色谱

色谱

• • 上一篇    下一篇

全自动在线固相萃取仪的研制及其在玉米中氨基甲酸酯类农药残留检测中的应用

李倩, 宁海静, 高岩, 陆家山, 姜晓琳, 崔爽, 吴琼, 丁坤*, 段春凤*   

  1. 中国科学院大连化学物理研究所, 辽宁 大连 116023
  • 收稿日期:2025-10-31
  • 通讯作者: *Tel:0411-84379590，E-mail：dingkun@dicp.ac.cn（丁坤）;Tel:0411-84379590，E-mail：cfduan@dicp.ac.cn（段春凤）.
  • 基金资助:
    国家自然科学基金项目（32170414）.

Development of a fully automatic online solid phase extraction instrument and its application in the determination of carbamate pesticide residues in corn

LI Qian, NING Haijing, GAO Yan, LU Jiashan, JIANG Xiaolin, CUI Shuang, WU Qiong, DING Kun*, DUAN Chunfeng*   

  1. Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China
  • Received:2025-10-31
  • Supported by:
    National Natural Science Foundation of China (No. 32170414).

PDF

6

摘要： 多维固相萃取-液相色谱分析技术是复杂样品中微量/痕量化合物定量分析的有力手段。国外已开发出全自动在线串联固相萃取仪，可实现多维固相萃取与液相色谱全自动、在线联用，极大地提高了分析效率。国内在这一技术领域研究较少，所使用的全自动在线固相萃取仪器大多为进口产品，价格高昂，限制了国内在相关领域的应用研究。本文研制了一种全自动在线串联固相萃取仪器，采用托盘携带萃取小柱运动，替代国外同类产品使用的机械手系统，通过3对双面密封高压压头和流程设计，实现串联固相萃取的全自动化及其与高效液相色谱系统的在线联用。系统考察了固相萃取小柱的耐压性能和使用寿命，结果表明制备的固相萃取小柱耐压≥30 MPa，使用寿命≥10次。将仪器应用于玉米中氨基甲酸酯类农药残留的在线串联固相萃取-高效液相色谱分析，单个样品前处理时间仅需15 min，大幅提高了分析效率。该仪器实现了多维固相萃取-在线洗脱-色谱进样-分离检测一体化，工作模式灵活，可以自由组合不同萃取小柱和柱上衍生，适配不同的应用场景，具有较好的实际应用潜力。

关键词: 在线串联固相萃取, 样品前处理, 高效液相色谱, 农药残留

Abstract: Multidimensional solid phase extraction (SPE) coupled with liquid chromatography (LC) is a powerful technique for the quantitative analysis of micro or trace-levels compounds in complex samples. Fully automated online tandem SPE instruments have been developed in other countries, enabling fully automated online coupling of multidimensional SPE with LC and significantly improving analytical efficiency. Domestic research in this area remains limited. Most fully automated online SPE instruments used are imported at high cost, which restricts application-oriented research in related fields in China. This paper presents the development of a fully automated online tandem SPE instrument. It employs a tray-based system to transport extraction cartridges, replacing a robotic arm system used in similar foreign products. Through the design of three pairs of double-sealed high-pressure heads and the corresponding workflow, the instrument enables fully automated tandem SPE and its online integration with a high performance liquid chromatography (HPLC) system. The pressure resistance and lifetime of the SPE cartridges were systematically evaluated. Results showed that the prepared cartridges exhibited a pressure resistance of ≥30 MPa and a service life of ≥10 cycles. The instrument was applied to detect carbamate pesticide residues in corn by online tandem SPE-HPLC method. Sample preparation time was only 15 min per sample, significantly improving analytical efficiency. The instrument integrates multidimensional SPE, online elution, chromatographic injection, separation and detection. Its flexible operational mode allows for the free combination of different extraction cartridges and the integration of on-column derivatization. It is adaptable to various application scenarios and demonstrates great application potential.

Key words: online tandem solid phase extraction, sample pretreatment, high performance liquid chromatography(HPLC), pesticide residues

中图分类号: