Method for preparing low-arsenic oyster protein peptide through targeted nano silica gel material adsorption
A technology of oyster protein peptide and nano-silica gel, which is applied in the field of oyster protein peptide, can solve the problems of limited arsenic removal rate and unsuitable arsenic removal, and achieves excellent removal effect, excellent effect and low cost.
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Embodiment 46
[0114] Under a nitrogen atmosphere, a solution of 3-mercaptopropyltrimethoxysilane (0.16 mol) and allyl chloride (0.32 mol) was stirred under reflux for 2 h, during which 0.05 g of AIBN was added every 15 min. Excess allyl chloride was removed under reduced pressure, then a solution of 2-mercapto 1-sodium sulfide ethane (0.16mol) in methanol (50ml) was added, the resulting solution was refluxed for 2h and sodium methoxide (0.16mol) was added. After 15 min, 1-chloro, 3-thioacetylpropane (0.16 mol) was added, and the mixture was heated to reflux for 2 h. Morpholine (0.16 mol) was added and the mixture was refluxed for 2h. The sodium chloride was filtered off and the resulting solution was added to a stirred mixture of silica gel (120 g, 150-300 μm, 100 OA) and xylene (320 ml). The resulting mixture was heated with stirring at 120 °C for 1 h, during which time methanol was distilled off by a Dean-Stark apparatus. Add 3-mercaptopropyltrimethoxysilane (0.05mol), and continue heat...
Embodiment 1B
[0117] Taking oyster protein peptide powder from a certain company in Hubei as a sample, after testing, it contained 12.78 mg / kg of arsenic. Take 30 g of the oyster protein peptide powder, dissolve it with 20 wt % phosphoric acid solution to 100 ml, add 5 g of the Adsorbent, reflux and stir at 80°C for 2 hours, and filter after cooling to room temperature. The filter residue is the adsorbent that has adsorbed arsenic, and the filtrate is oyster protein peptide powder solution. Put the filtrate in a vacuum drying oven to dry for 24 hours. Refer to GB5009 for sampling. 11-2014 The second method of the first article was used to measure the total arsenic. After the adsorption, the arsenic content in the oyster peptide powder was reduced to 0.89mg / kg.
[0118] Note: The concentration of the acid solution is the mass concentration, the same below.
Embodiment 1C
[0120] Using the targeted nano-silica gel material in Example 1A as an adsorbent, it is applied to the removal of arsenic in oyster protein peptide powder;
[0121] Taking oyster protein peptide powder from a company in Shandong Province as a sample, it was detected that it contained 7.94 mg / kg of arsenic. Take 10 g of the oyster protein peptide powder, dissolve it with 35% hydrochloric acid solution to 100 ml, and add 5 g of it to the above-mentioned Example 1A reflux and stir at 60°C for 4 hours, and filter after cooling to room temperature. The filter residue is the adsorbent that has adsorbed arsenic, and the filtrate is oyster protein peptide powder solution. Put the filtrate into a freeze dryer to dry for 48 hours. Refer to GB5009 for sampling. 11-2014 The second method of the first article was used to measure the total arsenic. After the adsorption, the arsenic content in the oyster peptide powder was reduced to 0.66mg / kg.
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