[Case-based teaching with both positive and negative examples in undergraduate analytical chemistry laboratory: determination of six nitrogen-containing pesticides in environmental samples by solid-phase microextraction-high performance liquid chromatography].

Jie Zhang, Xin-Zhong Zhang, Zhen Zhang, Jing-Wei Liu, Xue-Mei Wang
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Abstract

In analytical chemistry, separation and enrichment steps serve not only as critical stages in the analytical workflow, but also as core technologies that determine the accuracy, reliability, and applicability of analytical methods. However, in conventional experimental instruction, this step is frequently overlooked owing to time constraints and an overemphasis on instrumental techniques, leading to fragmented knowledge structures and hindering the development of integrated analytical thinking that connects theory with practice. To address this issue, this study, based on the "knowledge-ability-practice" three-dimensional integrated teaching objective, innovatively establishes a "positive-negative case-based teaching" model, using the solid-phase microextraction (SPME) of six nitrogen-containing pesticides from environmental water samples as the instructional case. By comparing fibers coated with non-polar polydimethylsiloxane (PDMS) and strongly polar polyacrylate (PA), and employing high performance liquid chromatography with ultraviolet detection (HPLC-UV), this study systematically investigates the matching relationship between analyte polarity and coating properties. In the positive case, the PDMS coating demonstrates superior extraction performance for weakly polar pesticides based on the "like dissolves like" principle, with a linear coefficient of determination R2≥0.993 7 and detection limits ranging from 0.019 to 0.17 μg/L. In contrast, in the negative case, the PA coating shows weaker extraction efficiency due to differences in the extraction mechanism, yielding detection limits between 0.066 to 1.069 μg/L. Based on spiked recovery tests conducted on actual river water samples from Lanzhou (recoveries: 81.5% to 117%), a multi-dimensional evaluation system of "knowledge internalization, competency enhancement, and practical literacy" is established accordingly. Teaching feedback demonstrates that the students show a marked improvement in their understanding of the core principles, and their innovative thinking and problem-solving skills are effectively cultivated. The "contrasting-case-based" pedagogical approach effectively bridges theory and experiment while stimulating students' investigative thinking. The study provides a replicable and scalable practical model for the reform of analytical chemistry experimental teaching, which holds significant value in cultivating high-caliber talents with rational method selection and problem-solving abilities.

[本科分析化学实验室正反例教学:固相微萃取-高效液相色谱法测定环境样品中6种含氮农药]。
在分析化学中,分离和富集步骤不仅是分析工作流程中的关键阶段,而且是决定分析方法准确性、可靠性和适用性的核心技术。然而,在传统的实验教学中,由于时间限制和过分强调仪器技术,这一步经常被忽视,导致知识结构碎片化,阻碍了将理论与实践联系起来的综合分析思维的发展。针对这一问题,本研究基于“知识-能力-实践”的三维一体化教学目标,以环境水样中六种含氮农药固相微萃取(SPME)为教学案例,创新性地建立了“正-负案例教学法”模式。通过比较非极性聚二甲基硅氧烷(PDMS)和强极性聚丙烯酸酯(PA)涂层的纤维,并采用高效液相色谱-紫外检测(HPLC-UV),系统地研究了分析物极性与涂层性能之间的匹配关系。在阳性情况下,PDMS涂层对弱极性农药具有较好的提取效果,基于“相似溶解相似”原理,线性系数R2≥0.993 7,检出限范围为0.019 ~ 0.17 μg/L。相反,在阴性情况下,由于提取机理的不同,PA涂层的提取效率较弱,检出限在0.066 ~ 1.069 μg/L之间。通过对兰州市实际河流水样进行加标回收率试验(回收率为81.5% ~ 117%),建立了“知识内化、能力提升、实践素养”的多维评价体系。教学反馈表明,学生对核心原理的理解有明显提高,创新思维和解决问题的能力得到有效培养。“案例对比教学法”有效衔接理论与实验,激发学生的探究性思维。本研究为分析化学实验教学改革提供了可复制、可扩展的实践模式,对培养具有合理选择方法和解决问题能力的高素质人才具有重要价值。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
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