Application of a quick, easy, cheap, effective, rugged and safe-based method for the simultaneous extraction of chlorophenols, alkylphenols, nitrophenols and cresols in agricultural soils, analyzed by using gas chromatography-triple quadrupole-mass spectrometry/mass spectrometry.
Due to the different physico-chemical properties of phenols, the development of a methodology for the simultaneous extraction and determination of phenolic compounds belonging to several families, such as chlorophenols (CPs), alkylphenols (APs), nitrophenols (NTPs) and cresols is difficult. This study shows the development and validation of a method for the analysis of 13 phenolic compounds (including CPs, APs, NTPs and cresols) in agricultural soils. For this purpose, a quick, easy, cheap, effective, rugged and safe (QuEChERS)-based procedure was developed, validated and applied to the analysis of real samples. A derivatization step prior to the final determination by gas chromatography (GC) coupled to a triple quadrupole analyzer operating in tandem mass spectrometry (QqQ-MS/MS) was performed by using acetic acid anhydride (AAA) and pyridine (Py). The optimized procedure was validated, obtaining average extraction recoveries in the range 69-103% (10microgkg(-1)), 65-98% (50microgkg(-1)), 76-112% (100microgkg(-1)) and 76-112% (300microgkg(-1)), with precision values (expressed as relative standard deviation, RSD)< or =22% (except for 4-chlorophenol) involving intra-day and inter-day studies. Furthermore, 15 real soil samples were analyzed by the proposed method in order to assess its applicability. Some phenolic compounds (e.g. 2,4,6-trichlorophenol or 4-tert-octylphenol) were found in the samples at trace levels (<10microgkg(-1)).
Padilla-Sánchez
Juan Antonio
JA
Department of Analytical Chemistry, University of Almeria, Spain.
Plaza-Bolaños
Patricia
P
Romero-González
Roberto
R
Garrido-Frenich
Antonia
A
Martínez Vidal
José Luis
JL
D005591:Chemical Fractionation; D004355:Drug Stability; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D010636:Phenols / Q000032:analysis*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012987:Soil / Q000737:chemistry; D012989:Soil Pollutants / Q000032:analysis*
D010636:Phenols; D012987:Soil; D012989:Soil Pollutants