响应面分析法优化家蚕1-脱氧野尻霉素的稀酸浸提工艺

本文以稀HCl从蚕粉中提取1-脱氧野尻霉素（1-deoxynojirimycin,1-DNJ）,通过单因素试验确定提取影响因素的水平,并采用响应面法研究料液比分数、浸提温度和浸提时间对蚕粉1-DNJ提取工艺的影响。其中1-DNJ含量测定采用9-芴基氯甲酸甲酯（FMOC-Cl）衍生化法,并用反相高效液相色谱对其衍生物进行测定。1-DNJ高效液相色谱检测谱图表明,通过液相色谱荧光可以检测蚕粉来源的1-DNJ。响应面优化实验结果表明,1-DNJ的最佳提取条件为：提取时间3.3h,浸提温度72.9℃,料液比分数为1：282。在此条件下,1-DNJ的理论提取率为0.493%,实际提取率为0.487%,相对误差为1.2%。本研究初步建立了稀酸浸提家蚕1-DNJ的二次多项数学模型,确定其最佳提取工艺条件,为工业化生产提供参考。

Optimizational Process of 1-Deoxynojirimycin Extraction from Silkworm Larvae by Response Surface Methodology

Diluted acid HCl was applied in this study for silkworm 1-DNJ extraction on the basis of single factor investigation so as to verify the influence level and three factors,the ratio of solid to liquid,temperature and extraction time follow by response surface methodology （RSM） to gain the optimum extraction yield.The extracted 1-DNJ was precolumnly derivatized with 9-fluorenylmethel chloroformate （FMOC-Cl） to achieve DNJ-FMOC,and determined by reverse-phase high performance liquid chromatograph equipped with fluorescence detector.The HPLC-FD chromatogram detecting of 1-DNJ from silkworm powders via HPLC was feasible.The results of RSM showed that the optimal extraction condition were defined as temperature 72.9℃,3 hours for 18 minutes and 1：282 of solid to liquid.The extracted ratio of 1-DNJ after optimization was 0.493%,while predicted value was 0.487%,the relative error was 1.2%.In this research,a second order quadratic equation for 1-deoxynojirimycin （1-DNJ） extraction from the silkworm,Bombyx mori,was established in order to define optimal condition for commercial process.