Broad Spectrum Analysis of 109 Priority Compounds Listed in the 76/464/CEE Council Directive Using Solid-Phase Extraction and GC/EI/MS

Abstract

A single multiresidue method was developed to determine 109 priority organic compounds included in the 76/464/EEC Council Directive on Pollution of the European Union. Such Directive includes 132 priority pollutants with a broad spectrum of polarities to be analyzed in drinking and surface waters, with the aim to protect water quality. From this list, the compounds analyzed included benzidines, chloroanilines, chloronitrobenzenes, chloronitrotoluenes, chlorophenols, chloronitrotoluidines, PAHs, PCBs, pesticides, phenylurea, and triazine herbicides. The method was developed in four steps. First, automated off-line solid-phase extraction using polymeric sorbent Oasis 60 mg cartridges was optimized to trap 109 compounds. Second, gas chromatography coupled to mass spectrometry with electron impact ionization (GC/EI/MS) was used in selected ion monitoring (SIM) mode for tentative identification of target analytes. Third, GC/EI/MS under full scan conditions was used for spectrum identification and analyte confirmation. Last, quantification was performed from SIM chromatogram using surrogates and internal standard. This method offered excellent sensitivity and selectivity, and the preconcentration of 200 mL permitted the achievement of limits of detection at the low nanogram/liter level and recoveries between 70 and 120%. Such methodology was applied to determine 109 organic compounds in French surface waters, and several pollutants were detected at levels from ppt to ppb. This multiresidue method developed was highly reproducible and robust and permitted a high sample throughput.

Evaluation of occurrence of NO3–, Coliform and atrazine in a karst aquifer, Colombo, PR

“…The atrazine was analyzed following the procedure of Lacorte et al (2000), that consists on the extractions with ethyl acetate and further dilution to quantifying on Gas Chromatograph coupled with an Mass Spectrogram (Varian CG and MS 220), equipped with a capillary column of VF 1 ms (30 meters of length × 0.25 millimeters of intern diameter × 25 millimeters of thickness of film). The CG-MS was programmed to 70 °C for 4 minutes, heathen to 280°C during 52.5 minutes, reaching 4 °C min -1…”

Determinação de herbicidas usados no cultivo de arroz irrigado na região sul do estado de Santa Catarina através da SPME-GC-ECD

“…São considerados produtos de mediana a extremamente tóxicos, sendo muito perigosos para o ambiente, tendo seus limites máximos para água de consumo humano estabelecido pela legislação brasileira em 2 μg L -1 para atrazina e 20 μg L -1 para alaclor e propanil. A determinação destes compostos em matrizes ambientais, de maneira geral, exige o uso de métodos de preparação de amostras seletivos para uma determinada classe de compostos e que envolvem etapas de extração, limpeza e pré-concentração anteriores à determinação cromatográfica 6 .…”

“…São considerados produtos de mediana a extremamente tóxicos, sendo muito perigosos para o ambiente, tendo seus limites máximos para água de consumo humano estabelecido pela legislação brasileira em 2 μg L -1 para atrazina e 20 μg L -1 para alaclor e propanil. A determinação destes compostos em matrizes ambientais, de maneira geral, exige o uso de métodos de preparação de amostras seletivos para uma determinada classe de compostos e que envolvem etapas de extração, limpeza e pré-concentração anteriores à determinação cromatográfica 6 .A extração líquido-líquido é um procedimento de preparo de amostras que consome um volume significativo de solventes orgâ-nicos, longo tempo de extração e intenso trabalho do analista. A técnica de extração em fase sólida, apesar de utilizar pequenas quantidades de solvente para eluir os analitos do sorvente, apresenta problemas de entupimento do sistema de extração e usa grandes volumes de amostra 7 .…”

Multiresidue determination of herbicides in environmental waters from Primavera do Leste Region (Middle West of Brazil) by SPE-GC-NPD

“…Lower recoveries of DIA and trifluralin have been reported in the literature. 9,[14][15][16] Many authors have described methods for the determination of these herbicides in water using gas chromatography with nitrogen phosphorus detection or mass spectrometric detector or ultraviolet or mass selective detector through different interfaces for HPLC technique, Table 4. In terms of recovery the effectiveness of the C 18 cartridge extraction procedure was compared with those obtained using SDVB resins and GCB sorbent.…”