因为是测土壤中的残留量,所以这个方法很麻烦--强酸加有机溶剂萃取后,polymer SPE净化,浓缩衍生后,再上
$$lcMSMS. 试过前两步后,直接浓缩上
$$lcMSMS,C18上基质效应还挺强,但检测限到0.01ppm没有问题。
有人有下面这个的全文吗,似乎水果蔬菜上的基质效应不高。
J AOAC Int. 2012 Mar-Apr;95(2):554-9.
Simultaneous determination of aminopyralid, clopyralid, and picloram residues in vegetables and fruits using ultra-performance liquid chromatography/tandem mass spectrometry.
Tian Y, Liu X, Dong F, Xu J, Lu C, Kong Z, Wang Y, Zheng Y.
Source
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.
Abstract
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.