| As an essential factor for animal growth,inositol has many biological activities such as lowering cholesterol and promoting hair growth,and is widely used in medicine,food,feed and other fields.Because of the six hydroxyl groups in its structure,it is easily soluble in water,but hardly soluble or insoluble in lipid systems,so its application is limited.Based on the demand for inositol modification to create new products with specific functional characteristics,this research uses fatty acid chloride to esterify the hydroxyl groups of inositol to prepare fatty acid inositol esters.The chemical separation method is used to separate and purify the products,and the product structure was characterized.Provide a reference for the in-depth development and utilization of inositol.A reverse-phase HPLC-ELSD method for the determination of inositol was established.Using methanol-0.1%acetic acid aqueous solution as the mobile phase,the standard curve equation y=3334026x-2572 between the concentration of inositol and the peak area was established in the concentration range of 0.01-1.0 mg/m L,and the correlation coefficient R~2was 0.9934.The accuracy of the instrument,the repeatability of the sample,the stability of the sample,and the recovery rate of the sample were analyzed.The results show that the detection method is accurate,reproducible,simple and reliable,and can be used for the quantitative analysis of inositol in this study.Using inositol and oleic acid chloride as raw materials,the reaction was carried out under vacuum conditions.Through single factor and response surface optimization,the optimal reaction conditions for preparing inositol oleate were obtained:reaction temperature160℃,reaction time 2.1 h,substrate The molar ratio is 1:9.35,and the stirring speed is 200rpm.Under these conditions,the conversion rate of inositol reached 98.75%.The reaction mixture was further washed with Na HCO3 solution,and the organic phase was collected to obtain a brown liquid after desolvation;the product was separated and purified by column chromatography,and the best eluent ratio was selected as n-hexane/ether=90/10.Identified and separated the products by TLC and HPLC,collected the high-purity products,and obtained a light-yellow liquid after rotary evaporation and vacuum drying.The purity of HPLC-ELSD analysis could reach 87%.The structure of the product was characterized by FT-IR,HPLC-MS,and NMR,and the product was determined to be inositol oleate.Lauroyl chloride was selected as the modified raw material,and the inositol laurate was prepared by heterogeneous reaction.The reaction temperature,reaction time,and the molar ratio of the substrate all have an impact on the inositol conversion rate.According to the experimental results,the level of different factors is analyzed.The changing trend of inositol conversion rate.The response surface optimization design was carried out on the basis of single factor experiments,and the best reaction conditions were obtained as follows:reaction temperature is 170℃,reaction time is 44 min,substrate molar ratio is 1:9,and stirring rate is200 rpm.Under these conditions,the conversion rate of inositol was 98.51±0.51%.Dissolve and filter the reacted mixture with chloroform;adjust the TLC developer and ratio to determine the best developer ratio as n-hexane/ether/glacial acetic acid=90/10/2;use column chromatography on the basis of TLC separation Separate and purify the products,choose the best eluent ratio as n-hexane:ether(95:5,v/v);identify the separated products by TLC and HPLC,collect the high-purity products,and dry by rotary evaporation and vacuum A white powder was obtained,and its liquid phase purity was 90%by HPLC analysis.The structure of the product was characterized by FT-IR,HPLC-MS,and NMR,and the product was determined to be inositol laurate. |
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