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GC-MS quantification of organophosphorous pesticides extracted from XAD-2 sorbent tube and foam patch matrices

机译:GC-MS量化从XAD-2吸附管和泡沫贴片基质中提取的有机磷农药

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This work presents a simple extraction procedure and a sensitive and simultaneous gas chromatography-mass spectrometry (GC-MS) method for quantifying five organophosphorous pesticides a€“ chlorpyrifos, dichlorvos, fenchlorphos, parathion-methyl and prothiofos a€“ currently used in flower and ornamental plant greenhouses, extracted from polyurethane foam dermal patches and sampling tubes packed with XAD-2 sorbent and quartz fiber filter. Analytical performance of the optimized method was evaluated taking into account specificity, selectivity, sensitivity, linearity, matrix effects, recovery and repeatability. Extraction procedures were made by addition of pure toluene to the spiked matrices, followed by gentle stirring or ultrasonic bath immersion. Analytes were eluted with a good resolution between 3.4 min and 13.1 min. Linearity responses were determined within the ranges of 25a€“550 ??g La?’1 for XAD-2 (R2 0.990) and 40a€“320 ??g La?’1 for PUF (R2 0.990). The ANOVA for linear regression (p 0.001), White test for homoscedasticity (p 0.05) and t-test for fitting parameters (p 0.001) indicated that the linear regression model provides a good interpolation of the experimental data. LOD and LOQ values were below 15.70 ?·g per sample and 47.56 ?·g per sample, respectively. Recoveries ranged from 81.17% to 114.48% with RSD 5%. The absence of significant matrix effects was statistically demonstrated by applying an F-test of equality of variances (p 0.05), and a two sample t-test assuming equal variances (p 0.05). The optimized method represents a useful tool for quantification of pesticides at low concentration levels for occupational matrices, allowing the future evaluation of occupational exposure from both inhaling and dermal routes.
机译:该工作提出了一种简单的提取方法和敏感的和同时的气相色谱 - 质谱(GC-MS)方法,用于量化五种有机磷农药A€“紫外线,二氯磷酸,福氯属,脱硫 - 甲基和普罗查菌A”,目前用于花和观赏植物温室,从聚氨酯泡沫皮肤贴片中提取,并用XAD-2吸附剂和石英纤维过滤器填充采样管。考虑特异性,选择性,灵敏度,线性,矩阵效应,恢复和重复性,评估了优化方法的分析性能。通过向尖刺基质中加入纯甲苯进行提取程序,然后温和搅拌或超声浴浸渍。分析物在3.4分钟和13.1分钟之间以良好的分辨率洗脱。对于XAD-2(R2> 0.990)和40A€“320→320→320?1的范围内测定线性响应,对于PUF(R2& 0.990)。用于线性回归的ANOVA(P <0.001),同性学性的白色测试(P&GT; 0.05)和用于拟合参数的T检验(P <0.001)表示线性回归模型提供了实验数据的良好插值。 LOD和LOQ值低于15.70?·G每样品,每样品47.56? RSD 5%的回收率范围为81.17%至114.48%。通过应用差异平等(P&GT; 0.05)的F检验,统计证明了没有显着的基质效应,以及假设等同差异的两个样品T检验(P&GT; 0.05)。优化的方法代表了用于职业矩阵低浓度水平的农药的有用工具,允许未来评估吸入和真皮途径的职业暴露。

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