双官能团化介孔二氧化硅材料的合成及其在氨基糖苷类药物检测中的应用  

Synthesis of Bifunctionalized Mesoporous Silica and Its Application in the Detection of Aminoglycosides

作　　者：唐敏敏 邵雪梅 高巍[1] 宋锦柱[1] 朱晓军[1] 冯云[1] 邹洁[1] 许丹科 TANG Minmin;SHAO Xuemei;GAO Wei;SONG Jinzhu;ZHU Xiaojun;FENG Yun;ZOU Jie;XU Danke(Jiangsu Product Quality Testing and Inspection Institute,Nanjing 210000,China;State Key Laboratory of Analytical Chemistry for Life Science,School of Chemistry and Chemical Engineering,Nanjing University,Nanjing 210046,China;School of Public Health,Nanjing Medical University,Nanjing 211166,China)

机构地区：[1]江苏省产品质量监督检验研究院,江苏南京210000 [2]南京大学化学化工学院,生命分析化学国家重点实验室,江苏南京210046 [3]南京医科大学公共卫生学院,江苏南京211166

出　　处：《食品科学》2023年第18期372-380,共9页Food Science

基　　金：江苏省市场监督管理局科技计划项目(KJ207548)。

摘　　要：采用3-氨丙基三乙氧基硅烷、琥珀酸苷和十八烷基三甲氧基硅烷对MCM-41进行改性,合成了新型反相/阳离子交换混合模式的介孔二氧化硅吸附剂作为固相萃取(solid phase extraction,SPE)填料。优化SPE参数,使用氨基(Amide)色谱柱分离,建立牛奶中6种氨基糖苷类药物(aminoglycosides,AGs)残留的超高效液相色谱-串联质谱检测方法。对合成材料进行结构表征,结果说明合成材料具有大的比表面积,均匀的孔径和官能团修饰,对AGs表现出强大的吸附能力和选择性。与仅羧基化的材料相比,双官能团化的合成材料显著改善了牛奶样本的基质干扰。结果表明,6种AGs在5~500 ng/mL的质量浓度范围内线性关系良好(0.992 7~0.999 5),方法检出限为0.30~2.50 ng/mL,平均回收率为74.3%~107%,相对标准偏差为2.6%~15.7%。该材料成本低廉、制作简单,作为SPE填料可操作性强,今后可拓展应用至其他食品或农产品样本中AGs的检测。In this work,a novel reversed phase/cation exchange mixed-mode sorbent for solid phase extraction(SPE)was synthesized by modifying the mesoporous material MCM-41 with 3-aminopropyltriethoxysilane(APTES)and octadecyltrimethoxysilane(C_(18) TMS)followed by succinic acid glycoside(SAA)in two steps.Various SPE parameters were optimized,and an analytical method was developed for the determination of six aminoglycosides(AGs)in milk by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)using an amide column for chromatographic separation.The results of structural characterization demonstrated that the synthesized material had a large specific surface area,uniform pore size,and modified functional groups,exhibiting strong adsorption capacity and selectivity for AGs.The bifunctionalized material significantly improved matrix interference of milk compared to the carboxylated material.The proposed method exhibited good linearity for the six AGs in the concentration range of 5–500 ng/mL with correlation coefficients of 0.9927–0.9995.The limits of detection(LOD)achieved using this method were 0.30–2.50 ng/mL.The average recoveries ranged from 74.3%to 107%with relative standard deviation(RSD)between 2.6% and 15.7%.The material is characterized by low cost,simple preparation and good operability as a SPE filler.It can be extended to the detection of AGs in other food or agricultural samples.

关 键 词：介孔材料 MCM-41 固相萃取 氨基糖苷类 超高效液相色谱-串联质谱法 基质效应 牛奶 

分 类 号：TS207.3[轻工技术与工程—食品科学]