快速溶剂萃取-气相色谱-质谱法同时测定土壤中环丙唑醇、烯唑醇和戊唑醇  

Simultaneous determination of cyproconazole, diniconazole and tebuconazole in soil by rapid solvent extraction and gas chromatography–mass spectrometry

作　　者：沈荷美 陈土明 Shen Hemei;Chen Tuming(Zhejiang hangkang Testing Technology Co.,Ltd.,Hangzhou 310011,China)

机构地区：[1]浙江杭康检测技术有限公司,杭州310011

出　　处：《化学分析计量》2021年第5期61-64,共4页Chemical Analysis And Meterage

摘　　要：建立快速溶剂萃取–气相色谱–质谱法同时测定蔬菜种植基地土壤中环丙唑醇、烯唑醇和戊唑醇的分析方法。随机采集蔬菜种植基地土壤样品,风干,粉碎,过筛,置于加速溶剂萃取池中用乙腈提取,以丙酮–正己烷混合溶剂净化,净化液置于氮吹仪中吹至近干,用丙酮–正己烷溶液复溶,采用气相色谱–质谱法测定,内标法定量。环丙唑醇、烯唑醇和戊唑醇的质量浓度在0.04~4.0μg/mL范围内与色谱峰面积具有良好的线性关系,相关系数均大于0.995,检出限分别为0.006、0.008、0.013 mg/kg,定量限分别为0.019、0.026、0.040 mg/kg。环丙唑醇、烯唑醇和戊唑醇的平均加标回收率分别为92.3%~99.8%、91.8%~100.3%、96.4%~101.2%,测定结果的相对标准偏差分别为2.62%、2.69%、4.04%。该方法适用于批量土壤样品农药残留的监测。A method for simultaneous determination of cyproconazole,diniconazole and tebuconazole in soil of vegetable planting base by rapid solvent extraction and gas chromatography–mass spectrometry was established.The soil samples from vegetable planting base were collected randomly,dried,crushed and sieved.They were extracted with acetonitrile in accelerated solvent extraction pond and purified with acetone–n-hexane mixed solvent.The purified liquid was blown to near dryness in nitrogen blowing instrument and redissolved with acetone–n-hexane solution.The samples were determined by gas chromatography-mass spectrometry and quantified by internal standard method.The mass concentration of cyproconazole,diniconazole and tebuconazole had a good linear relationships with the chromatographic peak area in the range of 0.04–4.0 μg/mL,the correlation coefficients were all more than 0.995,the detection limits were 0.006,0.008,0.013 mg /kg,and the quantitation limits were 0.019,0.026,0.040 mg/kg,respectively.The average recoveries of of cyproconazole,diniconazole and tebuconazole were 92.3%–99.8%,91.8%–100.3%,96.4%–101.2%,respectively,and the relative standard deviations were 2.62%,2.69%,4.04%,respectively.The method is suitable for the monitoring of pesticide residues in batch soil samples.

关 键 词：快速溶剂萃取 气相色谱–质谱法 土壤 环丙唑醇 烯唑醇 戊唑醇 

分 类 号：O657.7[理学—分析化学]