Analytical Unit of Residues and Contaminants, National Center for Animal and Plant Health (CENSA), San José de las Lajas, P.O. Box 10, 32700, Mayabeque, Cuba.
Agroscope Environmental Analytics, Reckenholzstrasse 191, 8046, Zurich, Switzerland.
Environ Sci Pollut Res Int. 2024 May;31(23):33623-33637. doi: 10.1007/s11356-024-33237-6. Epub 2024 Apr 30.
We present an analytical method to detect and quantify residues of currently used pesticides (CUPs), which include 31 active ingredients (ai) and seven transformation products (TPs) in tropical and agricultural soils of Cuba. Ten isotopically labeled analogous compounds served as internal standards (IL-IS). The novelty of this research is the inclusion of different tropical soils type scarcely studied for CUPs and TPs, based on the QuEChERS (quick, easy, cheap, effective, rugged and safe) method, followed by chromatography tandem mass spectrometry. All figures of merit proved to be satisfactory according to SANTE guidelines 2020 and 2021. Matrix effects (ME) calculated by the external standard method were significant (|ME| > 20% for almost all compounds; grand mean ± standard deviation (STD) 104 ± 108%) in all soils. The internal standard method compensated ME to non-significant levels (8 ± 50%), even for analytes with a non-structure identical IL-IS (STD, 13 ± 57%). Repeatability (relative standard deviation, RSD) and reproducibility (RSD) for skeletic regosol (SR) were 7.5 ± 2.8% and 11.7 ± 4.7%, respectively. Absolute (quantified for 11 analytes with structure identical IL-IS) and relative recovery from SR was 92 ± 13% (mean ± STD) and 90 ± 12%, respectively. Limits of quantification for SR ranged from 0.1 to 10 ng/g, except metalaxyl and oxyfluorfen (25 ng/g each). Linearity of matrix-matched (MM) calibration curves (5 to 100 ng/g) had an R of ≥ 0.99 for all soils and almost all analytes. The method was successfully applied to 30 real soil samples.
我们提出了一种分析方法，用于检测和定量古巴热带和农业土壤中目前使用的农药（CUPs）的残留，其中包括 31 种活性成分（ai）和 7 种转化产物（TPs）。十种同位素标记的类似化合物被用作内标（IL-IS）。本研究的新颖之处在于，根据 QuEChERS（快速、简单、廉价、有效、坚固和安全）方法，包括了不同的热带土壤类型，这些土壤类型很少被研究过 CUPs 和 TPs，随后进行了色谱串联质谱分析。所有的评价指标都根据 SANTE 指南 2020 和 2021 进行了验证，结果令人满意。通过外标法计算的基质效应（ME）在所有土壤中都非常显著（几乎所有化合物的|ME|>20%；总平均值±标准偏差（STD）为 104±108%）。内标法将 ME 补偿至非显著水平（8±50%），即使对于与非结构相同的内标物（STD，13±57%）也如此。骨架红壤（SR）的重复性（相对标准偏差，RSD）和再现性（RSD）分别为 7.5±2.8%和 11.7±4.7%。绝对回收率（用结构相同的内标物对 11 种分析物进行定量）和从 SR 中的相对回收率分别为 92±13%（平均值±STD）和 90±12%。SR 的定量限范围为 0.1 至 10ng/g，除了金属axyl 和氧氟草（各为 25ng/g）之外。所有土壤和几乎所有分析物的基质匹配（MM）校准曲线的线性相关系数（R）均≥0.99，范围为 5 至 100ng/g。该方法成功应用于 30 个实际土壤样品。
