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首页> 外文期刊>American Journal of Analytical Chemistry >Optimization of Solid Phase Microextraction Procedure Followed by Gas Chromatography with Electron Capture Detector for Pesticides Butachlor and Chlorpyrifos
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Optimization of Solid Phase Microextraction Procedure Followed by Gas Chromatography with Electron Capture Detector for Pesticides Butachlor and Chlorpyrifos

机译：固相微萃取程序的优化，然后采用气相色谱-电子捕获检测器测定农药丁草胺和毒死est

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摘要

In this study, headspace solid phase microextraction (HS-SPME) followed by gas chromatography using electron capture detection system (GC-ECD) were developed for the determination of chloraacetanilide (butachlor) and chlorpyrifos presented in biological samples. Different parameters affecting the extraction procedure were optimized including extraction time (30 minutes), extraction temperature (80°C), sample volume (3 mL), sample pH (2), added NaCl (0.3 gram) and sample stirring rate (400 rpm). Different concentrations of 1 - 100 ng/ml were applied for butachlor and a linear calibration curve was obtained. Furthermore, a similar linearity was obtained for chlorpyrifos, using a concentration range of 1 - 250 ng/ml. The limit of detection (LOD) obtained for butachlor and chlorpyrifos were 0.088 and 0.53 ng/ml respectively. The optimized methods for both compounds were validated using two concentrations of 25 and 50 ng/ml in spiked urine samples. Obtained recoveries of spiked urine samples were 83.06% - 99.8% with RSD of lower than 11%. Optimized technique was simple, inexpensive, solvent free and fast in comparison with other conventional methods and had compatibility with the chromatographic analytical system. This method offers low detection limits to analyze pesticides in urine samples that are very important in the exposure monitoring in occupational health.
机译：在这项研究中，开发了顶空固相微萃取（HS-SPME），然后使用电子捕获检测系统（GC-ECD）进行气相色谱法，用于测定生物样品中存在的氯乙酰苯胺（丁草胺）和毒死rif。优化了影响萃取程序的不同参数，包括萃取时间（30分钟），萃取温度（80°C），样品量（3 mL），样品pH（2），添加的NaCl（0.3克）和样品搅拌速率（400 rpm） ）。将不同浓度的1-100 ng / ml用于丁草胺，并获得线性校准曲线。此外，使用毒死obtained的浓度范围为1-250 ng / ml，获得了相似的线性。丁草胺和毒死rif的检出限（LOD）分别为0.088和0.53 ng / ml。在加标尿液样品中使用两种浓度分别为25和50 ng / ml的化合物对两种化合物的优化方法进行了验证。加标尿液样品的回收率为83.06％-99.8％，RSD低于11％。与其他常规方法相比，优化技术简单，便宜，无溶剂且速度快，并且与色谱分析系统兼容。该方法检测尿样中的农药的检测限较低，这在职业健康中的暴露监测中非常重要。

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