Beiramzadeh Sarina, Farazjadeh Mir Ali, Fathi Ali Akbar, Afshar Mogaddam Mohammad Reza, Abolhasani Jafar
Department of Chemistry, Tabriz Branch, Islamic Azad University, Tabriz, Iran.
Pharmaceutical Analysis Research Center, Tabriz University of Medical Sciences, Tabriz, Iran.
Anal Methods. 2025 Jan 16;17(3):576-584. doi: 10.1039/d4ay01564a.
This study focuses on the dispersive solid phase extraction technique for the efficient extraction and enrichment of imidacloprid and acetamiprid from pepper samples. A synthesized sorbent was used for this purpose. Once the target analytes were adsorbed, the sorbent was separated using a centrifuge and the analytes were desorbed using a carbon dot solution. After centrifugation, a portion of the eluent was injected into a high-performance liquid chromatography-tandem mass spectrometry system for analysis of the analytes. Several parameters affecting the performance of the method were investigated, such as the amount of sorbent, the type and volume of elution solvent, pH, and so on. By optimizing these parameters, the method showed favorable results under the following conditions: a sample solution volume of 5 mL, a sorbent amount of 10 mg, vortexing for 2 min, 150 μL of carbon dot solution as the elution solvent, a pH of 10, and 3 min of agitation during the desorption step. Notably, this optimized method exhibited high extraction recoveries ranging from 67% to 78% as well as low detection limits (0.44 μg L and 0.32 μg L) and quantification limits (1.4 μg L and 1.0 μg L) for imidacloprid and acetamiprid, respectively. To validate the effectiveness of the method, four pepper samples were successfully analyzed and no analyte was detected in any of them using this approach. Overall, the developed DSPE method represents a reliable and sensitive technique for the extraction and analysis of the studied pesticides in pepper samples.
本研究聚焦于分散固相萃取技术,用于从辣椒样品中高效萃取和富集吡虫啉和啶虫脒。为此使用了一种合成吸附剂。一旦目标分析物被吸附,通过离心机分离吸附剂,并用碳点溶液解吸分析物。离心后,将一部分洗脱液注入高效液相色谱 - 串联质谱系统进行分析物分析。研究了影响该方法性能的几个参数,如吸附剂用量、洗脱溶剂的类型和体积、pH值等。通过优化这些参数,该方法在以下条件下显示出良好的结果:样品溶液体积为5 mL,吸附剂用量为10 mg,涡旋2 min,150 μL碳点溶液作为洗脱溶剂,pH值为10,解吸步骤中搅拌3 min。值得注意的是,这种优化方法对吡虫啉和啶虫脒分别表现出67%至78%的高萃取回收率以及低检测限(分别为0.44 μg/L和0.32 μg/L)和定量限(分别为1.4 μg/L和1.0 μg/L)。为验证该方法的有效性,成功分析了四个辣椒样品,采用此方法在任何样品中均未检测到分析物。总体而言,所开发的分散固相萃取方法是一种用于辣椒样品中所研究农药萃取和分析的可靠且灵敏的技术。