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Research Detail

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Md. Mazharul Islam
Department of Chemistry, University of Dhaka, Dhaka-1000, Bangladesh

Robiul Islam
Department of Chemistry, University of Dhaka, Dhaka-1000, Bangladesh

Mohammad Shoeb
Department of Chemistry, University of Dhaka, Dhaka-1000, Bangladesh

Nilufar Nahar
Department of Chemistry, University of Dhaka, Dhaka-1000, Bangladesh

Bioaccumulation of organochlorine compounds in marine fish occurs as a result of environmental pollution through human activities such as industrial and agricultural waste discharged into water bodies. The main purpose of the present study is to evaluate the current status of the contamination level of organochlorine compounds such as 4,4´-DDT, 2,4´-DDT, 4,4´-DDE and 4,4´-DDD, in the fish samples of the Bay of Bengal. A total of 25 marine fish samples of 17 species including Eleutheronema tetradactylum, Metapenaeus monoceros, Lates calcarifer, Harpodon nehereus, Pampus argenteus, Setipinna phasa, Leiognathus equulus, Tenualosa ilisha, Megalapsis cordyla, Parastromateus niger, Coilia ramcarati, Otolithoides pama, Arius maculatus, Paraplagusia bilineata, Strongylura leiura, Platycephalus indicus and Gudusia chapra were collected from three different local markets for determination of organochlorine compounds using SPD (solid phase dispersion) and QuEChERS (quick, easy, cheap, effective, rugged and safe) extraction methods, and finally analyzed by gas chromatograph equipped with electron capture detector (GC-ECD). A comparison between these two methods was also made and it was found that SPD method is more efficient for the extraction of total fat content and bioaccumulation of DDTs in fish samples compared to QuEChERS method. The percentage recovery of DDTs was found to be 65%-105%. Limit of detection LOD and Limit of Quantification LOQ was found to be 0.10 ng/g and 0.30 ng/g, respectively. The total amount of DDT was found in the range of 3.83-37.80 ng/g in SPD method and 4.51-20.40 ng/g in the QuEChERS method. All fish samples contained DDTs less than MRL (maximum residue limit) value (5 mg/kg according to the Codex Alimentarius Commission).

  Bioaccumulation, Organochlorine compounds, SPD, QuEChERS, GC-ECD, Marine fish.
  Bangladesh
  
  
  Chemical Analysis
  Marine fish

As per our ongoing research on monitoring of organochlorine pesticides in fish samples [2, 9], twenty five marine fish samples were analysed and reported here

2.1 Sampling Area Seventeen different species of marine fish samples (n = 25) were purchased randomly from three different local markets of Chittagong area near the coastal site of Bay of Bengal. Fish samples were labelled and preserved using ice and transported to laboratory. All the samples were kept at -20 °C until analysis. 2.2 Certified Chemical Reagents and Solvents Organochlorine compounds (4,4´-DDT, 2,4´-DDT, 4,4´-DDE and 4,4´-DDD) of 99% purity were purchased from Dr. Ehrenstorfer, Germany. The following analytical grade chemicals, reagents and solvents were used in this research work: anhydrous sodium sulphate (Scharlab S. L., 08181 Sentmenat Spain), silica sand (Kanto Chemical Co. Inc.), ethyl acetate (RCI Labscan Limited, USA), n-hexane (RCI Labscan Limited, USA), concentrated H2SO4 (Merck, Darmstadt, Germany), acetone (Sigma-Aldrich, France), silica gel (Merck KGaA, 64271 Dramstadt, Germany), NaCl and H2SO4 (98%) were purchased from Merck, Germany. 2.3 Extractions and Clean-up Procedures of Fish Samples Fish samples were extracted by two separate methods, i.e., SPD (solid phase dispersion) and QuEChERS (quick, easy, cheap, effective, rugged and safe). In SPD method, the muscle tissues of the fish samples were blended homogeneously. Blended sample (10.0 g) was taken into a pre-cleaned and dried mortar with silica sand (10.0 g) and anhydrous sodium sulphate (30.0 g). This powder (sample, sand and sodium sulphate) was taken in a 250 mL ground joint conical flask and extracted by shaking for 3 minutes successively with 60, 20, 20 mL ethyl acetate. The extracts were combined and filtered through anhydrous sodium sulphate. The filtrated extract was evaporated to dryness and the weight of the fatwas recorded. The solvent was exchanged from ethyl acetate to n-hexane by evaporation and the volume of the extract was adjusted up to 4 mL. From this 2 mL concentrated extract was transferred quantitatively in a graduated test tube. Clean-up was carried out through silica gel: saturated sulphuric acid (2:1 g/g) column. The extract was then concentrated to 1 mL through the nitrogen gas evaporator. Then it was taken into a GC vial for injection to the GC-ECD. In QuEChERS method, 10 g homogenized blended marine fish sample was taken in a 50 mL tefl on centrifuge tube. And 20 mL ethyl acetate was added to it and shaken by hand for 1 minute and vortexed for about 2 minutes. Anhydrous magnesium sulphate (6.0 g) and sodium chloride (1.5 g) were added and the mixture was again vortexed for 1 minute followed by centrifugation (4,000 rpm for 5 minutes). The supernatant was taken into a clean, dried and pre-weighed round bottom flask and the solvent was evaporated (below 40 °C) to dryness by rotary vacuum evaporator. Then, the weight of total fat content was recorded. The solvent was exchanged from ethyl acetate to n-hexane by evaporation and the volume of the extract was adjusted up to 4 mL. From this 2 mL concentrated extract was transferred quantitatively in a graduated test tube. Then, 2 mL saturated H2SO4 was added and shaken for 1 minute. Then the mixture was centrifuged for 10 minutes. The supernatant was taken using a pasture pipette, kept into GC vial and analyzed by GC-ECD. 2.4 LOD, LOQ and Recovery Experiment At first, 100 mg/L primary standard solution was prepared by diluting proper amount of DDTs (99% purity) in n-hexane and serially diluted to the different concentrated solution like 0.2, 0.1, 0.05, 0.02, 0.01, 0.005, 0.002, 0.001 and 0.0005 mg/kg. The limit of detection (LOD) was determined by injecting serially diluted mixtures of standard DDTs solution in GC-ECD. For LOD, the peak area of each standard was considered 3 times higher than the baseline noise, i.e., signal to noise ratio was 3:1. LODs for DDT, DDE and DDD were found to be 0.10 ng/g. The LOQ is the minimum concentration that can be quantified at a specified level of precision or accuracy (or both). For LOQ, the peak area of each standard was considered 10 times higher than the baseline noise, i.e., signal to noise ratio was 10:1 and LOQ for fish samples DDTs residue analysis 0.30 ng/g.

  Journal of Food Science and Engineering 8 (2018) 78-85
  doi: 10.17265/2159-5828/2018.01.004
Funding Source:
1.   Budget:  
  

The present study compared the efficiency between two methods, i.e., SPD and QuEChERS for the extraction of organochlorine compounds from marine fish samples, and SPD method was found more efficient than QuEChERS method. For most of the samples, the level of DDTs was found below the MRL value analyzed by both methods. But excess intake of contaminated fishes may impose a health risk factor, especially fishers and coastal communities who may eat fishes every day. Again, the ratio of 4,4´-DDT/∑DDTs was in the range of 0.06-0.45 which implies that the exposure of DDT is not for recent or ongoing use. The present research recommends that the sources of DDTs in the vicinity of the Bay of Bengal should be strictly monitored for protecting the contamination of marine ecosystem along with the fish community.

  Journal
  


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