UPLC/MS/MS同位素内标法检测水果中7种农药残留  

Detection of seven kinds of pesticide residues in fruitsby isotope-labelled internal standard quantitation with UPLC/MS/MS methods

作　　者：管秋美 郑仁锦[1] 刘琳琳 黄宏南[1,2] 康孟丹 卢嘉丽 

机构地区：[1]福建省疾病预防控制中心,福州350001 [2]福建医科大学药学院,福州350004 [3]福建中医药大学药学院,福州350122

出　　处：《海峡预防医学杂志》2017年第1期3-5,84,共4页Strait Journal of Preventive Medicine

摘　　要：目的建立以同位素为内标物同时测定水果中7种农药残留(多菌灵、甲基硫菌灵、甲霜灵、嘧霉胺、三唑酮、氯吡脲、2,4-二氯苯氧乙酸)的超高效液相色谱-串联质谱(UPLC/MS/MS)方法。方法样品经1%(V/V)乙酸的乙腈溶液提取,无水硫酸镁和醋酸钠脱水,分散固相萃取管净化,ACQUITY HSS T3色谱柱分离,以乙腈-5mmol/L甲酸铵10mmol/L甲酸溶液为流动相,流速0.3mL/min,柱温30℃,电喷雾电离,正负离子分段扫描和多反应监测模式检测,同位素内标法定量。结果 7种农药在10~200μg/kg范围内线性关系良好。平均回收率73.1%~103%,RSD=2.1%~5.0%。检出限(LOD)为0.25~0.65μg/kg,定量限(LOQ)为0.83~2.16μg/kg。结论该方法简便快速,定量准确,可满足多种水果中7种农药残留的检测要求。Objective To establish an isotope-labelled internal standard method for rapid detection of seven kinds of pesticides（carbendazim,thiophanate-methyl,metalaxyl,pyrimethanil,triadimefon,forchlorfenuron and 2,4-D）in fruits by ultra performance liquid chromatography/mass/mass spectrometry（UPLC/MS/MS）.Methods The samples were extracted by acetonitrile containing 1%（V/V）acetic acid,followed by dehydrate using the powder of anhydrous magnesium sulfate and sodium acetate and then purifies by dispersive solid-phase extraction pipe.The resulting samples were separated on a ACQUITY HSS T3 column,using acetonitrile-5 mmoL/L ammonium formate and 10mmoL/L formic acid in water as mobile phase,with a flow rate at 0.3mL/min,a column temperature at 30℃.The samples were detected under positive and negative multiple reactions monitoring（MRM）mode through polarity switching between time segments.The quantitative analysis was carried out by isotope-labelled internal standard method.Results The method showed a good linearity in the rang of 10-200μg/kg.The recoveries ranged from 73.1% to103%,and the relative standard deviation ranged from 2.1%to 5.0%.The detection limit（LOD）ranged from 0.25 to 0.65μg/kg.The quantification limit（LOQ）ranged from 0.83 to 2.16μg/kg.Conclusion The method was simple,quick and accurate,and suitable for the detection of seven kinds of pesticide residues in fruits.

关 键 词：农药残留 超高效液相色谱-串联质谱法(UPLC/MS/MS) 同位素内标法 分散固相萃取 水果 

分 类 号：R155.5[医药卫生—营养与食品卫生学]