摘要
建立了同时测定果蔬中6种酰胺类农药的固相萃取-超高效液相色谱-串联质谱（SPE-UPLC-MS/MS）方法。样品经乙腈高速匀浆提取、Florisil固相萃取柱净化,采用超高效液相色谱-串联质谱法测定6种农药。质谱分析采用电喷雾电离,正负双离子扫描,多反应监测（MRM）模式。结果表明：6种农药在0.000 5~1.00 mg/L范围内均呈现良好的线性关系,相关系数均大于0.999;在0.01、0.1和1.0 mg/kg（氟苯虫酰胺为0.001、0.01和0.1 mg/kg）3个浓度添加水平下的平均回收率为72.4%~119.4%,相对标准偏差（n=5）小于15%;定量限为0.01 mg/kg（溴氰虫酰胺、双炔酰菌胺、啶酰菌胺、氟吡菌胺和噻呋酰胺）和0.001 mg/kg（氟苯虫酰胺）。该方法简单、快速、重现性好、灵敏度高,可满足果蔬中6种酰胺类农药残留检测的要求。
A solid phase extraction coupled with ultra high performance liquid chromatographytandem mass spectrometry（SPE-UPLC-MS / MS） method was developed for simultaneous determination of six amide pesticides,cyantraniliprole,mandipropamid,boscalid,fluopicolide,thifluzamide and flubendiamide,in vegetables and fruits. After extraction with acetonitrile,purification with Florisil SPE cartridges and dissolution with methanol,the targets in the sample solutions were analyzed by UPLC-MS / MS on an Agilent Proshell 120 EC-C18 column with a mixture of 0. 1% formic acid solution and methanol as the mobile phases under gradient elution conditions. The mass spectrometer operated in multiple reaction monitoring（MRM）mode with the negative and positive modes. Good linearity was obtained for the six amide pesticides at the mass concentrations of 0. 000 5- 1. 00 mg / L with the correlation coefficients more than 0. 999.The fortified recoveries were in the range of 72. 4%- 119. 4% with the concentration levels at0. 01,0. 1 and 1. 0 mg / kg for cyantraniliprole,mandipropamid,boscalid,fluopicolide,thifluzamide,and 0. 001,0. 01 and 0. 1 mg / kg for flubendiamide. The relative standard deviations（RSDs）were less than 15% and the limits of quantification were 0. 01 mg/ kg for cyantraniliprole,mandipropamid,boscalid,fluopicolide,thifluzamide,and 0. 001 mg / kg for flubendiamide.All the above observations indicate that the established analytical method is simple,efficient and sensitive,and suitable for the determination of the six amide pesticides in vegetables and fruits.
出处
《色谱》
CAS
CSCD
北大核心
2015年第10期1019-1025,共7页
Chinese Journal of Chromatography
基金
上海市农委科技攻关项目(沪农科攻字(2015)第4-6号)
关键词
超高效液相色谱-串联质谱
固相萃取
酰胺类农药
残留
蔬菜
水果
ultra high performance liquid chromatography-tandem mass spectrometry（UPLC-MS / MS）
solid phase extraction（SPE）
amide pesticides
residues
vegetables
fruits
