Research On Extraction And Purification Of Spinosad

Spinosad was a new microbial pesticides,which was secondary metabolite produced byaerobic fermentation of saccharopolyspora spinosa.With the properties of both safety ofbiological pesticide for nontarget animal and fast effect of agrochemical,In this paper,resin adsorption technolog y combined with back-extracted are used to solid powder in a small test spinosad separation and purification technology research and amplification experiments.The main findings are as follows:At first,the method of detection and analysis for spinosad b y high performance liquid chrpmatography was established.The concentration of spinosad was accurately detected by HPLC.The physico-chemical characteristics of spinosad were reported in this paper.Spinosad was purified by solvent extraction,macroporous adsorbent resin,silica column chromatography and ion-exchange chromatography methods.The extraction,isolation and purification technique of spinosad were obtained.The use of back extraction of the aqueous phase crystallization technique the isotope separation of the oil phase sterilization,is determined as optimum p H = 2 with aqueous tartaric acid and back-extracted extracted three times,the extraction volume 1: 1(V / V),each extraction time 15 min,the combined aqueous phases;saturated Na HCO3 solution was p H adjusted aqueous phase crystallization solvent,adjusting the p H = 9-10 until no crystal precipitation,filtration,crystallization,yield spinosad powder accounts for 0.81% by weight purity of 63.1%.By orthogonal experiment to optimize the soli d powder after degreasing ultrasonic extraction process,the results showed that methanol as extraction reagent,ultrasonic frequency of 75 Hz,to extract solid-liquid ratio 1:15,extraction times twice every extraction time 80 min extraction efficiency is the highest,the extraction rate of 88.47%,the degree of influence on the extraction rate of spinosad three factors in this experiment were solid-liquid ratio> extraction times> extraction time.The effects of macroporous resin separation less than the ex traction of oil extract of spinosad technology,non-oil phase extract by macroporous resin adsorption,preferably acetone / water as eluent,results showed that 70% within ~ 95% acetone / water elution range,spinosad are largely eluted recovery rate of 80.72%.Research on the anion exchange resin after kill prime solution bleaching effect results after purification was: anion exchange resin decolorization 2.5h,filling amount of the resin was 5%(g / V),constant temperature shaker speed was 120 r / min,wherein the solution p H=9,the above conditions,anion exchange resin extraction spinosad decolorization rate of 75% solution,which spinosad loss rate of 3%.After bleaching products have significantly improved in color,it can basically meet the production requirements.150kg,400 kg of Solid powder were carried out for amplified process validation,after degreasing process,the aqueous phase was back-extracted crystallization process,ultrasonic extraction technology,macroporous resin purification process,bleaching process,150 kg solid powder obtained 1.8kg spinosad crude purity 67%;400kg 2.4kg spinosad powder obtained crude purity of 56%.