Tian Yingying, Liu Xingang, Dong Fengshou, Xu Jun, Lu Caihong, Kong Zhiqiang, Wang Yunhao, Zheng Yongquan
Chinese Academy of Agricultural Sciences, Institute of Plant Protection, Ministry of Agriculture, Key Laboratory of Pesticide Chemistry and Application, Beijing 100193, People's Republic of China.
J AOAC Int. 2012 Mar-Apr;95(2):554-9. doi: 10.5740/jaoacint.11-120.
A sensitive and effective method for the simultaneous quantitative determination of aminopyralid, clopyralid, and picloram in vegetables (eggplant, cucumber, and tomato) and fruits (apple and grape) was developed and validated using ultra-performance LC coupled with MS/MS. The three herbicides were successfully separated and independently confirmed in a single run. Different extraction and cleanup methods were used to optimize the pretreatment processes of the residue analysis method. The final method is straightforward and involves extraction with 1% formic acid-acetonitrile, and no complicated cleanup process is needed. Determination of the compounds was achieved within 3.0 min. Respective average recoveries using this method at four concentration levels (0.05, 0.1, 0.5, and 1.0 mg/kg) ranged from 66.5 to 109.4%, with RSDs in the range of 1.1-19.7% (n = 5) for all analytes. The LODs were below 0.010 mg/kg, and the LOQs did not exceed 0.036 mg/kg, which were lower than the maximum residue limits (MRLs) of 0.5-5.0 mg/kg clopyralid in vegetables and fruits samples, as established by the European Union. This study provides a theoretical basis for China to develop MRLs and an analytical method for aminopyralid, clopyralid, and picloram in vegetables and fruits.
建立了一种灵敏有效的方法，用于同时定量测定蔬菜（茄子、黄瓜和番茄）和水果（苹果和葡萄）中的氨氯吡啶酸、氯吡脲和毒莠定，并采用超高效液相色谱-串联质谱法进行了验证。这三种除草剂在一次运行中成功分离并独立确认。采用不同的提取和净化方法优化了残留分析方法的预处理过程。最终方法简单直接，采用1%甲酸-乙腈提取，无需复杂的净化过程。在3.0分钟内完成了化合物的测定。在四个浓度水平（0.05、0.1、0.5和1.0mg/kg）下，该方法的平均回收率分别为66.5%至109.4%，所有分析物的相对标准偏差（RSD）在1.1%-19.7%范围内（n = 5）。检测限低于0.010mg/kg，定量限不超过0.036mg/kg，低于欧盟规定的蔬菜和水果样品中氯吡脲0.5-5.0mg/kg的最大残留限量（MRL）。本研究为我国制定氨氯吡啶酸、氯吡脲和毒莠定在蔬菜和水果中的最大残留限量提供了理论依据及分析方法。
