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    韩文涛, 胡克娇, 赵婉凝, 李松卿, 陆鹏飞. 现场分散液液微萃取−气相色谱法检测水体中5种拟除虫菊酯类农药[J]. 北京林业大学学报, 2021, 43(9): 131-138. DOI: 10.12171/j.1000-1522.20210075
    引用本文: 韩文涛, 胡克娇, 赵婉凝, 李松卿, 陆鹏飞. 现场分散液液微萃取−气相色谱法检测水体中5种拟除虫菊酯类农药[J]. 北京林业大学学报, 2021, 43(9): 131-138. DOI: 10.12171/j.1000-1522.20210075
    Han Wentao, Hu Kejiao, Zhao Wanning, Li Songqing, Lu Pengfei. Determination of five pyrethroid pesticides in water using on-site DLLME-GC[J]. Journal of Beijing Forestry University, 2021, 43(9): 131-138. DOI: 10.12171/j.1000-1522.20210075
    Citation: Han Wentao, Hu Kejiao, Zhao Wanning, Li Songqing, Lu Pengfei. Determination of five pyrethroid pesticides in water using on-site DLLME-GC[J]. Journal of Beijing Forestry University, 2021, 43(9): 131-138. DOI: 10.12171/j.1000-1522.20210075

    现场分散液液微萃取−气相色谱法检测水体中5种拟除虫菊酯类农药

    Determination of five pyrethroid pesticides in water using on-site DLLME-GC

    • 摘要:
        目的  由于森林病虫害频发,大量化学农药用于病害虫防治。而农药残留进入水体造成了水资源的污染,因此,拟建立一种新颖的实现现场处理的样品前处理方法,对环境水体中的农药进行检测。
        方法  称量0.499 2 g柠檬酸、0.405 6 g磷酸二氢钠、0.218 4 g碳酸氢钠和0.180 0 g己酸钠,研磨混合均匀,使用压片机压制成泡腾片待用。将吸油棉裁卷为2 cm高度和60 mg/cm密度的圆柱体,填装入过滤柱,手动制成聚丙烯吸油棉过滤柱。将10 mL样品盛于注射器中,加入泡腾片,待完全反应后,经自制过滤柱过滤,200 μL乙腈洗脱,气相色谱-电子捕获检测器检测。
      最佳条件下,该方法在5 ~ 500 μg/L范围内,相关系数均大于0.999 0,具有良好的线性。按照3倍信噪比和10倍信噪比计算检出限和定量限,检测限为0.22 ~ 1.88 μg/L,定量限为0.75 ~ 6.25 μg/L。加标回收率在88.2% ~ 113.0%之间,相对标准偏差为4.5% ~ 11.8%,富集倍数在65 ~ 108之间。
        结论  本研究建立了一种基于可转换亲水性溶剂的泡腾片辅助现场分散液液微萃取−气相色谱法,检测了环境水样中的5种拟除虫菊酯类农药。该方法不需要使用用电设备,能够实现样品现场预处理,减少了人力物力的消耗,具有广阔的应用前景。

       

      Abstract:
        Objective  Due to the frequent occurrence of forest pests and diseases, a large number of chemical pesticides were used for pest control which enter the water and pollute the water resources. Therefore, it is planned to establish a novel sample pretreatment method for on-site processing to detect pesticides in environmental water bodies.
        Method  0.499 2 g of citric acid, 0.405 6 g of sodium dihydrogen phosphate, 0.218 4 g of sodium bicarbonate and 0.180 0 g of sodium caproate are weighed, ground and mixed evenly. The powder was compressed by a tablet machine into effervescent tablets for use. The polypropylene oil-absorbent cotton was cut into a cylinder with a height of 2 cm and a density of 60 mg/cm and packed into a filter column, and a novel homemade filter column was accomplished finally. The 10 mL sample was placed in a syringe and added with effervescent tablets. After the reaction was complete, it was filtered through a self-made filter column. After the filter column being eluted with 200 μL of acetonitrile, the filtrate was detected by gas chromatography-electron capture detector.
        Result  Under the optimal conditions, the linearity was in the concentration ranges of 5−500 μg/L, with coefficients greater than 0.999 0. The limit of detection and limit of quantification were calculated based on 3 times signal-to-noise ratio and 10 times signal-to-noise ratio. The limit of detection and the limit of quantitation were in the range of 0.22−1.88 μg/L and 0.75−6.25 μg/L. The recovery rate ranged between 88.2%−113.0%, the relative standard deviation was 0.8%−6.1%, and the enrichment factor was between 65−108.
        Conclusion  In this study, a new method named switchable hydrophilic solvent-based effervescent tablet assisted on-site dispersion liquid-liquid microextraction-gas chromatography was established to determine five pyrethroid pesticides in environmental waters. This method does not require the use of electrical equipment and can realize on-site pretreatment, which reduces the consumption of manpower and material resources and has broad application prospects.

       

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