less than0.28%.(3)Doing the content determination of different processed products of Tangerine Seed:the content of limonin and nomilin is lower after tangerine seed proceessed, the descending order is heating drugs with salt> stir-fried>stir-fried with bran.(4)The content of limonin and nomilin in Tangerina seed from October to February is monitored:the content of limonin and nomilin are increased to different extent from October to December;Since the January of next year, the content of limonin and nomilin began to fall, until the end of the fruiting period.(5)Doing the identification microscopic quantitative study about the different varieties of Tangerine seed:long size and short size of calcium oxalate solitary crystal in the seeds of red tangerine and pokan has significant difference (P<0.05),we can distinguish differences between the two species.(6)Through the research of HPLC fingerprint of all the18samples:there are11common peaks in total,peak4is hesperidin,peak9is limonin,peak10is nomilin; All the similarity of the18samples were more than0.90compared with the control group. It showed that the chemical composition of Tangerine Seed are stable.2. Study on Purification of Limonoids:(1)Doing the inspection on HPD-722macroporous resin with loading conditions(concentration of the sample,flow rate of sample,pH value of sample), and elution conditions(concentration of eluent, pH value of eluent,flow rate of eluent,amount of eluent):The purification technological parameters after optimizatio:sample concentration is3.50mg· mL-1-5.50mg mL-1,the flow rate is1BV/h-2BV/h, pH is about6;using1BV of distilled water cleaning; the best solution is80%ethanol solvent elution, the elution flow rate is2BV/h, the eluent pH is7, the elution volume is6BV.(2)It can prepare high-purity limonoids, it contains limonoids more than80%, contains limonin more than20%, contains nomilin more than40%, effectively improve the purity of limonoids.The residues of macroporous resin in accordance with the relevant provisions.This topic provides a theoretical basis for the quality control of Tangerine Seed, at the same time to prepare high purity limonoids extract. For Chinese medicine objectification, modernization and internationalization laid a foundation.