Nuclear and Energy Research Institute, São Paulo 05508-000, Brazil.
Applied Mass Spectrometry Center (CEMSA), São Paulo 05508-000, Brazil.
Int J Environ Res Public Health. 2020 Aug 5;17(16):5666. doi: 10.3390/ijerph17165666.
Technological advances have promoted improvements in several science fields, especially related to environmental and analytical areas with the improvement of detection and development of environmentally friendly extraction techniques. This study applied Quick, Easy, Cheap, Effective, Rugged and Safe method (QuEChERS) for soil extraction and assessed its performance through a validation study using samples from the soil of a contaminated area in Caieiras, SP, Brazil. Nine organochlorine pesticides, including the isomers alpha, beta, gamma and delta- hexachlorocyclohexane; and -heptachlor epoxide; and -chlordane and heptachlor were analyzed by gas chromatography coupled to electron capture detector. The method was validated according to ISO 5725-4 (2020), EURACHEM (2014) and DOQ-CGCRE-008 (2016). The limits of detection and quantification of the method for the nine organochlorines were α-HCH (1.2 and 12.6 µg kg), β-HCH (1.7 and 12.0 µg kg), γ-HCH (1.5 and 11.6 µg kg), δ-HCH (0.8 and 11.6 µg kg), heptachlor (1.0 and 10.8 µg kg), -heptachlor epoxide (0.9 and 11.5 µg kg), heptachlor epoxide (0.9 and 11.5 µg kg), -chlordane (0.4 and 7.9 µg kg) and chlordane (0.5 and 10.9 µg kg), respectively, and all of them were within the maximum limits recommended by the EPA for the compounds α-HCH (86.0 and 360.0 µg kg), β-HCH (300.0 and 1.3 × 10 µg kg), γ-HCH (570.0 and 2.5 × 10 µg kg), δ-HCH (not defined), heptachlor (130.0 and 630.0 µg kg), heptachlor epoxide (7.0 and 330.0 µg kg), -chlordane (1.77 × 10 and 7.7 × 10 µg kg) in residential and industrial soil, respectively. Recovery results were between 65% and 105% for almost all compounds, which is an optimum result for multi-residue analytical methods, considering the complexity of the matrix used in the study. Caieiras presented contamination levels of α-HCH in the range of 2.0 to 66.0 µg g, which was higher than the limits established by EPA, corresponding to 0.077 µg g for residential soil and 0.27 µg g for industrial soil. According to the validation study, the analytical method proposed was reliable for organochlorine quantification, and the QuEChERS was considered efficient for organochlorine extraction from soil.
技术进步促进了几个科学领域的改进，特别是与环境和分析领域相关的领域，因为检测和开发了更环保的提取技术。本研究应用快速、简单、廉价、有效、坚固和安全方法（QuEChERS）进行土壤提取，并通过使用巴西 Caieiras 污染地区土壤样本的验证研究评估其性能。分析了九种有机氯农药，包括异构体α、β、γ和δ-六氯环己烷；和 -七氯环氧化物；和 -氯丹和七氯。使用气相色谱法结合电子俘获检测器进行分析。该方法按照 ISO 5725-4（2020）、EURACHEM（2014）和 DOQ-CGCRE-008（2016）进行了验证。该方法对九种有机氯农药的检测限和定量限分别为α-HCH（1.2 和 12.6 µg kg）、β-HCH（1.7 和 12.0 µg kg）、γ-HCH（1.5 和 11.6 µg kg）、δ-HCH（0.8 和 11.6 µg kg）、七氯（1.0 和 10.8 µg kg）、-七氯环氧化物（0.9 和 11.5 µg kg）、-七氯环氧化物（0.9 和 11.5 µg kg）、-氯丹（0.4 和 7.9 µg kg）和氯丹（0.5 和 10.9 µg kg），所有这些均在 EPA 对 α-HCH（86.0 和 360.0 µg kg）、β-HCH（300.0 和 1.3 × 10 µg kg）、γ-HCH（570.0 和 2.5 × 10 µg kg）的化合物推荐的最大限量内δ-HCH（未定义）、七氯（130.0 和 630.0 µg kg）、-七氯环氧化物（7.0 和 330.0 µg kg）、-氯丹（1.77 × 10 和 7.7 × 10 µg kg），用于住宅和工业土壤。几乎所有化合物的回收率均在 65%至 105%之间，这是多残留分析方法的最佳结果，考虑到研究中使用的基质的复杂性。Caieiras 的α-HCH 污染水平在 2.0 至 66.0 µg g 之间，高于 EPA 设定的限值，分别对应于住宅土壤 0.077 µg g 和工业土壤 0.27 µg g。根据验证研究，所提出的分析方法可可靠地用于有机氯的定量，而 QuEChERS 被认为是从土壤中提取有机氯的有效方法。
