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双亲性去磷脂填料的制备及其在兽残检测中的应用OA

Preparation of Amphiphilic Phospholipid Removal Fillers and the Application in Animal Residue Detection

中文摘要英文摘要

针对复杂食品基质中兽残检测困难、磷脂去除难的问题,通过在硅胶表面修饰十八烷基三氯硅烷(Octadecyltrichlo-rosilane.OTS),制备了一种双亲性的去磷脂材料(Phospholipid removal material,PPR).通过 FT-IR、SEM、N2 吸附-脱附仪等对材料进行表征,证明PPR填料的成功制备.基于PPR填料的固相萃取与液相色谱-质谱/质谱(HPLC-MS/MS)联用技术,建立了一种能快速净化食品基质磷脂并检测食品中19种兽残的分析方法.结果表明,制备的PPR填料对鸡蛋、全脂牛奶、鸡肉、猪肉这4种食品基质的磷脂净化率为98.58%~99.91%,相对标准偏差3.9%~5.6%,PRiME HLB的磷脂去除率为94.09%~99.64%,相对标准偏差2.8%~5.9%;在19种β-受体激动剂和喹诺酮类兽残加标实验中,PPR填料对鸡蛋的兽残加标回收率为81.0%~102.3%,相对标准偏差1.4%~8.2%,PRiME HLB的兽残加标回收率为80.5%~104.3%,相对标准偏差3.1%~9.4%.PPR填料的磷脂净化率及兽残加标回收率与市售进口产品性能相当,且具有制备简便、成本低、磷脂净化效率高等特点,在食品安全检测领域具有广泛应用前景.

To address the analytical challenges in veterinary drug residue detection in complex food matrices,particularly the interference from phospholipid that can affect detection accuracy and instrument performance,a novel amphiphilic phospholipid removal material(PPR)was developed.The PPR material was prepared by surface modification of octadecyltrichlorosilane(OTS)on silica gel,providing both hydrophobic and hydrophilic properties.The successful fabrication of the PPR material was confirmed using fourier-transform infrared spectroscopy(FT-IR)for functional group identification,scanning electron microscopy(SEM)for morphological analysis,and nitrogen adsorption-desorption measurements for surface area and pore structure evaluation.A reliable analytical methodology was subsequently established by integrating the PPR filler based solid-phase extraction(SPE)with high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS),enabling rapid purification of phospholipids from food matrices and simultaneous detection of 19 veterinary drug residues.The results showed that the prepared PPR filler had a phospholipid purification rate of 98.58%~99.91%,with a relative standard deviation of 3.9%~5.6%for four food matrices:eggs,whole milk,chicken,and pork.The phospholipid removal rate of PRiME HLB was 94.09%~99.64%,with a relative standard deviation of 2.8%~5.9%;In the animal residue spiked experiments of 19 types of β-receptor agonists and quinolones,the recovery rate of PPR fillers for animal residues in eggs was 81.0%~102.3%,with a relative standard deviation of 1.4%~8.2%.The recovery rate of PRiME HLB for animal residues was 80.5%~104.3%,with a relative standard deviation of 3.1%~9.4%.The phospholipid removal efficiency and residue recovery of PPR fillers are comparable to the performance of commercially available imported products.PPR fillers have the characteristics of simple preparation,good stability,low cost,high phospholipid purification efficiency,indicating potential for widespread application in food safety testing.

徐晨;王明;陈武炼

上海安谱实验科技股份有限公司,上海 200000上海安谱实验科技股份有限公司,上海 200000上海安谱实验科技股份有限公司,上海 200000

化学化工

兽残磷脂固相萃取喹诺酮受体激动剂

beast remnantsphospholipidssolid phase extractionquinolonereceptor agonist

《化学试剂》 2026 (3)

19-26,8

上海市松江区产业化关键或共性技术项目(2021-13)上海市专业技术服务平台项目(21DZ2292900)长三角G60科创走廊青年创新英才项目(2022).

10.13822/j.cnki.hxsj.2025.0293

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