scholarly journals Analytical methods for the determination of common booster biocides in marine samples

2012 ◽  
Vol 10 (3) ◽  
pp. 521-533 ◽  
Author(s):  
Álvaro Sánchez-Rodríguez ◽  
Zoraida Sosa-Ferrera ◽  
José Santana-Rodríguez

AbstractBooster biocides are organic compounds that are added to antifouling copper-based paints to improve their efficacy. Due to their widespread use, they are common pollutants of marine ecosystems. Some of these compounds show acute and chronic toxic effects in non-targeted organisms at concentrations as low as ng L−1. The determination of these compounds is therefore important, and for some, which are prioritized in the EU water framework directive, a necessity. Because of their low concentrations and the matrix effect, these contaminants often require a suitable sample preparation step (extraction/pre-concentration) prior to chromatographic determination. The aim of the present article is to review extraction and chromatographic methodologies related to the determination of common booster biocides in marine samples published in the scientific literature. These methodologies include liquid-liquid extraction (LLE), solid phase extraction (SPE), solid phase microextraction (SPME), single drop microextraction (SDME), Soxhlet extraction, microwave-assisted extraction (MAE), supercritical fluid extraction (SFE) and pressurized liquid extraction (PLE) as extraction methods, and both gas and liquid chromatography as determination techniques.

Molecules ◽  
2021 ◽  
Vol 26 (7) ◽  
pp. 1837
Author(s):  
Harischandra Naik Rathod ◽  
Bheemanna Mallappa ◽  
Pallavi Malenahalli Sidramappa ◽  
Chandra Sekhara Reddy Vennapusa ◽  
Pavankumar Kamin ◽  
...  

A quick, sensitive, and reproducible analytical method for the determination of 77 multiclass pesticides and their metabolites in Capsicum and tomato by gas and liquid chromatography tandem mass spectrometry was standardized and validated. The limit of detection of 0.19 to 10.91 and limit of quantification of 0.63 to 36.34 µg·kg−1 for Capsicum and 0.10 to 9.55 µg·kg−1 (LOD) and 0.35 to 33.43 µg·kg−1 (LOQ) for tomato. The method involves extraction of sample with acetonitrile, purification by dispersive solid phase extraction using primary secondary amine and graphitized carbon black. The recoveries of all pesticides were in the range of 75 to 110% with a relative standard deviation of less than 20%. Similarly, the method precision was evaluated interms of repeatability (RSDr) and reproducibility (RSDwR) by spiking of mixed pesticides standards at 100 µg·kg−1 recorded anRSD of less than 20%. The matrix effect was acceptable and no significant variation was observed in both the matrices except for few pesticides. The estimated measurement uncertainty found acceptable for all the pesticides. This method found suitable for analysis of vegetable samples drawn from market and farm gates.


2017 ◽  
Vol 2017 ◽  
pp. 1-7 ◽  
Author(s):  
Hale Seçilmiş Canbay

Steam distillation is used to isolate scent of rose flowers. Rose aromatic water is commonly used in European cuisine and aromatherapy besides its use in cosmetic industry for its lovely scent. In this study, three different sampling techniques, liquid-liquid extraction (LLE), headspace technique (HS), and solid phase extraction (SPE), were compared for the analysis of volatile water-soluble compounds in commercial rose aromatic water. Some volatile water-soluble compounds of rose aromatic water were also analyzed by gas chromatography mass spectrometry (GCMS). In any case, it was concluded that one of the solid phase extraction methods led to higher recoveries for 2-phenylethyl alcohol (PEA) in the rose aromatic water than the liquid-liquid extraction and headspace technique. Liquid-liquid extraction method provided higher recovery ratios for citronellol, nerol, and geraniol than others. Ideal linear correlation coefficient values were observed by GCMS for quantitative analysis of volatile compounds (r2≥0.999). Optimized methods showed acceptable repeatability (RSDs < 5%) and excellent recovery (>95%). For compounds such as α-pinene, linalool, β-caryophyllene, α-humulene, methyl eugenol, and eugenol, the best recovery values were obtained with LLE and SPE.


2000 ◽  
Vol 83 (5) ◽  
pp. 1076-1081 ◽  
Author(s):  
Mara Gennari ◽  
Lucia Ferraris ◽  
Michèle Nègre ◽  
Alessandro Cignetti

Abstract Two extraction methods were developed for the determination of triasulfuron in soil. Method I included extraction with methanol–phosphate buffer at pH 7 (2 + 1, v/v), liquid–liquid partition with dichloromethane, and cleanup on a liquid chromatographic Si adsorption solid-phase extraction tube. In Method II, Extrelut was added and the sample was then extracted with acetonitrile. In both cases, the extracts were analyzed by liquid chromatography (LC) with UV detection and the LC peak was confirmed by LC/mass spectrometry (MS). The 2 methods were tested on 3 soils having different physicochemical characteristics. Method I gave 83% average recovery and a determination limit of 0.4 μg/kg soil. Method II gave 67% average recovery and a determination limit of 2 μg/kg soil. Examples of application of Method I to field samples are reported.


2012 ◽  
Vol 65 (4) ◽  
pp. 743-749 ◽  
Author(s):  
O. I. Olukunle ◽  
O. J. Okonkwo ◽  
K. K. Kefeni ◽  
M. Lupankwa

Brominated flame retardants (BFRs) are considered to be environmental pollutants due to their toxicity, persistence and ubiquity in the environment. Little information is known about the presence of brominated flame retardants in South Africa's water systems. Therefore, this study examined and compared different extraction methods (liquid–liquid (LL) vs. solid phase (SP) for water, Soxhlet extraction (SE) vs. ultrasonic for sediment) for extraction efficiencies in the determination of polybrominated diphenyl ethers (PBDEs) and polybrominated biphenyls (PBBs) in water and sediment from Jukskei River. Clean-up of sample extracts was performed using disposable Pasteur pipettes containing neutral, acidified and basic silica gel. Final extracts, after concentration and dilution to 200 μL were analyzed by injecting 1 μL in the GC-ECD and GC-MS. Results obtained showed good recoveries for most of the tested analytes in water; for LLE, values ranged between 80.5 ± 10.22% and 126.6 ± 1.94%; SPE, 70.41 ± 2.01%–124.78 ± 3.78% (n = 3) and for sediment (73–114%, with an RSD &lt;17%) using SE. The ultrasonic extraction method gave less than 50% recovery for most of the congeners. The concentrations of the BFRs in water samples were less than the detection limit while the concentrations in sediment ranged from 1.95 to 36.61 ng g−1 dry weight for Σ11 BFRs. Dichloromethane and n-hexane : acetone (2 : 1, v/v) gave optimum value of recovery for water and sediment respectively.


2004 ◽  
Vol 87 (1) ◽  
pp. 56-59 ◽  
Author(s):  
Jason A Ferrell ◽  
William K Vencill

Abstract A method was developed for determining flumioxazin in soil and water. Recovery efficiencies for solid-phase extraction (SPE) of flumioxazin from deionized, well, and surface water were between 72 and 77%. SPE was superior to liquid–liquid extraction, using water–hexane and water–chloroform emulsions, which resulted in retrieval efficiencies of 25 and 22%, respectively. However, liquid–liquid extraction with ethyl acetate improved recovery of total flumioxazin to &gt;64%. Extraction from soil samples by direct solvent/soil extraction methods recovered between 18 and 76% of applied flumioxazin, depending on the solvent combination used. However, the use of accelerated solvent extraction techniques resulted in a 106 ± 8% recovery of flumioxazin from soil. In analysis by capillary gas chromatography with mass selective detection, flumioxazin had a calculated limit of detection of 9 ng/mL with a retention time of 16.66 min.


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