目的:基于优化的QuEChERS(Quick,Easy,Cheap,Effective,Rugged and Safe)法,建立气相色谱-串联质谱(Gas chromatography-tandem mass spectrometry,GC-MS/MS)测定茶叶中 10种拟除虫菊酿类农药残留的分析方法.方法:茶叶样品经2 mL饱和氯化钠水溶液浸泡后,乙腈提取.酰胺改性的聚苯乙烯、弗洛里硅土、Z-Sep+和多壁碳纳米管(Multi walled carbon nanotubes,MWCNTs)作为优化QuEChERS法的净化材料进行净化,GC-MS/MS分析测定,以茶叶基质空白溶液配制标准曲线,内标法定量.结果:净化材料的最佳用量为:酰胺改性的聚苯乙烯60 mg/mL,弗洛里硅土60 mg/mL,Z-Sep+60 mg/mL,MWCNTs 20 mg/mL.10种拟除虫菊酯类农药在0.01～0.20 mg/L范围内线性良好,相关系数为0.9964～0.9999.检出限为0.0002～0.004 mg/kg,定量限为0.0006～0.012 mg/kg.样品基质空白的3个不同浓度加标水平的平均回收率为95.6％～114.3％,相对标准偏差为0.2％～7.1％(n=5).结论:该方法灵敏、准确,可以满足茶叶中拟除虫菊酯类农药残留的快速定量分析.
Detection of Pyrethroid Pesticide Residues in Tea Based on Optimized QuEChERS Method
Objective:Based on optimized QuEChERS(Quick,Easy,Cheap,Effective,Rugged and Safe)method,the gas chromatography-tandem mass spectrometry(GC-MS/MS)analysis was established for the determination of 10 pyrethroid pesticide residues in tea.Method:After soaking in 2 mL of saturated sodium chloride aqueous solution,the prepared tea samples were extracted with acetonitrile.The amide modified polystyrene,florisil,Z-Sep+,and multi walled carbon nanotubes(MWCNTs)were uesd as purification agents of the optimized QuEChERS method for the purification,the GC-MS/MS analysis was used for determination,with standard curves prepared in blank tea matrix solution and quantified using internal standard method.Result:The optimal dosage of purification agents were 60 mg/mL of amide modified polystyrene,60 mg/mL of florisil,Z-Sep+at 60 mg/mL,and 20 mg/mL of MWCNTs.Good linearities were oberved for the 10 pyrethroid pesticide residues in the concentration range of 0.01-0.20 mg/L,with the correlation coefficients for the compounds were 0.9964-0.9999.The limits of detection and the limits of quantification were 0.0002-0.004 mg/kg and 0.0006-0.012 mg/kg,the average recoveries of three different spiked levels of the blank tea samples were 95.6％-114.3％,and the relative standard deviations were 0.2％-7.1％(n=5).Conclusion:This method is sensitive and accurate,which is suitable for the rapid quantitative analysis of pyrethroid pesticide residues in tea.
pyrethroid pesticidesoptimized QuEChERS(Quick,Easy,Cheap,Effective,Rugged and Safe)methodteagas chromatography-tandem mass spectrometry
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