Abstract Two new sensitive and selective methods were developed to quantify thirteen pesticides in soil and water. The method developed in soil was optimized and modified based on the Quick, Easy, Cheap, Effective, Rugged, and Safe (QuECHERS) procedure, followed by a dispersive solid phase extraction (dSPE) clean-up technique. The method developed in the water samples was based on glass fiber and nylon filtration, followed by the solid phase extraction (SPE) clean-up technique. Both methods used ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS) for analysis. The developed method showed good linearity at calibration points ranging from the instrumental quantification limit (IQL) to 500 ng mL−1, and the correlation coefficients (R2) for all of the target analytes were higher than 0.9990. The method showed recoveries ranging from 74% to 111% in soil and 77% to 117% in water. The method detection limit (MDL) for all of the target analytes ranged from 0.03 ng g−1 to 0.4 ng g−1 in soil and 0.1 ng L−1 to 10 ng L−1 in water. Both methods were applied to field paddy soil and water samples to quantify pesticide residues in the samples. Isoprothiolane was the highest concentration pesticide in paddy soil (34.81 ng g−1), whereas chlorantraniliprole (11.83 ng mL−1) was the highest concentration pesticide in the paddy water sample. Based on the instrument and method performance validation results, the developed methods can be applied as part of pesticide residue analysis in environmental and agricultural matrices, thus aiding in regulating and monitoring pesticide usage in agricultural fields.

中文翻译：

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改进的 QuEChERS 和固相萃取用于使用超高效液相色谱串联质谱法对稻田土壤和水中的农药进行多残留分析

摘要 开发了两种新的灵敏和选择性方法来定量土壤和水中的 13 种农药。在土壤中开发的方法基于快速、简单、廉价、有效、坚固和安全 (QuECHERS) 程序进行了优化和修改，然后是分散固相萃取 (dSPE) 净化技术。在水样中开发的方法基于玻璃纤维和尼龙过滤，然后是固相萃取 (SPE) 净化技术。两种方法均使用超高效液相色谱联用串联质谱 (UHPLC-MS/MS) 进行分析。开发的方法在从仪器定量限 (IQL) 到 500 ng mL-1 的校准点显示出良好的线性，并且所有目标分析物的相关系数 (R2) 均高于 0.9990。该方法在土壤中的回收率为 74% 至 111%，在水中的回收率为 77% 至 117%。所有目标分析物的方法检测限 (MDL) 范围为土壤中的 0.03 ng g-1 至 0.4 ng g-1 和水中的 0.1 ng L-1 至 10 ng L-1。两种方法均应用于田间稻田土壤和水样以量化样品中的农药残留。Isoprothiolane 是稻田土壤中浓度最高的农药 (34.81 ng g-1)，而氯虫苯甲酰胺 (11.83 ng mL-1) 是稻田水样中浓度最高的农药。基于仪器和方法性能验证结果，开发的方法可以作为环境和农业基质中农药残留分析的一部分，从而有助于规范和监测农业领域的农药使用。