PMID- 22649944 OWN - NLM STAT- MEDLINE DCOM- 20120730 LR - 20191112 IS - 1060-3271 (Print) IS - 1060-3271 (Linking) VI - 95 IP - 2 DP - 2012 Mar-Apr TI - Simultaneous determination of aminopyralid, clopyralid, and picloram residues in vegetables and fruits using ultra-performance liquid chromatography/tandem mass spectrometry. PG - 554-9 AB - 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. FAU - Tian, Yingying AU - Tian Y AD - 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. FAU - Liu, Xingang AU - Liu X FAU - Dong, Fengshou AU - Dong F FAU - Xu, Jun AU - Xu J FAU - Lu, Caihong AU - Lu C FAU - Kong, Zhiqiang AU - Kong Z FAU - Wang, Yunhao AU - Wang Y FAU - Zheng, Yongquan AU - Zheng Y LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't PL - England TA - J AOAC Int JT - Journal of AOAC International JID - 9215446 RN - 0 (Carboxylic Acids) RN - 0 (Herbicides) RN - 0 (Pesticide Residues) RN - 0 (Picolinic Acids) RN - 0 (Pyridines) RN - 10G14M0WDH (clopyralid) RN - 9S4EMJ60LF (aminopyralid) RN - O7437X49DW (Picloram) SB - IM MH - Carboxylic Acids/*chemistry MH - Chromatography, High Pressure Liquid/*methods MH - Food Analysis MH - Fruit/*chemistry MH - Herbicides/chemistry MH - Molecular Structure MH - Pesticide Residues/chemistry MH - Picloram/*chemistry MH - Picolinic Acids/*chemistry MH - Pyridines/*chemistry MH - Sensitivity and Specificity MH - Tandem Mass Spectrometry/methods MH - Vegetables/*chemistry EDAT- 2012/06/02 06:00 MHDA- 2012/07/31 06:00 CRDT- 2012/06/02 06:00 PHST- 2012/06/02 06:00 [entrez] PHST- 2012/06/02 06:00 [pubmed] PHST- 2012/07/31 06:00 [medline] AID - 10.5740/jaoacint.11-120 [doi] PST - ppublish SO - J AOAC Int. 2012 Mar-Apr;95(2):554-9. doi: 10.5740/jaoacint.11-120.