scholarly journals Optimized Multiresidue Analysis of Organic Contaminants of Priority Concern in a Daily Consumed Fish (Grass Carp)

2017 ◽  
Vol 2017 ◽  
pp. 1-13 ◽  
Author(s):  
Wei He ◽  
Yanru Chen ◽  
Chen Yang ◽  
Wenxiu Liu ◽  
Xiangzhen Kong ◽  
...  

The organic contaminants, including polycyclic aromatic hydrocarbons (PAHs), organochlorine pesticides (OCPs), polybrominated diphenyl ethers (PBDEs), and polychlorinated biphenyls (PCBs), are of priority concern because of their persistence, toxicity, and long-distance transportation in global environment. Their residues in a daily consumed fish (grass carp) pose potential threat to human health and aquatic ecosystems. The present study optimized an analytical protocol of microwave-assisted extraction (MAE), lip-removal by gel permeation chromatography (GPC), cleanup by solid phase cartridge (SC) or adsorption chromatography column (CC), and gas chromatography-mass spectrometry (GC/MS). Besides traditional statistical parameters, some indicators were calculated to judge the performances of extraction by various methods. The optimization experiment showed that n-hexane/acetone was the best MEA extraction solvent; an optimal fraction time of 10–39 min could simultaneously elute all the target chemicals in a single GPC run. Both CC and SC showed good recoveries. However, CC performed better than SC (p<0.05) for OCPs, and SC performed better than CC for PBDEs (p<0.05). We also emphasized the limitations and advantages of SC and CC and finally proposed SC as the promising cleanup method because of its low-cost materials, time-saving steps, being free of manual filling, and operation by automated SPE system.

2013 ◽  
Vol 781-784 ◽  
pp. 1852-1855 ◽  
Author(s):  
Wen Zheng Shi ◽  
Qing Yun Chen ◽  
Xi Chang Wang ◽  
Jin Qing Wan

In this paper, the dorsal meat of grass carp was used as research object. The volatile compounds of grass carp were extracted and concentrated by headspace solid phase micro-extraction (HS-SPME). Then the volatiles were identified by gas chromatography-mass spectrometry (GC-MS). The results showed that SPME-GC-MS was effective to analysis of the volatiles in grass carp meat. According to GC-MS, 42 volatile compounds were detected in dorsal meat of grass carp. The volatile components are mostly carbonyl compounds and alcohols, and the relative contents are 95.74%. The method of odor activity value was applied to determine predominant volatile components of grass carp. There are 12 predominant components were determined in dorsal meat of grass carp, including: 1-Octen-3-ol, 2,6-Nonadienal, Nonanal, (E,E)-2,4-Decadienal, (E,Z)-2,4-Decadienal, Hexanal, 2-Nonenal, Octanal, 2-Decenal, Heptanal, Heptanol and 2-Octenal etc. The study will enrich the theoretical knowledge of flavor chemistry .


2014 ◽  
Vol 97 (4) ◽  
pp. 978-986 ◽  
Author(s):  
Ramón Aznar ◽  
Beatriz Albero ◽  
Consuelo Sánchez-Brunete ◽  
Esther Miguel ◽  
José L Tadeo

Abstract An analytical method was developed for the simultaneous determination in poultry manure of 41 organic contaminants belonging to different chemical classes: pesticides, polycyclic aromatic hydrocarbons, polychlorinated biphenyls, and polybrominated diphenyl ethers. Poultry manure was extracted with a modified QuEChERS method, and the extracts were analyzed by isotope dilution GC/MS. Recovery of these contaminants from samples spiked at levels ranging from 25 to 100 ng/g was satisfactory for all the compounds. The developed procedure provided LODs from 0.8 to 9.6 ng/g. The analysis of poultry manure samples collected on different farms confirmed the presence of some of the studied contaminants. Pyrethroids and polycyclic aromatic hydrocarbons were the main contaminants detected. DDT and its metabolite DDE were also found but at relatively low concentrations.


2004 ◽  
Vol 87 (4) ◽  
pp. 1021-1027 ◽  
Author(s):  
Ana Gago-Martínez ◽  
María J Nogueiras ◽  
Sandra Rellán ◽  
Juan Prado ◽  
María F Alpendurada ◽  
...  

Abstract In this work, solid-phase microextraction (SPME) has been applied as an alternative for the selective extraction of 3 polybrominated diphenyl ethers (PBDEs), 2,2′,4,4′-tetrabromodiphenyl ether (PBDE-47); 2,2′,4,4′,5-pentabromodiphenyl ether (PBDE-99); and 2,2′,4,4′,6-pentabromodiphenyl ether (PBDE-100), and 2 alkylphenols, 4-tert-OP and 4-NP, prior to their analysis by gas chromatography/mass spectrometry (GC/MS). The advantages of this technique are mainly its simplicity, cost-effectiveness, and time-saving sample preparation, as well as being a solvent-free technique. With the aim of optimizing the conditions for an efficient extraction of the studied compounds, different fiber coatings and the main parameters affecting the extraction procedure have been evaluated. The results obtained showed a good linearity in the range of concentrations investigated, and adequate relative standard deviation values were found according to the range accepted for SPME. Recovery values were in the range of 78–108%, and good detection and quantitation limits at ppt levels were obtained for both methods, allowing the determination of the selected compounds in samples at trace levels. The results obtained clearly show the potential of SPME for efficient concentration of the target compounds and also demonstrate the reliability of this extraction technique for their GC/MS analysis.


2003 ◽  
Vol 38 (4) ◽  
pp. 667-682 ◽  
Author(s):  
Hing-Biu Lee ◽  
Kurtis Sarafin ◽  
Thomas E. Peart ◽  
M. Lewina Svoboda

Abstract A gas chromatography/mass spectrometry (GC/MS) method for the determination of 11 selected acidic pharmaceuticals in sewage influent and effluent at trace levels has been developed. The drugs studied were salicylic acid, clofibric acid, ibuprofen, acetaminophen, gemfibrozil, fenoprofen, naproxen, ketoprofen, diclofenac, fenofibrate, and indomethacin, which are commonly used as analgesic/anti-inflammatory agents or lipid regulators. The antibacterial agent triclosan was also included in this study. A solid-phase extraction procedure using the Waters Oasis HLB (hydrophilic-lipophilic balance) cartridge was optimized for the extraction and elution of these compounds. The acids were then converted into their trimethylsilyl (TMS) derivatives. Final analysis was performed with a Mass Selective Detector in the EI/SIM (electron impact/selected ion monitoring) mode. Recoveries of the drugs in spiked distilled water samples at 1 and 0.1 μ/L levels were better than 80%. Similar recoveries of the drugs were obtained from fortified final effluent samples except for acetaminophen, which could not be recovered even if the extraction was performed immediately. The detection limits for the drugs, based on a concentration factor of 1000, were between 10 and 20 ng/L. A stability study indicated that, except for salicylic acid and acetaminophen, the other acidic pharmaceuticals were better than 75% recovered after the samples had been stored at 4°C in the dark for up to seven days. This method has been applied to quantify acidic drugs in wastewater samples collected from several sewage treatment plants in Ontario. While clofibric acid, acetaminophen, fenoprofen, and fenofibrate have never been detected, the other eight compounds were found in nearly all the influent and effluent samples, from low μ/L to low ng/L levels. Eight sewage treatment plants removed from 0 to 98% of these drugs from the influent.


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