PMID- 18969031 OWN - NLM STAT- PubMed-not-MEDLINE DCOM- 20121002 LR - 20081030 IS - 1873-3573 (Electronic) IS - 0039-9140 (Linking) VI - 60 IP - 1 DP - 2003 May 28 TI - Determination of 2,4-dichlorophenoxyacetic acid and its major transformation product in soil samples by liquid chromatographic analysis. PG - 115-21 LID - 10.1016/S0039-9140(03)00113-9 [doi] AB - The 2,4-dichlorophenoxyacetic acid (2,4-D) is one of the most applied herbicides around the world to control broad leave herbs in many crops. In this study, a method was developed for simultaneous extraction and determination of 2,4-D and its major transformation product, i.e., the 2,4-dichlorophenol (2,4-DCP), in soil samples. The herbicide and its degradation product were extracted twice from soil samples, after acidification, by dichloromethane on ultrasound system for 1 h. Both extracts were combined and filtrated in qualitative filter paper and Celite((R)). The total extract was concentrated in rotatory evaporator, dried under N(2) and finally dissolved in 1 ml of methanol. High Performance Liquid Chromatography with UV detection at 230 nm was used for analysis. Recoveries were obtained from soil samples fortified at 0.1, 1.0, 2.0, 3.0 and 4.0 mgkg(-1) levels and the results varied from 85 to 111% (for 2,4-D) and from 95 to 98% (for 2,4-DCP). For both compounds, the limits of quantification were 0.1 mgkg(-1), which were the loss level at which the accuracy and the precision were studied. Nevertheless, the limits of detection, calculated by considering the blank standard deviation and the minimum concentration level, were 0.03 and 0.02 mgkg(-1), for 2,4-D and 2,4-DCP, respectively. This proposed method was applied to soil samples of eucalyptus crops, which was previously treated with the herbicide. Despite that, neither 2,4-D nor its degradation product were detected 30 days after the herbicide application. FAU - de Amarante, O P Jr AU - de Amarante OP Jr AD - Nucleus of Pesticide Residue Analysis (NARP), Department of Technological Chemistry, Federal University of Maranhao, UFMA 65.080-040, Sao Luis, Maranhao, Brazil. FAU - Brito, N M AU - Brito NM FAU - Dos Santos, T C R AU - Dos Santos TC FAU - Nunes, G S AU - Nunes GS FAU - Ribeiro, M L AU - Ribeiro ML LA - eng PT - Journal Article PL - Netherlands TA - Talanta JT - Talanta JID - 2984816R EDAT- 2008/10/31 09:00 MHDA- 2008/10/31 09:01 CRDT- 2008/10/31 09:00 PHST- 2002/07/24 00:00 [received] PHST- 2003/01/14 00:00 [revised] PHST- 2003/01/17 00:00 [accepted] PHST- 2008/10/31 09:00 [pubmed] PHST- 2008/10/31 09:01 [medline] PHST- 2008/10/31 09:00 [entrez] AID - S0039-9140(03)00113-9 [pii] AID - 10.1016/S0039-9140(03)00113-9 [doi] PST - ppublish SO - Talanta. 2003 May 28;60(1):115-21. doi: 10.1016/S0039-9140(03)00113-9.