Musarurwa Herbert, Tavengwa Nikita Tawanda, Mokgehle Tebogo Mphatlalala, Madala Ntakadzeni Edwin, Selahle Shirley Kholofelo
Department of Chemistry Faculty of Science Engineering and Agriculture University of Venda Thohoyandou South Africa.
Department of Biochemistry Faculty of Science Engineering and Agriculture University of Venda University of Venda Thohoyandou South Africa.
Anal Sci Adv. 2025 Aug 19;6(2):e70039. doi: 10.1002/ansa.70039. eCollection 2025 Dec.
In response to an emerging need for the development of advanced analytical methods to guarantee food quality and safety, this study presents a novel medicine dropper-assisted SBME (MD-SBME) that was developed. The technique uses a meltdown layer of a facemask (MLF) as a holder of the extraction solvent. A hydrophobic natural deep eutectic solvent (NADES) made from thymol and menthol was used as the extraction solvent during the MD-SBME analysis of imidacloprid pesticide in fruit samples. Characterization of the NADES was done using Fourier-transform infrared spectroscopy (FT-IR), and the experimental results confirmed that it was successfully synthesized. The MD-SBME parameters, like ionic strength, sample pH, elution solvent type, elution solvent volume, type of DES and extraction solvent volume, were studied and optimized using both the univariate and multivariate approaches. The greenness of the MD-SBME technique was evaluated using the Complementary Modified Green Analytical Procedure Index (ComplexMoGapi) algorithm, and the total score was 85. A total score of 65 was obtained when the practicality of the MD-SBME procedure was evaluated using the blue applicability grade index (BAGI) metric tool. HPLC-PDA was used for the analysis of imidacloprid residues in fruit samples using the developed MD-SBME technique. Under the optimum conditions, limits of detection and quantification were in the range of 0.007-0.02 and 0.02-0.069 g, respectively. The correlation of determinations ( ) for pineapple, pear and apple samples were 0.9986, 0.9982 and 0.9973, respectively. The extraction recoveries of these fruit samples ranged from 72% to 110%. Good precision was obtained when the MD-SBME technique was used to analyse imidacloprid residues in real sample, as all the percentage relative standard deviation (%RSD) were below 5%.
为了满足开发先进分析方法以确保食品质量和安全这一新兴需求，本研究提出了一种新开发的医用滴管辅助单滴微萃取技术（MD - SBME）。该技术使用口罩的熔解层（MLF）作为萃取溶剂的载体。在水果样品中吡虫啉农药的MD - SBME分析过程中，使用由百里香酚和薄荷醇制成的疏水性天然深共熔溶剂（NADES）作为萃取溶剂。使用傅里叶变换红外光谱（FT - IR）对NADES进行了表征，实验结果证实其已成功合成。采用单变量和多变量方法对MD - SBME参数，如离子强度、样品pH值、洗脱溶剂类型、洗脱溶剂体积、深共熔溶剂类型和萃取溶剂体积进行了研究和优化。使用互补修正绿色分析程序指数（ComplexMoGapi）算法评估了MD - SBME技术的绿色度，总分为85分。使用蓝色适用性等级指数（BAGI）度量工具评估MD - SBME程序的实用性时，获得的总分为65分。使用所开发的MD - SBME技术，采用高效液相色谱 - 光电二极管阵列检测器（HPLC - PDA）对水果样品中的吡虫啉残留进行分析。在最佳条件下，检测限和定量限分别在0.007 - 0.02和0.02 - 0.069 μg范围内。菠萝、梨和苹果样品的测定相关系数（ ）分别为0.9986、0.9982和0.9973。这些水果样品的萃取回收率在72%至110%之间。当使用MD - SBME技术分析实际样品中的吡虫啉残留时，获得了良好的精密度，因为所有相对标准偏差百分比（%RSD）均低于5%。
