Department of Biotechnology, Institute of Biology and Biotechnology, Collegium of Natural Sciences, University of Rzeszow, 1 Pigoń St., 35-310 Rzeszow, Poland.
Molecules. 2022 Mar 25;27(7):2140. doi: 10.3390/molecules27072140.
New analytical approaches to the simultaneous identification and quantification of 94 pesticides and 13 polycyclic aromatic hydrocarbons (PAHs) in five representative matrices (pepper, apple, lettuce, wheat, and soil) were developed. The analyses were based on gas chromatography coupled with triple quadrupole tandem mass spectrometry (GC-MS/MS). The procedure was optimized by changing the solvent used during the extraction, from acetonitrile to the acetone: -hexane mixture at a volume ratio of 1:4 (/), as well as the use of a reduced amount of water during the extraction of compounds from cereals. An additional modification was the use of florisil instead of GCB in the sample cleanup step. A full method validation study was performed, at two concentration levels (LOQ and 1000 × LOQ), which showed satisfactory results for all analytes from the PAHs group, with recoveries ranging from 70.7-115.1%, and an average RSD of 3.9%. Linearity was tested in the range of 0.001-1.000 mg/kg and showed coefficients of determination (R) ≥ 0.99 for all PAHs. Satisfactory recovery and precision parameters (LOQ and 100 × LOQ) were achieved for almost all analytes from the pesticide group in the range of 70.1-119.3% with the mean RSD equal to 5.9%. The observed linearity for all analytes in the concentration range of 0.005-1.44 mg/kg was R ≥ 0.99, with the exception of famoxadone, chizalofop-p-ethyl, prothioconazole, spirodiclofen, tefluthrin, and zoxamid. The extended uncertainties were estimated, using a top-down approach of 9.9% (average) and 15.3% (average) for PAHs and pesticides samples, respectively (the coverage factor k = 2, the 95% confidence level). Ultimately, the method was successfully applied to determine pesticide residues in commercial samples of fruit, vegetables and grain, and soil samples for PAHs, which were collected from selected places in the Podkarpacie region. A total of 38 real samples were tested, in which 10 pesticides and 13 PAHs were determined. Proposed changes allow us to shorten the sample preparation time (by 20%) and to reduce the consumption of organic solvents (by 17%). The use of florisil for sample cleanup, instead of GCB, improves the recovery of compounds with flat particles.
开发了一种新的分析方法，用于同时鉴定和定量五种代表性基质（辣椒、苹果、生菜、小麦和土壤）中的 94 种农药和 13 种多环芳烃（PAHs）。分析基于气相色谱-三重四极杆串联质谱联用（GC-MS/MS）。通过改变提取过程中使用的溶剂，从乙腈变为丙酮：正己烷体积比为 1:4（/），以及在从谷物中提取化合物时减少用水量，对该方法进行了优化。另一个改进是在样品净化步骤中使用弗罗里硅土代替 GCB。在两个浓度水平（LOQ 和 1000×LOQ）进行了全面的方法验证研究，结果表明 PAHs 组的所有分析物的回收率均令人满意，范围为 70.7-115.1%，平均 RSD 为 3.9%。在线性测试范围内为 0.001-1.000mg/kg，所有 PAHs 的决定系数（R）均≥0.99。在农药组中，几乎所有分析物在 LOQ 和 100×LOQ 的范围内的回收率和精密度参数（LOQ 和 100×LOQ）均达到 70.1-119.3%，平均 RSD 等于 5.9%。除了 famoxadone、chizalofop-p-ethyl、prothioconazole、spirodiclofen、tefluthrin 和 zoxamid 外，所有分析物在 0.005-1.44mg/kg 浓度范围内的观察线性 R≥0.99。使用自上而下的方法分别估算 PAHs 和农药样品的扩展不确定度，平均值分别为 9.9%（平均值）和 15.3%（平均值）（覆盖因子 k=2，95%置信水平）。最终，该方法成功应用于测定水果、蔬菜和谷物商业样品以及从喀尔巴阡地区选定地点采集的土壤样品中的农药残留。共测试了 38 个实际样品，其中确定了 10 种农药和 13 种 PAHs。所提出的更改允许我们缩短样品制备时间（缩短 20%）并减少有机溶剂的消耗（减少 17%）。使用弗罗里硅土代替 GCB 进行样品净化可提高具有扁平颗粒的化合物的回收率。
