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Preparation of iron chlorophyllin sodium salt

    At present, sericulture has become a major industry in our country. According to relevant data, there are 1,687,500 tons of dried silkworm sand in China every year. Silkworm sand is rich in chlorophyll, pectin, phytoalcohol, carotenoids and other precious ingredients.in order to improve the comprehensive utilization of silkworm sand and change waste into treasure, the study on extracting chlorophyll from silkworm sand and preparing its derivatives has good economic and social benefits. The biggest active component in silkworm sand is natural chlorophyll, which has a wide range of uses, but its thermal stability and photostability is poor, so people prepare various stable chlorophyll metal derivatives according to the structure characteristics of chlorophyll and use them. At present, the most studied salt is sodium copper chlorophyllin, but the copper ion in it is a heavy metal and has some disadvantages such as toxicity. In this paper, bivalent iron is used to replace copper ions to form sodium iron chlorophyllin, which can not only be used as a colorant, but also provide iron needed by human body and reduce toxicity. However, the research on sodium iron chlorophyllin is not mature at present, and there are few reports on the preparation of sodium iron chlorophyllin from silkworm sand. Therefore, this paper explores a simple process, less pollution and efficient preparation of sodium iron chlorophyllin from silkworm sand, which lays a theoretical foundation for further development. The main contents of this paper are as follows: (1) The preparation of sodium iron chlorophylls by indirect method was explored. The optimized conditions were as follows: dry silkworm sand 2g, softener 3mL, softening time 20min, microwave radiation time 65s, ultrasonic time 31min, extraction temperature 60℃, extraction time 2h; The technological conditions of preparation of sodium iron chlorophyllin by saponification of paste chlorophyll were optimized by orthogonal test scheme. The optimized conditions were as follows: The pH of the system is 12, the saponification temperature is 60℃, the saponification time is 80min, after the saponification, the pH of the system is 2 ~ 3, the acidification time is 30min, the iron content is 4mL, the iron temperature is 65℃, the iron time is 80min. (2) The effect of softening treatment on the extraction rate of chlorophyll was studied, and the experimental results showed that softening can greatly improve the extraction rate of chlorophyll; Through scanning electron microscope analysis and comparison of the original silkworm sand and the softened silkworm sand, the results further illustrate the softening effect, which can make the cells absorb water and expand, thus easy to be broken, and can fully contact with the organic solvent, so as to improve the extraction rate. (3) The technological conditions of preparation of sodium iron chlorophyllin by direct saponification were studied. Optimized by single factor test and orthogonal test, the optimal extraction conditions were as follows: 10g dry silkworm sand powder was first in the system of pH≈12, ultrasonic 120min at 80℃; Then in the system with pH≈2 ~ 3, acidize for 30min at 65℃, add 6ml 10%FeSO4 solution, and place iron for 150min. Finally, adjust the solution with 10%NaOH-CH3CH2OH to make the chaloferric acid to salt out. (4) The process comparison test of direct and indirect preparation method was carried out. The results show that the direct preparation method not only has higher yield than indirect preparation method, but also is simpler than indirect preparation method, which not only saves the production cost but also improves the production. Therefore, direct preparation method is superior to indirect preparation method. (5) Through the characterization and analysis of the prepared products, it was found that the dried products were dark green crystals, prepared with 0.01% sodium iron chlorophyllin salt solution, and scanned its absorption spectrum by 7230G UV-visible spectrophotometer. The maximum absorption wavelength was found at 405nm and 655nm, which was consistent with the literature reports. The infrared characterization of the prepared product and the commercial sample showed that the infrared absorption spectra of the prepared product and the commercial sample were basically the same, with the structural characteristics of chlorophyll porphyrin ring, and the absorption peak generated by the moderate intensity Of Fe-N vibration at about 875cm-1. Therefore, the prepared product was proved to be iron chlorophyll-sodium salt. (6) By studying the properties of the prepared products, it is found that the photostability of sodium iron chlorophyllin is poor; When the temperature is lower than 80℃, the temperature has almost no effect on it, while when the temperature is higher than 80℃, the stability is poor. It is relatively stable under neutral or alkaline conditions, but unstable under acidic conditions. Most of the low concentration of food additives such as vitamin C, sodium benzoate, citric acid, sodium chloride, glucose are not affected; Strong reduction resistance and poor oxidation resistance; It is stable to some metal ions such as K+, Cu2+ and Al3+, but unstable to Ca2+ and Mn2+.

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