摘要
试验旨在建立一种适用于植物源性宠物饲粮中多种农药残留的分析方法。样品经水浸泡后,采用乙腈振荡提取并结合净化管进行净化。使用DB-5ms色谱柱(30 m×0.25 mm,0.25μm)进行分离,在高纯氦载气(流速1.3 mL/min)条件下,依托气相色谱-串联质谱联用技术(GC-MS/MS),用电子轰击离子源(EI),在动态多反应监测模式(dMRM)下进行检测,并采用内标法进行定量分析。结果显示,目标化合物在0.01~0.50 mg/L范围线性良好(相关系数R^(2)>0.997 0),方法定量限为0.001~0.300 mg/kg,加标回收率为62.2%~117.2%,精密度范围为0.3%~13.0%。应用该方法对6种市售植物源性宠物饲粮进行检测,马拉硫磷、联苯菊酯、甲氰菊酯、氯菊酯、氟胺氰菊酯和溴氰菊酯最高检出含量分别为0.013、0.039、0.027、0.056、0.341和0.080 mg/kg。研究表明,试验建立的检测方法操作简单、灵敏度高、适用性强,可用于植物源性宠物饲粮中多种农药残留的同步检测。
This experiment aimed to establish an analytical method for the determination of multiple pesticide residues in plant-derived pet feed.Samples were soaked in water and extracted with acetonitrile by shaking,followed by purification using a cleanup tube.Separation was achieved using a DB-5ms capillary column(30 m×0.25 mm,0.25μm)under a high-purity helium carrier gas(flow rate 1.3 mL/min),relying on gas chromatography-mass spectrometry(GC-MS/MS)and electron bombardment ion source(EI)for detection in dynamic multi reaction monitoring mode(dMRM),and quantitative analysis was performed using internal standard method.The results showed that good linearity for the target compounds in the range of 0.01 to 0.50 mg/L(R^(2)>0.9970).The method quantification limits were 0.001 to 0.300 mg/kg,the average recoveries for matrix-spiked samples ranged from 62.2%to 117.2%,and the precision was from 0.3%to 13.0%.The method was applied to analyze six commercially available plant-derived pet feed products.The maximum detected concentrations of malathion,bifenthrin,fenpropathrin,permethrin,tau-fluvalinate,and deltamethrin were 0.013,0.039,0.027,0.056,0.341,and 0.080 mg/kg,respectively.The study shows that the established method is simple,sensitive,and widely applicable,enabling simultaneous detection of multiple pesticide residues in plant-derived pet feed.
作者
黄仁贵
袁涛
段成
熊璞
陈序根
毛慧娟
谭莎莎
杨琴
HUANG Rengui;YUAN Tao;DUAN Cheng;XIONG Pu;CHEN Xugen;MAO Huijuan;TAN Shasha;YANG Qin
出处
《饲料研究》
北大核心
2025年第22期142-147,共6页
Feed Research
基金
重庆仕益产品质量检测有限责任公司科研开发类项目(项目编号:CBS202403-T)。