在线净化-气相色谱法测定土壤中有机磷农药
Determination of Organophosphate Residues in Soil Using On-line Purification and Gas Chromatography with a Nitrogen-Phosphorus Detector
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摘要: 建立了一套利用加速溶剂萃取仪在线净化,气相色谱氮磷检测器测定土壤中20种有机磷农药的方法。考察了加速溶剂萃取仪的萃取温度、氧化铝的类型和加入方式、溶剂萃取体系、分散剂用量等因素对土壤中有机磷农药残留测定的影响。合适的萃取温度在萃取效率和回收效率之间找到最佳平衡点,酸性氧化铝和底部加入方式保证了土壤的净化效果和有机磷的回收率,分散剂的加入使得土壤中有机磷分布更加均匀。以酸性氧化铝和石墨碳黑为净化剂,水为分散剂,土壤样品经加速溶剂萃取仪在线净化萃取,浓缩后采用气相色谱氮磷检测器检测。在萃取温度为60℃,酸性氧化铝底部加入,分散剂水为1.0 mL的条件下,20种有机磷的检出限为0.005~0.014 mg/L。本方法将萃取过程与净化过程合二为一,简化了操作步骤,提高了工作效率。Abstract: A method based on on-line purification using Accelerated Solvent Extraction (ASE) and Gas Chromatography with a Nitrogen-Phosphorus Detector has been developed to determine 20 kinds of organophosphate pesticide residues in soil samples. The temperature for solvent extraction, the type and addition method of alumina, solvent extraction system and the dosage of dispersant were studied for the determination of organophosphate pesticide in soil samples. The selected optimal extraction temperature was based on extraction efficiency and recovery efficiency. Adding acidic alumina at the bottom of the bottle could ensure the purify effect of the soil and the recovery of organophosphate. Adding the dispersant to the soil made organophosphate distribution in the soil more uniform. When the purificants were acidic alumina and graphite carbon, the temperature was 60℃, acid-alumina was added at the bottom and the volume of dispersant water was 1.0 mL, the detection limits of 20 kinds of organophosphate pesticide were 0.005-0.014 mg/L. The operation procedure was simplified and work efficiency was improved by combined processes of extraction and purification.
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Key words:
- soil /
- organophosphate /
- on-line /
- purification
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