QuEChERS-高效液相色谱-串联质谱法检测莲子中8种农药残留

Determination of 8 kinds of pesticide residues in lotus seed by QuEChERS combined with high performance liquid chromatography-tandem mass spectrometry

中文关键词:  QuEChERS  高效液相色谱-串联质谱法  农药残留  莲子

英文关键词:QuEChERS  high performance liquid chromatography-tandem mass spectrometry  pesticide residues  lotus seed

中文摘要:

      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0.1~250.0 μg/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0.01~0.09 μg/kg和0.04~0.3 μg/kg; 在4个加标水平下(0.3 μg/kg、0.01、0.10、0.50 mg/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。

英文摘要:

      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.