摘要
目的建立一种加速溶剂萃取结合气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry, GC-MS/MS)同时检测菊花中123种农药残留的方法。方法样品采用乙腈提取,经加速溶剂萃取,石墨化碳/氨基固相萃取小柱净化,SH-Rxi-5SilMS (30 m×0.25 mm, 0.25μm)毛细管色谱柱分离,在气相色谱串联质谱多反应监测离子(multiple reaction monitoring, MRM)扫描模式下进行测定,基质外标法定量。结果在0.005~0.5mg/L范围内,123种农药有良好的线性关系(r^2≥0.9967),方法检出限为0.5~29.1μg/kg,定量下限为1.7~97.1μg/kg,在100、200、400μg/kg 3个添加水平下,123种农药的平均回收率在70.0%~128.8%之间,相对标准偏差(RSD)在0.5%~10.1%。结论该方法提取效率高、准确、灵敏,可应用于菊花中多种农药残留的筛查与测定。
Objective To establish a method for simultaneous determination of 123 pesticide residues in chrysanthemum by accelerated solvent extraction coupled with gas chromatography-tandem mass spectrometer (GC-MS/MS). Methods Chrysanthemum samples were extracted by acetonitrile, and purified through Carb/NH2 solid phase extraction (SPE) cartridges after accelerated solvent extraction. The residues were separated on the SH-Rxi-5SilMS (30 m×0.25 mm, 0.25 μm) capillary column, analyzed by GC-MS/MS with multiple reaction monitoring mode, and quantified by external standard method. Results The results showed that 123 kinds of pesticides had good linear relationships at the range of 0.005-0.5 mg/L, with correlations coefficients more than 0.9967. The limits of detection were 0.5-29.1 μg/kg, and the limits of quantitation were 1.5-97.1 μg/kg. The average recoveries of 123 compounds at three spiked levels of 100, 200, 400 μg/kg ranged from 70.0% to 128.8%, with relative standard deviations of 0.5%-10.1%. Conclusions This method is accurate and sensitive with higher extraction efficiency, which can be applied to the screening and simultaneous determination of multiresidue in chrysanthemum.
作者
韩梅
侯雪
邱世婷
王悦涵
HAN Mei;HOU Xue;QIU Shi-Ting;WANG Yue-han(Center of Analysis and Testing, Sichuan Academy of Agricultural Sciences, Risk Assessment Lab for Agricultural Products (Chengdu), Ministry of Agriculture, Chengdu 610066, China)
出处
《食品安全质量检测学报》
CAS
2019年第10期3065-3077,共13页
Journal of Food Safety and Quality
关键词
菊花
加速溶剂萃取
石墨化碳/氨基固相萃取
气相色谱-串联质谱法
农药残留
chrysanthemum
accelerated solvent extraction
Carb/NH2 solid phase extraction
gas chromatography-tandem mass spectrometry
pesticide residues
