UHPLC-MS-MS同时测定蔬菜中12种磺酰脲类除草剂  

Determination of 12 Kinds Sulfonylurea Herbicides in Vegetables by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：周敏 沈雄雅 倪娟桢 赵月钧 钟寒辉 孙文闪 ZHOU Min;SHEN Xiongya;NI Juanzhen;ZHAO Yuejun;ZHONG Hanhui;SUN Wenshan(Greentown Agricultural Testing Technology Co.,Ltd.,Hangzhou 310051)

机构地区：[1]绿城农科检测技术有限公司,杭州310051

出　　处：《食品工业》2022年第1期281-285,共5页The Food Industry

基　　金：国家重点研发计划资助(2018YFC1602800)。

摘　　要：该试验旨在建立分散固相萃取超高效液相色谱-串联质谱法同时测定蔬菜中12种磺酰脲除草剂残留量的方法。方法在对样品的前处理方法及目标物质谱分析条件进行优化的条件下,蔬菜样品经1%乙酸-乙腈提取,分散固相萃取净化,经UHPLC-AQ-C_(18)色谱柱分离,乙腈-0.1%甲酸溶液为流动相梯度洗脱,经超高效液相色谱-串联质谱仪采用电喷雾多反应监测模式检测,基质匹配标准溶液外标法定量。磺酰脲除草剂在3.00~500μg/kg范围内均呈良好线性关系,相关系数为0.999 0~0.999 8,检出限(S/N=3)均为1.00μg/kg,定量限(S/N=10)均为3.00μg/kg,3个加标水平(3.00,10.0和500μg/kg)下的加标回收率在80.1%~99.5%,相对标准偏差(n=6)为3.31%~9.82%。该方法简便、快速、结果准确可靠、灵敏度高,适用于蔬菜中12种磺酰脲类除草剂的同时测定。A method was established for the simultaneous determination sulfonylurea herbicides with dispersive solid phase extractionin vegetables by ultra-high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Samples were extracted by 1% acetic acid acetonitrile.The UPLC-MS/MS method was performed with an UHPLC-AQ-C_(18) column using gradient elution with a mobile phase of acetonitrile and 0.1% formic acid in water.The target compounds were detected by multiple reaction monitoring(MRM) with an electrospray ionization source in the positive ion mode,and quantified by an external standard method using a matrix-match standard solution.The calibration curves showed good linearity with correlation coefficients 0.999 0-0.999 8,in the range of 3.00-500 μg/kg,the limit of detection(S/N=3) was 1.00 μg/kg,the limit of quantitation(S/N=10) was 3.00 μg/kg,and the recovery rate of three levers(3.00,10.0 and 500 μg/kg) was 80.1%-99.5%.The relative standard deviation(n=6) was 3.31%-9.82%.The established method was simple,sensitive,accurate and reliable,and could be applied for the simultaneous determination of 12 kinds sulfonylurea herbicides in the vegetables.

关 键 词：分散固相萃取 蔬菜 磺酰脲 除草剂 液相色谱-串联质谱 

分 类 号：O657.63[理学—分析化学] TS255.7[理学—化学]