固相萃取-气相色谱-串联质谱法测定豆粕饲料中35种农药残留OA
Determination of 35 pesticide residues in soybean meal feed by solid phase extraction combined with gas chromatography-tandem mass spectrometry
本研究旨在建立固相萃取前处理与气相色谱-三重四极杆质谱联用技术(GC-MS/MS)的高通量分析方法,用于检测 35 种农药在豆粕饲料基质中的残留.采用乙腈溶剂提取目标物,结合GC-MS/MS多反应离子监测(MRM)模式进行检测,外标法定量,通过石墨化碳黑/氨基(Carb-GCB/NH2)复合柱净化体系去除基质干扰.结果表明:35 种农药在浓度0.01~0.50 mg/L内线性关系良好,相关系数均≥0.99,方法灵敏度检出限为0.003 mg/kg,定量限为0.01mg/kg.在 0.01、0.05、0.10 mg/kg三个加标浓度下,平均回收率为70.20%~120.67%,相对标准偏差(RSD)为0.63%~12.53%.该方法操作简单,具备良好的准确度与重现性,适用于饲料产品中多种农药残留的快速筛查与定量分析.
This study aimed to established a high-throughput analytical method combining solid-phase extraction pretreatment with gas chromatography-triple quadrupole tandem mass spectrometry(GC-MS/MS)for detecting 35 pesticide residues in soybean meal feed matrices.The target compounds were extracted using acetonitrile solvent and detected through GC-MS/MS in multiple reaction monitoring(MRM)mode,with quantification performed via external standard method.A graphitized carbon black/aminopropyl(Carb-GCB/NH2)composite cartridge purification system was employed to eliminate matrix interferences.Results demonstrated excellent linear relationships for all pesticides within the range of 0.01~0.50 mg/L,with correlation coefficients≥0.99.The method exhibited high sensitivity,showing a detection limit of 0.003 mg/kg and quantification limit of 0.01 mg/kg.At three spiked concentration levels(0.01,0.05,0.10 mg/kg),average recoveries ranged from 70.20%to 120.67%,with relative standard deviations(RSD)between 0.63%and 12.53%.This optimized approach simplifies operational procedures while maintaining good accuracy and reproducibility,proving suitable for rapid screening and quantitative analysis of multiple pesticide residues in feed products.
刘慧玲;张冀平;康占省;王敬
秦皇岛海关煤炭检测技术中心,河北 秦皇岛 066000秦皇岛海关煤炭检测技术中心,河北 秦皇岛 066000石家庄海关技术中心,河北 石家庄 050051石家庄海关技术中心,河北 石家庄 050051
农业科技
气相色谱-质谱农药残留固相萃取前处理豆粕饲料
GC-MS/MSpesticides residualsolid-phase extractionpretreatmentsoybean meal feed
《中国饲料》 2026 (11)
106-112,7
海关总署科研项目(2023HK081)
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