Herein, we proposed a simple and efficient microwave-assisted preparation method for the fabrication of zirconium (IV) intercalated expanded graphite (Zr-EG). The synthetic approach could be completed in one step within 20 s, where KMnO 4 was used as the oxidizing agent, H 2 SO 4 and ZrOCl 2 as the intercalating agents. The as-prepared Zr-EG exhibited thin multi-layered structure, plenty of small Zr-relevant particles and oxygenated groups in both layers and surface, which gave Zr-EG high absorption capability. Subsequently, the Zr-EG, as a new kind of solid-phase extraction absorbent, was applied to the separation, purification and enrichment of chlorpyrifos in honey samples, followed by high-performance liquid chromatography analysis. Under optimal extraction and analysis conditions, the detection limit was 100 ng g −1 . The relative standard deviations ranged from 2.6 to 6.8%. At three spiked levels (1, 10, 100 μg g −1 ), the recoveries of chlorpyrifos were in the range of 86.1–92.2%. Comparison with other conventional solid-phase extraction adsorbents, modified EG showed rapid synthesis, layered modification flexibility, stable structure, large adsorption capacity and good selectivity, demonstrating great potential in pollutants separation and detection.

中文翻译：

---

微波辅助制备用于测定蜂蜜中毒死蜱的锆插层膨胀石墨

在此，我们提出了一种简单有效的微波辅助制备方法，用于制备锆 (IV) 插层膨胀石墨 (Zr-EG)。该合成方法可以在20秒内一步完成，其中KMnO 4 为氧化剂，H 2 SO 4 和ZrOCl 2 为插层剂。所制备的 Zr-EG 表现出薄的多层结构，在层和表面都有大量与 Zr 相关的小颗粒和含氧基团，这使 Zr-EG 具有高吸收能力。随后，Zr-EG作为一种新型固相萃取吸收剂，应用于蜂蜜样品中毒死蜱的分离、纯化和富集，并进行高效液相色谱分析。在最佳提取和分析条件下，检测限为100 ng g -1 。相对标准偏差范围为 2.6 至 6.8%。在三个加标水平（1、10、100 μg g -1 ）下，毒死蜱的回收率在 86.1-92.2% 的范围内。与其他传统固相萃取吸附剂相比，改性EG具有合成快速、分层改性灵活、结构稳定、吸附容量大、选择性好等特点，在污染物分离检测方面具有巨大潜力。