Zhang Shibing, Wang Yiran, Yang Chunyu, Wang Xi, Wang Siyi, Yin Jiping, Du Yinan, Wu Di, Hu Jiangning, Zhao Qi
State Key Laboratory of Marine Food Processing and Safety Control, Dalian Polytechnic University, Dalian 116034, China.
National Engineering Research Center of Seafood, School of Food Science and Technology, Dalian Polytechnic University, Dalian 116034, China.
Foods. 2024 Aug 28;13(17):2736. doi: 10.3390/foods13172736.
In this study, amino-modified micro-mesoporous silica (NH-MMS) with hierarchical pores was prepared by modifying micro-mesoporous silica ZSM-5 with 3-aminopropyltriethoxysilane and used as an adsorbent in solid-phase extraction to analyze free fatty acids (FFAs) in krill oil during storage for an initial time. The Brunner Emmet Teller adsorption experiment and Fourier transform infrared spectroscopy demonstrate that NH-MMS, with a hierarchical pore structure, was successfully synthesized. The adsorption experiments, especially static adsorption, indicate that the absorption ability of the prepared NH-MMS, with a hierarchical pore structure, toward FFAs was better than that of traditional amino-modified mesoporous silica (SBA-15) with a mesoporous structure at all temperature and concentrations. Fairly low limits of detection (0.06-0.15 μg g), acceptable recoveries (85.16-94.31%), and precision (0.08-5.26%) were attained under ideal circumstances. Moreover, NH-MMS has the advantages of easy preparation and being environmentally friendly. As a result, this method offers an alternative to the current method for determining FFAs in different kinds of oil specimens.
在本研究中，通过用3-氨丙基三乙氧基硅烷修饰微孔-介孔二氧化硅ZSM-5制备了具有分级孔结构的氨基修饰微孔-介孔二氧化硅（NH-MMS），并首次将其用作固相萃取吸附剂来分析磷虾油储存期间的游离脂肪酸（FFA）。Brunner Emmet Teller吸附实验和傅里叶变换红外光谱表明成功合成了具有分级孔结构的NH-MMS。吸附实验，尤其是静态吸附实验表明，所制备的具有分级孔结构的NH-MMS在所有温度和浓度下对FFA的吸附能力均优于具有介孔结构的传统氨基修饰介孔二氧化硅（SBA-15）。在理想情况下，检测限相当低（0.06-0.15μg g），回收率可接受（85.16-94.31%），精密度良好（0.08-5.26%）。此外，NH-MMS具有制备简便且环保的优点。因此，该方法为目前测定不同种类油样中FFA的方法提供了一种替代方法。
