Residual Pattern of Acequinocyl and Hydroxyacequinocyl in Perilla Leaf Grown under Greenhouse Conditions using Ultra Performance Liquid Chromatography-Photo Diode Array Detector with Tandem Mass Confirmation
Residual Pattern of Acequinocyl and Hydroxyacequinocyl in Perilla Leaf Grown under Greenhouse Conditions using Ultra Performance Liquid Chromatography-Photo Diode Array Detector with Tandem Mass Confirmation
复制标题
DOI：
10.1007/s13765-012-2101-x
复制
发表时间：
2012-10-01
影响因子：
--
通讯作者：
Shim, Jae-Han
中科院分区：
文献类型：
--
作者：
Na, Tae Woong;Rahman, Md. Musfiqur;Shim, Jae-Han
在温室条件下生长的紫苏叶中测定了喹螨醚和羟基喹螨醚的残留及降解行为。将喹螨醚（15%，悬浮剂）以37.5克/250升水/10公亩的推荐剂量进行单次和双倍剂量喷施于紫苏叶上。在施药后0（施药后2小时）、1、3、5和7天从两个不同地块随机采集叶片样本。样本用乙腈提取，通过固相萃取程序净化，并采用超高效液相色谱 - 光电二极管阵列检测器（UPLC - PDA）进行分析。通过液相色谱 - 串联质谱（LC - MS/MS）在正离子电喷雾电离（ESI +）模式下对残留进行确认。校准曲线在分析物的浓度范围内呈线性，相关系数r²≥0.992。喹螨醚和羟基喹螨醚的检测限和定量限分别为0.05毫克/千克和0.165毫克/千克。该方法在基质的两个添加浓度下进行了三次验证。目标分析物的回收率良好，介于94.95% - 113.26%之间，相对标准偏差小于6%。单次和双倍剂量下紫苏叶上总喹螨醚的消失速率符合一级动力学，半衰期分别为2.8天和3.1天。
Persistence and degradation behaviors of acequinocyl and hydroxyacequinocyl were determined in perilla leaf grown under greenhouse conditions. Acequinocyl (15%, SC) was sprayed on perilla leaf at the recommended dose rate of 37.5 g/250 L water/10a with single and double dose applications. Leaf samples were collected randomly at 0 (2 h after application), 1, 3, 5, and 7 days post-application from two different plots. The samples were extracted with acetonitrile, purified through a solid phase extraction procedure, and analyzed via ultra performance liquid chromatography coupled with photo diode array detector (UPLC-PDA). Residues were confirmed via liquid chromatography tandem mass spectrometry (LC-MS/MS) in positive-ion electrospray ionization (ESI+) mode. Calibration curves were linear over the concentration ranges for the analytes with r(2) >= 0.992. The limits of detection and quantification were 0.05 and 0.165 mg/kg for both acequinocyl and hydroxyacequinocyl. The method was validated in triplicate at two fortification concentrations in the matrix. Good recoveries were observed for the target analytes, ranging between 94.95 and 113.26% with relative standard deviations less than 6%. The rates of disappearance of total acequinocyl on perilla leaf for single and double doses were described as first-order kinetics with half-lives of 2.8 and 3.1-days, respectively.