Position: Home > Articles > Solid Phase Preparation and Characterization of L-Hydroxyproline-Cu(Ⅱ) under Pressurized Microwave Irradiation
FOOD SCIENCE
2017,38
(8)
213-219
加压微波固相法制备L-羟脯氨酸-Cu(Ⅱ)及其结构表征
作 者：
许先猛;董文宾;卢军;孙皎皎
单 位：
汉中市食品药品监督管理局;陕西科技大学化学与化工学院
关键词：
L-羟脯氨酸-Cu(Ⅱ);微波固相法;加压;二级处理;结构表征
摘 要：
为减少食品和动物饲料加工过程中无机铜的使用和添加对环境的污染和营养物质的浪费,开发新型氨基酸铜制剂具有重要意义。本实验从食品级猪皮明胶中分离制备L-羟脯氨酸(L-Hyp),并以L-Hyp和Cu SO_4·5H_2O为原料,采用固相微波辐射和加压二级处理的方法制备L-羟脯氨酸-Cu(Ⅱ)(L-Hyp-Cu(Ⅱ)),制备条件为:L-Hyp和Cu SO_4·5H_2O物质的量比2.5∶1,即10.5 g L-Hyp和8.0 g Cu SO_4·5H_2O充分混匀,加入引发水20 m L,微波功率600 W,添加除酸剂无水Na_2CO_3 5.6 g,微波时间180 s;二级加压处理,将微波辐射处理后的样品转入加压反应釜中,在二级反应温度90℃、二级反应压强15 MPa、搅拌速率100 r/min条件下,反应35 min。并用紫外光谱、红外光谱、X衍射、扫描电子显微镜、配合分析、元素分析、重量分析等手段对配合物的组成和结构进行表征。结果表明:经微波辐射和加压二级处理可以提高L-Hyp-Cu(Ⅱ)螯合率,产品螯合率为86.4%。通过表征分析发现,Cu(Ⅱ)与L-Hyp中的羧基和亚氨基发生配位,反应所得产物L-Hyp-Cu(Ⅱ)配位比为1∶2,分子式为Cu(C_5H_8NO_3)_2。
译 名：
Solid Phase Preparation and Characterization of L-Hydroxyproline-Cu(Ⅱ) under Pressurized Microwave Irradiation
作 者：
XU Xianmeng;DONG Wenbin;LU Jun;SUN Jiaojiao;College of Chemistry and Chemical Engineering,Shaanxi University of Science and Technology;Hanzhong Food and Drug Administration;
关键词：
L-hydroxyproline-Cu(Ⅱ);;microwave-assisted solid-state method;;pressurization;;two-stage treatment;;characterization
摘 要：
The significance of developing amino acid-chelated copper is evident to reduce environmental pollution and nutrient wastes caused by the use copper inorganic salts in food and feed processing. In this experiment, L-hydroxyproline(L-Hyp) was prepared and separated from food grade pig skin gelatin and further used to obtain L-hydroxyproline-Cu(Ⅱ)(L-Hyp-Cu(Ⅱ) with Cu SO4·5H_2O by sequential microwave irradiation and solid-state synthesis under pressurized conditions. The synthesis conditions were established as follows: after thorough mixing of L-Hyp with Cu SO_4·5H_2O at a molar ratio of 2.5:1 namely 10.5:8.0(m/m), the reaction was triggered by adding 20 m L of water followed by addition of 5.6 g of anhydrous Na_2CO_3 for acid removal under microwave irradiation for 180 s at 600 W, and then transferred to a pressurized reaction kettle at 90 ℃ and 15 MPa with an agitation speed of 100 r/min for 35 min. The composition and structure of the final product were characterized by ultraviolet(UV) spectroscopy, infrared spectroscopy, X-ray diffraction(XRD), scanning electron microscope(SEM), coordination analysis, elemental analysis and gravimetry. Results indicated that this synthesis procedure gave higher chelate rate of L-Hyp-Cu(Ⅱ), reaching 86.4%. The chelating reaction between copper(Ⅱ) and carboxyl and imino groups in L-Hyp to fomr L-Hyp-Cu(Ⅱ) with a coordination ratio of 1:2, whose molecular formula was established as Cu(C_5H_8NO_3)_2.
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