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Abstract

The procedure for simultaneous extraction from soil and determination by means of GC-ECD insecticides: aldrin, dieldrin, endrin and herbicide: atrazine was worked out. The proposed GC-ECD technique provides limits of detection in range 12 μg/mL - 18 μg/mL and 2 μg/mL, for insecticides and atrazine, respectively. Two different types of extraction: microwave assisted extraction (MAE) and ultrasound assisted extraction (UAE) with different solvents were tested to choose the procedure that provides the highest recoveries of analytes and low detection limits, typical for trace analysis (100 ppm or 100 mg/g, IUPAC). On the basis of recoveries and precision both extraction methods were compared. The insecticides recovery from soil samples obtained by UAE were in range 40-85%, coefficient of variation (CV): 1.3-5.0%, whereas for atrazine recovery was below 15% (CV: 8-18%). The most efficient and precise extraction procedure turned out to be MAE with n-hexane: acetone. The recoveries were in range 70-85% for insecticides and 84% for atrazine, CV: 0.4-2.2% and 5.3% for insecticides and atrazine, respectively. The presented MAE-GC-ECD procedure enables extraction and determination of aldrin, dieldrin, endrin and atrazine in soil samples with high recoveries, precision and limits of detections in range 6 ng/g - 8 ng/g in the case of insecticides and 1.5 ng/g for atrazine.

The MAE-GC-ECD procedure was applied for the above mentioned pesticides determination in environmental samples. Soils were collected in agricultural as well as rural areas in Poland. In all cases atrazine was determined in concentration range: 0.0187 mg/g - 0.1107 mg/g. Aldrin and dieldrin was detected in soil samples from two locations.

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Authors and Affiliations

Marianna Czaplicka
Hanna Barchańska
Anna Giemza
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Abstract

Tannic acid or tannin, type of phenolic compound contains in kenaf bast fibre. Conventional extraction has certain limitations in terms of time, energy, and solvent consumption. Ultrasound assisted extraction (UAE) can extract bioactive components in shorter time, low temperature, with lesser energy and solvent requirement. UAE as alternative extraction technique is better equipped to retain the functionality of the bioactive compounds. In this study, the conditions for ultrasound assisted extraction (UAE) of tannic acid from kenaf bast fibre by assessing the effect of sonication time and different duty cycles were optimized. The use of ultrasound to extract tannic acid from kenaf bast fiber was evaluated. Ultrasound-assisted extraction (UAE) was carried out using ethanol as solvent to intensify the extraction efficacy. Phytochemical screening was conducted to identify the presence of tannic acid in extracts. The extracts then were analyzed using High-Performance Liquid Chromatography (HPLC) and Scanning Electron Microscopy (SEM). It was found that 0.2429 mg/mL of tannic acid was obtained under the extraction conditions of extraction temperature of 40℃, sonication time of 20 minutes and duty cycle of 50%. From SEM analysis, it was found that the raw sample demonstrated rough surface and no porous but kenaf bast fibre display smoother surface with less impurities and few pores appeared after the extraction process using UAE. These results indicate that ultrasound-assisted extraction is an efficient method for extracting tannic acid from kenaf bast fibre with the advantages of lower extraction time and higher extraction yield.
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Authors and Affiliations

M. Mohamad
1
ORCID: ORCID
H.A. Ibrahim
1
M.F.M. Nasir
2
N.A. Mohidem
3
ORCID: ORCID
N.F. Shoparwe
1
P.T. Teo
1
ORCID: ORCID
M.N. Masri
1
ORCID: ORCID
A.R. Irfan
4 5
ORCID: ORCID

  1. Universiti Malaysia Kelantan, Faculty of Bioengineering and Technology, Jeli Campus, Kelantan, Malaysia
  2. National Kenaf and Tobacco Board, Kubang Kerian, Kelantan, Malaysia
  3. Universiti Putra Malaysia, Faculty of Engineering Selangor, Department of Biological and Agricultural Engineering, Malaysia
  4. Universiti Malaysia Perlis, Faculty of Mechanical Engineering Technology, Perlis, Malaysia
  5. Universiti Malaysia Perlis, Center of Excellence Geopolymer and Green Technology (CEGeoGTech), Perlis, Malaysia

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