第 51 卷第 4 期Vol. 51 No. 4
2021 年 8 月Aug 2021

所属栏目:分析与测试

超高效液相色谱-串联质谱法同时检测氟啶虫酰胺、呋虫胺及两种代谢物在桃中的残留量
曾利红1,2,3,欧阳宇迪1,2,欧晓明1,2,侯根连1,2,3,晏 姣1,2,3,欧 将1,2,3,梁贵平1,2,3,宋强勇1,2,3,聂春林1,2,3 (1. 湖南化工研究院有限公司 国家农药创制工程技术研究中心,湖南 长沙 410014;2. 农用化学品湖南省重点实验室,湖南 长沙 410014;3. 湖南化研院检测技术有限公司,湖南 长沙 410014)
摘 要:建立了超高效液相色谱-串联质谱(UPLC-MS/MS)测定桃中氟啶虫酰胺、呋虫胺及代谢物残留量的方法。样品经1%乙酸水溶液涡旋提取,采用电喷雾离子源正离子扫描,多反应监测(MRM)模式下,外标法定量。结果表明:方法在0.002~0.100 μg/mL范围内线性良好,相关系数(R2)>0.99;在0.05、0.8、4.0 mg/kg添加水平下四种农药的平均回收率为80%~115%,相对标准偏差1%~6%,定量限均为0.05 mg/kg。
关键词:UPLC-MS/MS;氟啶虫酰胺;呋虫胺及代谢物DN、UF;桃;残留检测
中图分类号:O657.7  文献标识码:A  文章编号:1009-9212(2021)04-0077-04
Determination of Flonicamid, Dinotefuran and 2 Kinds of Metabolites in Peach by UPLC-MS/MS
ZENG Li-hong1,2,3, OUYANG Yu-di1,2, OU Xiao-ming1,2, HOU Gen-lian1,2,3, YAN Jiao1,2,3, OU Jiang1,2,3, LIANG Gui-ping1,2,3, SONG Qiang-yong1,2,3, NIE Chun-lin1,2,3 (1. National Engineering Research Center for Agrochemicals, Hunan Research Institute of Chemical Industry, Changsha 410014, China; 2. Hunan Province Key Laboratory for Agrochemicals, Changsha 410014, China; 3. HRICI Test Co.,Ltd., Changsha 410014, China)
Abstract:A method was established for the simultaneous determination of flonicamid, dinotefuran and metabolites residues in peach by UPLC-MS/MS. The sample was vortexed extraction with 1% acetic acid water, then detected by MS/MS eqipped with positive electrospray ionization(ESI+) in multiple reaction monitoring (MRM) mode and quantified by external standard method. The results showed that the limits of quantitation were 0.05 mg/kg; the correlation coefficient of 4 pesticides were higher than 0.99 in a concentration ranged from 0.002 μg/mL to 0.100 μg/mL. The mean spiked recoveries of 4 pesticides at 0.05, 0.8 and 4 mg/kg with spiked levels ranged from 80% to 115% at a relative standard deviations (RSD) between 1% and 6%
Key words:UPLC-MS/MS; flonicamid; dinotefuran and metabolites DN, UF; peach; residue determination
基金项目:湖南省企业科技创新团队支持计划资助项目(海利新材料科技创新创业团队)。
作者简介:曾利红(1987—),女,湖南醴陵人,工程师,硕士研究生,研究方向:农药残留检测(E-mail:645470004@qq.com)。
收稿日期: 2021-07-2