QuEChERS方法结合超高效液相色谱-串联质谱法测定木槿花中77种农药的残留量  

Determination of 77 Pesticide Residues in Hibiscus syriacus L.Flowers by QuEChERS Method Coupled with Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：黄承远 HUANG Chengyuan(Fujian Agricultural Product Quality and Safety Inspection and Testing Center,Fuzhou 350003,China)

机构地区：[1]福建省农产品质量安全检验检测中心,福建福州350003

出　　处：《现代食品》2025年第3期210-221,共12页Modern Food

摘　　要：本文建立QuEChERS前处理结合超高效液相色谱-串联质谱法同时测定木槿花鲜样和干样中77种农药残留的方法。样品经粉碎后,使用乙腈进行提取,干样加水后再提取。提取液经乙二胺-N-丙基硅烷化硅胶(PSA)与石墨化炭黑(Graphitized Carbon Black,GCB)分散固相萃取净化,外标法定量。结果显示,77种农药在0.01~0.50 mg·L^(-1)线性关系良好,决定系数R2均在0.99以上。鲜木槿花的检出限在0.3~0.6μg·kg^(-1),定量限在1.0~2.0μg·kg^(-1);干木槿花的检出限在0.3~1.5μg·kg^(-1),定量限在1.0~5.0μg·kg^(-1)。在0.01、0.10、0.50 mg·kg^(-1)的3个加标水平下,鲜样的平均回收率为62.2%~105.7%,相对标准偏差为0.2%~3.8%;干样的平均回收率为70.7%~118.0%,相对标准偏差为0.1%~7.0%。该方法准确度、精密度以及灵敏度均能满足相关要求,适用于木槿花中77种农药残留的定性定量分析。A method was developed for the simultaneous determination of 77 pesticide residues in fresh and dry samples of Hibiscus syriacus L.flowers by QuEChERS pretreatment combined with ultra-high performance liquid chromatography-tandem mass spectrometry.After the samples were crushed,acetonitrile was used for extraction,and dry samples were extracted after adding water.The extract was purified by solid-phase extraction of ethylenediamine-n-propyl silanized silica gel(PSA)and graphitized carbon black(GCB),and quantified by external standard method.The results showed that the linear relationship of 77 pesticides was good in the range of 0.01 mg·L^(-1) to 0.50 mg·L^(-1),and the coefficient of determination R2 was above 0.99.The detection limits of fresh Hibiscus syriacus L.flowers were 0.3μg·kg^(-1) to 0.6μg·kg^(-1),and the quantitation limits were 1.0μg·kg^(-1) to 2.0μg·kg^(-1);the detection limit of dried Hibiscus syriacus L.flower was 0.3μg·kg^(-1) to 1.5μg·kg^(-1),and the quantitation limit was 1.0μg·kg^(-1) to 5.0μg·kg^(-1).Under the three additive levels of 0.01,0.10 and 0.50 mg·kg^(-1),the average recoveries of fresh samples were 62.2%to 105.7%and the relative standard deviations were 0.2%to 3.8%;the average recoveries of dry samples were 70.7%to 118.0%,and the relative standard deviations were 0.1%to 7.0%.The accuracy,precision and sensitivity of the method can meet the relevant requirements,and it is suitable for the qualitative and quantitative analysis of 77 pesticide residues in Hibiscus syriacus L.flowers.

关 键 词：QUECHERS 超高效液相色谱-串联质谱 木槿花 农药残留 

分 类 号：O657.63[理学—分析化学]