摘要
目的建立基于QuEChERS前处理与高效液相色谱-串联质谱法(high performance liquid chromat ography-tandem mass spectrometry, HPLC-MS/MS)测定莲子中8种农药(多菌灵、甲基硫菌灵、精甲霜灵、戊唑醇、苯醚甲环唑、肟菌酯、吡虫啉、克百威)残留量的分析方法。方法样品经乙腈和QuEChERS提取包提取, QuEChERS净化管净化,在HPLC-MS/MS系统的多反应监测模式(multiple reaction monitoring, MRM)下进行8种农药的定量和定性分析。结果 8种农药在0.1~250.0μg/L的范围内呈现良好线性关系,相关系数r2均大于0.998;方法的检出限和定量限分别为0.01~0.09μg/kg和0.04~0.3μg/kg;在4个加标水平下(0.3μg/kg、0.01、0.10、0.50mg/kg),加标回收率为79.1%~97.0%,相对标准偏差(relative standard deviation,RSD)为1.35%~6.44%。结论本方法的重复性和回收率满足实验要求,适用莲子中部分农药残留的分析检测。
Objective To establish a method for the determination of 8 kinds of pesticide residues(carbendazim, thiophanate-methyl, metalaxyl-M, tebuconazole, difenoconazole, trifloxystrobin, imidacloprid, carbofuran) in lotus seed based on QuEChERS pretreatment and high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS). Methods The samples were extracted with acetonitrile and QuEChERS extraction kit, followed by purification with QuEChERS purification tube. The qualitative and quantitative analysis of 8 kinds of pesticide were performed by HPLC-MS/MS in the multiple reaction monitoring(MRM) mode. Results Eight kinds of pesticide exhibited good linear relationships within the range of 0.1-250.0 μg/L, and the correlation coefficients r2 were greater than 0.998. The limit of detection and limit of quantitative were 0.01-0.09 μg/kg and 0.04-0.3 μg/kg, respectively. At the 4 spiked levels(0.3 μg/kg, 0.01, 0.10, and 0.50 mg/kg), the spiked recoveries were 79.1%-97.0%, and the relative standard deviations were 1.35%-6.44%. Conclusion The repeatability and recovery of this method meet the experimental requirements, and it is suitable for the analysis and detection of some pesticide residues in lotus seed.
作者
陈祥奕
姚奋增
CHEN Xiang-Yi;YAO Fen-Zeng(Fujian Institite for Food and Drug Quality Control,Fuzhou 350002,China)
出处
《食品安全质量检测学报》
CAS
北大核心
2021年第12期4903-4908,共6页
Journal of Food Safety and Quality
关键词
QUECHERS
高效液相色谱-串联质谱法
农药残留
莲子
QuEChERS
high performance liquid chromatography-tandem mass spectrometry
pesticide residues
lotus seed
