混合模式固相萃取-高效液相色谱法测定牛奶中4种非甾体抗炎药残留

引用本文: 丁健桦, 徐文平, 朱玉玲. 混合模式固相萃取-高效液相色谱法测定牛奶中4种非甾体抗炎药残留[J]. 分析化学, 2023, 51(6): 1013-1023. doi: 10.19756/j.issn.0253-3820.211239 shu

Citation: DING Jian-Hua, XU Wen-Ping, ZHU Yu-Ling. Mixed-mode Solid Phase Extraction Coupled with High Performance Liquid Chromatography for Analysis of Non-steroidal Anti-inflammatory Drugs Residues in Bovine Milk[J]. Chinese Journal of Analytical Chemistry, 2023, 51(6): 1013-1023. doi: 10.19756/j.issn.0253-3820.211239 shu

混合模式固相萃取-高效液相色谱法测定牛奶中4种非甾体抗炎药残留

东华理工大学化学与材料学院, 南昌 330013

通讯作者: 朱玉玲,E-mail:zyl9568@ecut.edu.cn

基金项目:
江西省科技厅重点研发计划项目(No.20192BBG7008)和东华理工大学博士科研启动基金项目(No.DHBK2019145)资助。

摘要: 制备了咪唑离子液体功能化的混合模式硅胶吸附剂（Sil-IL），将其作为固相萃取（SPE）吸附剂，结合高效液相色谱-紫外检测方法（HPLC-UV），建立了测定牛奶中酮洛芬、萘普生、吲哚美辛和托芬那酸4种非甾体类抗炎药物（NSAIDs）的分析方法。通过红外光谱、拉曼光谱和元素分析对Sil-IL进行了表征，初步探索了Sil-IL对目标物的保留作用机理，考察了样品溶液的pH值、上样流速、淋洗液及洗脱溶剂体积等因素对SPE效率的影响。结果表明，Sil-IL对4种NSAIDs的保留主要通过疏水作用和阴离子交换作用，Sil-IL吸附剂对4种NSAIDs具有较好的萃取选择性和萃取效率。在优化的SPE条件下，托芬那酸的线性检测范围为4~1000 μg/L，其它3种NSAIDs的线性范围为3~1000 μg/L，相关系数（R²）为0.9996~0.9998，检出限为1.2~1.9 μg/kg（S/N=3），日内和日间精密度分别为1.0%~3.0%和1.9%~6.3%，加标回收率为90.8%~105.3%。本方法准确可靠、灵敏度高、背景干扰低小、操作简便，可用于奶制品中4种NSAIDs残留的同时检测。

关键词:

English

Mixed-mode Solid Phase Extraction Coupled with High Performance Liquid Chromatography for Analysis of Non-steroidal Anti-inflammatory Drugs Residues in Bovine Milk

School of Chemistry and Material Science, East China University of Technology, Nanchang 330013, China

Corresponding author: ZHU Yu-Ling, zyl9568@ecut.edu.cn

Received Date: 21 March 2021
Revised Date: 29 May 2023
Fund Project:
Supported by the Department of Science and Technology of Jiangxi Province (No. 20192BBG7008) and the Doctoral Research Fund of East China University of Technology (No. DHBK2019145).

Abstract: A imidazolium ionic liquid-functionalized silica (Sil-IL) was synthesized and used as mixed-mode sorbent for solid phase extraction (SPE) of non-steroidal anti-inflammatory drugs (NSAIDs, naproxen, ketoprofen, indoometacin and tolfenamic acid) residues from bovine milk. A method combining this mixed-mode SPE and high performance liquid chromatography-ultraviolet detector (HPLC-UV) was established for simultaneous analysis of four kinds of NSAIDs residues in bovine milk. The prepared Sil-IL was characterized by Fourier transform infrared spectra, Raman spectra and elemental analysis. Then the retention mechanism of NSAIDs on Sil-IL sorbent was explored and the parameters affecting the extraction efficiency were optimized. Experimental results showed that Sil-IL had good extraction selectivity and high extraction efficiency towards four kinds of NSAIDs. Meanwhile, the interaction between Sil-IL and NSAIDs was mainly hydrophobic and anion exchange interactions. Under optimal SPE conditions, good sensitivity was achieved with a limit of detection of 1.2-1.9 μg/kg. The method displayed good linear relationship in the concentration range of 3-1000 μg/L for ketoprofen, naproxen, indomethacin and 4-1000 μg/L for tolfenamic acid, with the correlation coefficient (R²) of 09996-0.9998. The intra-day and inter-day precision were 1.0%-3.0% and 1.9%-6.3%, respectively. The recoveries of four kinds of NSAIDs in bovine milk at two spiked levels were 90.8%-105.3% with relative standard deviations less than 6.1%. The established method was proved to be accurate, reliable, simple, sensitive and selective, and could be used for determination of NSAIDs residues in milk sample.

Key words:

Ionic liquid
/ Nonsteroidal anti-inflammatory drugs
/ Solid phase extraction
/ High performance liquid chromatography
/ Bovine milk

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沈阳化工大学材料科学与工程学院沈阳 110142

混合模式固相萃取-高效液相色谱法测定牛奶中4种非甾体抗炎药残留

通讯作者: 朱玉玲,E-mail:zyl9568@ecut.edu.cn

English

Mixed-mode Solid Phase Extraction Coupled with High Performance Liquid Chromatography for Analysis of Non-steroidal Anti-inflammatory Drugs Residues in Bovine Milk

Corresponding author: ZHU Yu-Ling, zyl9568@ecut.edu.cn

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

混合模式固相萃取-高效液相色谱法测定牛奶中4种非甾体抗炎药残留

通讯作者: 朱玉玲,E-mail:zyl9568@ecut.edu.cn

English

Mixed-mode Solid Phase Extraction Coupled with High Performance Liquid Chromatography for Analysis of Non-steroidal Anti-inflammatory Drugs Residues in Bovine Milk

Corresponding author: ZHU Yu-Ling, zyl9568@ecut.edu.cn

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

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