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目的:建立刺梨中甲萘威、灭多威、涕灭威、残杀威、克百威等5种氨基甲酸酯类农药残留检测方法。方法:采用高速匀浆制备样品,以乙腈为提取溶剂,提取液浓缩后经氨基固相萃取小柱净化,采用梯度洗脱分离,色谱系统条件为Thermo Hypersil GOLD色谱柱(2.1 mm×100 mm,1.9μm),柱温20℃,流速300μL·min-1,进样量10μL。在电喷雾正离子模式下,使用三重四级杆质谱仪上以多反应检测模式测定,质谱系统条件为喷雾电压3.0 kV,鞘气压力40 psi,碰撞气压力1.5 mTorr,离子传输管温度350℃,蒸发温度250℃。结果:5种农药在0.5~100μg·L-1线性关系良好,相关系数均>0.999 0,方法检出限为0.2μg·kg;低、中、高3个水平的加标平均回收率在77.9%~107.2%,RSD在4.5%~13.2%。结论:该法快速、准确、灵敏,适合刺梨中克百威等5种氨基甲酸酯类农药的残留分析。
Objective: To establish a method for the determination of carbamate residues in carbaryl, methomyl, aldicarb, propoxur and carbofuran. Methods: The sample was prepared by high speed homogenization. Acetonitrile was used as the extraction solvent. The extract was concentrated and purified by Amino Solid Phase Extraction (SPE) column. The residue was separated by gradient elution. The chromatographic conditions were Thermo Hypersil GOLD column (2.1 mm × 100 mm, 1.9μm), the column temperature was 20 ℃, the flow rate was 300μL · min-1, and the injection volume was 10μL. In electrospray positive mode, the triple quadrupole mass spectrometer was used in the multi-reaction detection mode with mass spectrometry system conditions of 3.0 kV spray pressure, 40 psi sheath pressure, 1.5 mTorr collision gas pressure, 350 ° C ion transport tube temperature , Evaporation temperature 250 ℃. Results: The linear correlations of the five pesticides at 0.5-100 μg · L-1 were good with the correlation coefficients> 0.999 0 and the detection limit of 0.2 μg · kg-1. The average recoveries of three pesticides at the low, medium and high levels were 77.9 % ~ 107.2%, RSD 4.5% ~ 13.2%. Conclusion: The method is rapid, accurate and sensitive and suitable for the residue analysis of carbamate pesticides in Cili.