| 摘要: |
| 结合快速-简单-低廉-有效-稳定-安全（QuEChERS）前处理方法和气相色谱-质谱法测定砂质土壤中的19种有机氯农药，采用标准质控样品优化提取时间和涡旋转速，比较不同溶剂、萃取盐和净化剂对19种有机氯农药回收效果的影响，并用新鲜砂质土壤进行方法的质量评估。结果表明，19种有机氯农药在0.5～10 mg/L质量浓度范围内相关性良好，在涡旋转速为2 000 r/min，提取时间为10 min，溶剂为正己烷/丙酮（V∶V=1∶1），萃取盐为氯化钠/无水硫酸镁（0.5 g+1.0 g），净化剂为C18-硫酸镁时，能有效回收19种有机氯农药。方法评估显示，19种有机氯农药在0.5，2.0和5.0 mg/kg的加标水平下平行实验的相对标准偏差（RSD）为4.5%～23.0%，各组分的平均回收率为68.5%～127.0%，各组分的检出限范围为0.02～0.08 mg/kg。该方法操作简单、成本低、溶剂消耗少且易于批量处理，适用于砂质土壤中19种有机氯农药的检测。 |
| 关键词: 快速-简单-低廉-有效-稳定-安全前处理方法 气相色谱-质谱法 有机氯农药 土壤 |
| DOI：DOI：10.3969/j.issn.1674-6732.2025.02.011 |
| 分类号:O657， X833 |
| 基金项目:四川省地质调査研究院科研项目（SDDY-Z2022020） |
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| Determination of 19 Organo-Chlorine Pesticides in Soil Using QuEChERS Combined with Gas Chromatography-Mass Spectrometry |
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LI Linling， XI Le， YU Ziheng， CHEN Zhongyi， LONG Zhen， GONG Li， YAO Xusong
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Sichuan Keyuan Testing Center of Engineering Technology Co. Ltd.， Key Laboratory of Investigation， Monitoring， Protection and Utilization for Cultivated Land Resources， Ministry of Natural Resources， Chengdu，Sichuan 611133， China
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| Abstract: |
| The determination methodology of 19 organochlorine pesticides（OCPs） in sandy soil was established by QuEChERS pretreatment method and gas chromatography-mass spectrometry（GC-MS）. The extraction time and vortex speed were optimized via standard QC soil samples. The influence of different solvents， extraction salts， and purification reagents on the recovery ratio of 19 OCPs was compared. The fresh sandy soil samples were used to validate the effectiveness of the established method. The results showed that 19 OCPs possess a good correlation in the concentration range of 0.5～10 mg/L. The 19 OCPs can be effectively recovered at the following conditions： vortex speed of 2 000 r/min， extraction time of 10 min， n-hexane/acetone（V∶V=1∶1） as solvent， NaCl/MgSO4（0.5 g+1 g） as extraction salt， and purification with C18-MgSO4. According to the quality assessment information， the RSD of parallel experiments were between 4.5% and 23.0% at the addition amount of 0.5， 2.0， and 5.0 mg/kg， the average recovery rates of each component ranged from 68.5% to 127.0%， and the limit of detection for each component were amongst 0.02 to 0.08 mg/kg. The proposed method is simple， cost-effective， and requires minimal solvent consumption， making it suitable for high-throughput analysis and the detection of 19 OCPs in sandy soil. |
| Key words: QuEChERS Gas chromatography tandem mass spectrometry Organochlorine pesticides Soil |
