基于优化QuEChERS法检测茶叶中拟除虫菊酯类农药残留  

Detection of Pyrethroid Pesticide Residues in Tea Based on Optimized QuEChERS Method

作　　者：刘佳 赵金利 谭锦萍 林泽珊 黄松 黄小清 王宇 王成龙 LIU Jia;ZHAO Jinli;TAN Jinping;LIN Zeshan;HUANG Song;HUANG Xiaoqing;WANG Yu;WANG Chenglong(Guangzhou Food Inspection Institute,Guangzhou 511400,China)

机构地区：[1]广州市食品检验所,广东广州511400

出　　处：《食品科技》2024年第3期335-344,共10页Food Science and Technology

基　　金：广州市市场监督管理局科技项目(2021KJ48)。

摘　　要：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种拟除虫菊酯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。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.

关 键 词：拟除虫菊酯类农药 优化QuEChERS法 茶叶 气相色谱-串联质谱 

分 类 号：TS207.53[轻工技术与工程—食品科学]