摘要
研究旨在采用QuEChERS前处理技术结合气相色谱-三重四级杆串联质谱法(GC-MS/MS)对不同批次青贮玉米饲料中20种农药残留进行定性、定量检测分析。以青贮玉米为试验原料,在饲料样品中加入乙腈溶剂和氯化钠提取,取上层离心提取液经50 mg乙二胺-N-丙基硅烷(PSA)、75 mg十八烷基硅烷键合硅胶(C_(18))、40 mg石墨化炭黑(GCB)、200 mg无水硫酸镁净化。在GC-MS/MS多反应监测模式(MRM)下检测分析,空白基质提取液配标,外标法定量分析。结果显示,在质量浓度为0.05~1.00 mg/L范围内线性关系良好,相关系数(R~2)≥0.996 4,方法检出限为0.124~5.324μg/kg,定量限为0.413~14.11μg/kg。20种农药在20、60、100μg/kg的加标浓度下,各农药的平均加标回收率为76.35%~104.56%。回收率试验结果相对标准偏差(RSD)为0.89%~11.45%,满足日常农药残留痕量分析工作要求。研究表明,该方法具有前处理操作简单、重复性好、灵敏度高等优势,能够有效地消除基质干扰,减少假阳性的检出率,提高分析选择性,降低分析成本。
The study was to qualitatively and quantitatively detect and analyze 20 pesticide residues in different batches of silage corn feed by QuEChERS pretreatment technology combined with GC-MS/MS.Using silage corn as the experimental material,acetonitrile solvent and sodium chloride were added to the feed sample for extraction.The upper centrifuged extract was treated with 50 mg PSA,75 mg Cig,40 mg GCB and 200 mg anhydrous magnesium sulfate were used for purification,detected and analyzed under GC-MS/MS MRM,and the blank matrix extract was quantitatively analyzed by standard external standard method.The results showed that the linear relationship was good in mass concentration range of 0.05~1.00 mg/L,and R²≥0.9964.The detection limit of the method was 0.124~5.324μg/kg,and the quantitative limit of the method was 0.413-14.11μg/kg.The average recoveries of 20 pesticides at 20,60,100μg/kg ranged from 76.35%~104.56%.The RSD of the recovery test results was 0.89%~11.45%,which could fully meet the daily work of trace analysis of pesticide residues.The study indicates that the method has the advantages of simple pretreatment operation,good repeatability,high sensitivity,which can effectively eliminate matrix interference,reduce the detection rate of false positives,improve the selectivity of analysis and reduce the cost of analysis.
作者
余磊
赵志燊
YU Lei;ZHAO Zhi-shen
出处
《饲料研究》
CAS
北大核心
2023年第10期116-121,共6页
Feed Research
基金
贵州生态环境中优势农产品残留农药降解关键技术研究重点实验室项目(项目编号:黔教合KY字[2018] 005)
贵阳市科技局贵阳学院专项资金(项目编号:GYU-KY-[2021])。
