Kapsi Margarita, Sakkas Vasileios, Boti Vasiliki, Albanis Triantafyllos
Laboratory of Industrial Chemistry, Department of Chemistry, University of Ioannina, 45110 Ioannina, Greece.
Institute of Oceanography, Hellenic Centre for Marine Research, 70014 Gournes, Greece.
Molecules. 2025 May 7;30(9):2076. doi: 10.3390/molecules30092076.
In this study, C18-functionalized magnetic silica nanoparticles (FeO@SiO@C18) were used as adsorbents for the magnetic solid-phase extraction (MSPE) of organic contaminants commonly applied to aquaculture water (organic booster biocides, herbicides, and insecticides) followed by Gas Chromatography coupled to Mass Spectrometry (GC-MS). The extraction conditions and efficiency of the nanoparticles for the determination of ten pesticides (atrazine, ethoxyquine, chlorothalonil, chlorpyriphos methyl, methyl parathion, chlorpyriphos, resmethrin, λ-cyhalothrin, permethrin, and irgarol) were thoroughly investigated. Several experimental parameters affecting the extraction efficiency such as the amount of sorbent, extraction time, and elution time were optimized by employing experimental designs as response surface methodology. Validation experiments showed that the average recoveries of target analytes were in the range of 60% to 99%. The optimized method exhibited good linearity (R > 0.9901) and satisfactory precision (Relative Standard deviations, RSDs < 15%). The method detection limits ranged between 1.9 ng L and 62 ng L. Finally, the MSPE method was successfully applied to aquaculture water samples collected from the Thesprotia region (N.W. Greece), Thermaikos Gulf (N. Greece) and Butrint (S.W. Albania).
在本研究中，C18功能化磁性二氧化硅纳米颗粒（FeO@SiO@C18）被用作吸附剂，用于对水产养殖用水中常用的有机污染物（有机增效杀生剂、除草剂和杀虫剂）进行磁性固相萃取（MSPE），随后采用气相色谱-质谱联用（GC-MS）分析。对纳米颗粒测定十种农药（阿特拉津、乙氧喹啉、百菌清、甲基毒死蜱、甲基对硫磷、毒死蜱、炔丙菊酯、高效氯氟氰菊酯、氯菊酯和藻菌清）的萃取条件和效率进行了深入研究。通过采用响应面法等实验设计，对影响萃取效率的几个实验参数，如吸附剂用量、萃取时间和洗脱时间进行了优化。验证实验表明，目标分析物的平均回收率在60%至99%之间。优化后的方法具有良好的线性（R>0.9901）和令人满意的精密度（相对标准偏差，RSDs<15%）。方法检测限在1.9 ng/L至62 ng/L之间。最后，MSPE方法成功应用于从希腊西北部的色萨利地区、希腊北部的塞尔迈湾和阿尔巴尼亚西南部的布特林特采集的水产养殖水样。
