PMID- 26723494 OWN - NLM STAT- MEDLINE DCOM- 20161101 LR - 20161230 IS - 1096-0309 (Electronic) IS - 0003-2697 (Linking) VI - 497 DP - 2016 Mar 15 TI - Miniaturized and direct spectrophotometric multi-sample analysis of trace metals in natural waters. PG - 18-23 LID - S0003-2697(15)00570-9 [pii] LID - 10.1016/j.ab.2015.11.025 [doi] AB - Trends in the analysis of trace metals in natural waters are mainly based on the development of sample treatment methods to isolate and pre-concentrate the metal from the matrix in a simpler extract for further instrumental analysis. However, direct analysis is often possible using more accessible techniques such as spectrophotometry. In this case a proper ligand is required to form a complex that absorbs radiation in the ultraviolet-visible (UV-Vis) spectrum. In this sense, the hydrazone derivative, di-2-pyridylketone benzoylhydrazone (dPKBH), forms complexes with copper (Cu) and vanadium (V) that absorb light at 370 and 395 nm, respectively. Although spectrophotometric methods are considered as time- and reagent-consuming, this work focused on its miniaturization by reducing the volume of sample as well as time and cost of analysis. In both methods, a micro-amount of sample is placed into a microplate reader with a capacity for 96 samples, which can be analyzed in times ranging from 5 to 10 min. The proposed methods have been optimized using a Box-Behnken design of experiments. For Cu determination, concentration of phosphate buffer solution at pH 8.33, masking agents (ammonium fluoride and sodium citrate), and dPKBH were optimized. For V analysis, sample (pH 4.5) was obtained using acetic acid/sodium acetate buffer, and masking agents were ammonium fluoride and 1,2-cyclohexanediaminetetraacetic acid. Under optimal conditions, both methods were applied to the analysis of certified reference materials TMDA-62 (lake water), LGC-6016 (estuarine water), and LGC-6019 (river water). In all cases, results proved the accuracy of the method. CI - Copyright (c) 2015 Elsevier Inc. All rights reserved. FAU - Albendin, Gemma AU - Albendin G AD - Laboratory of Toxicology Faculty of Marine and Environmental Sciences, Universidad de Cadiz, Cadiz 11510, Spain. FAU - Lopez-Lopez, Jose A AU - Lopez-Lopez JA AD - Department of Analytical Chemistry, Faculty of Marine and Environmenal Sciences, Universidad de Cadiz, Cadiz 11510, Spain. Electronic address: joseantonio.lopezlopez@uca.es. FAU - Pinto, Juan J AU - Pinto JJ AD - Department of Analytical Chemistry, Faculty of Marine and Environmenal Sciences, Universidad de Cadiz, Cadiz 11510, Spain. LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20151223 PL - United States TA - Anal Biochem JT - Analytical biochemistry JID - 0370535 RN - 0 (Hydrazones) RN - 0 (Indicators and Reagents) RN - 00J9J9XKDE (Vanadium) RN - 789U1901C5 (Copper) SB - IM MH - Copper/*analysis MH - Environmental Monitoring/methods MH - Fresh Water/*analysis MH - Hydrazones/chemistry MH - Indicators and Reagents MH - Spectrophotometry, Ultraviolet/*methods MH - Vanadium/*analysis OTO - NOTNLM OT - Box-Behnken OT - Cu OT - Microanalysis OT - Trace metals OT - V OT - dPKBH EDAT- 2016/01/03 06:00 MHDA- 2016/11/02 06:00 CRDT- 2016/01/03 06:00 PHST- 2015/07/16 00:00 [received] PHST- 2015/11/04 00:00 [revised] PHST- 2015/11/28 00:00 [accepted] PHST- 2016/01/03 06:00 [entrez] PHST- 2016/01/03 06:00 [pubmed] PHST- 2016/11/02 06:00 [medline] AID - S0003-2697(15)00570-9 [pii] AID - 10.1016/j.ab.2015.11.025 [doi] PST - ppublish SO - Anal Biochem. 2016 Mar 15;497:18-23. doi: 10.1016/j.ab.2015.11.025. Epub 2015 Dec 23.