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目的:建立分散液-液微萃取-气相色谱串联质谱法同时测定水中13种三唑类杀菌剂。方法:水样中加入50μl四氯化碳(萃取剂)和1.0 ml丙酮(分散剂),0.1 g氯化钠,分散混匀后,以5000 rpm/min离心5 min,吸取四氯化碳层进样,以气相色谱-串联质谱多反应监测(MRM)模式定量测定。结果:13种三唑类杀菌剂农药的富集倍数达81倍～785倍。在0.5μg/L～500μg/L范围内具有良好的线性关系,线性相关系数为0.9990～0.9999;回收率为72.0%～128.0%,相对标准偏差(RSD)为2.1%～6.6%,定量限为0.0015μg/L～0.25μg/L。结论:本法具有操作简单、富集效率高和灵敏度高等特点,可满足水样中13种三唑类杀菌剂农药残留同时检测要求。
OBJECTIVE: To establish a liquid - liquid microextraction - gas chromatography tandem mass spectrometry for the simultaneous determination of 13 triazole fungicides in water. Methods: Add 50 μl of carbon tetrachloride (extractant) and 1.0 ml of acetone (dispersant) and 0.1 g of sodium chloride into the water sample. After dispersing and mixing, centrifuge at 5000 rpm / min for 5 min and draw carbon tetrachloride Injection, quantitative determination by gas chromatography-tandem mass spectrometry multiple reaction monitoring (MRM) mode. Results: Thirteen kinds of triazole fungicides pesticide enrichment fold of 81 times to 785 times. The linear correlation coefficients ranged from 0.9990 to 0.9999. The recoveries ranged from 72.0% to 128.0% and the relative standard deviations (RSDs) ranged from 2.1% to 6.6%. The limits of quantitation 0.0015 μg / L to 0.25 μg / L. Conclusion: The method has the characteristics of simple operation, high enrichment efficiency and high sensitivity, which can meet the simultaneous detection of 13 pesticides residues in water samples.