利用保留时间自动调整功能快速建立土壤中15种有机氯农药气相色谱-串联质谱检测方法

Determination of 15 kinds of organochlorine pesticide residues in soil by QuEChERS-gas chromatography-tandem mass spectrometry and automatic adjustment of retention time

目的通过保留时间自动调整(automatic adjustment of retentiontime,AART)功能快速简便建立土壤中有机氯的多级反应检测方法。方法土壤采用QuEChERS方法去除杂质,选择Rxi-5silMS色谱柱(30 m×0.25 mm, 0.25μm),柱箱采用程序升温模式,分流模式进样,分流比为20:1,柱流量为1.00 mL/min,以多反应监测(multiple reaction monitoring, MRM)扫描模式进行检测,内标法定量。结果 15种有机氯农药方法检出限(S/N=3)范围为1.5～11.0μg/kg之间;定量限(S/N=10)在5.0～36.7μg/kg之间; 3种水平土壤样品添加浓度回收率在66.50%～114.43%之间,相对标准偏差在1.25%～16.11%之间。结论利用AART功能创建的土壤中15种有机氯的多级反应检测方法满足实际检测要求,创建过程快速、简便,节约研究人员时间和精力,方法精密度和准确度均满足要求。

Objective To establish a method for the determination of 15 kinds of organochlorine pesticide residues in soil by QuEChERS-gas chromatography-tandem mass spectrometry and automatic adjustment of retention time(AART). Methods Soil was purified by QuEChERS. The gas was performed on Rxi-5sil MS (30 m×0.25 mm, 0.25 μm) with split mode (split ratio=20:1) and programmed temperature vaporization and column flow of 1.00mL/min. The sample was detected in multiple reaction monitoring (MRM) mode, and quantified by internal standard method. Results The limits of detection (S/N=3) were 1.5-11.0 μg/kg, and the limits of quantitation (S/N=10) were 5.0-36.7 μg/kg. The average recoveries were 66.50%-114.43%, with the relative standard deviations ranged from 1.25% to 16.11%. Conclusion The method is simple, rapid and reliable, which can be used for determination of 15 kinds of organochlorine pesticide residues in soil.