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Punjab College of Commerce

UCP Campus Gujranwala

Discipline: BS Chemistry

Semester: 04

Section: A

Course: Biochemistry

Course Code: CHM2741

Name: Ameera Ehsan

Roll: G1F17BSCH0002

Instructor: Prof. Muhammad Tauseef

Submission Date: 13th April, 2019

Assignment # 1

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Determination of organochlorine pesticides in marine sediments samples
using ultrasonic solvent extraction followed by GC/ECD

M.C. Vagi, A.S. Petsas, M.N. Kostopoulou, M.K. Karamanoli, T.D. Lekkas.

Original Abstract:

A rapid multiresidue method has been developed for the analysis of 17 organochlorine
pesticides (OCPs) (α-HCH, γ-HCH, β-HCH, δ-HCH, aldrin, heptachlor epoxide, endosulfan I,
4,4-DDE, dieldrin, endrin, 4,4-DDD, endosulfan II, 4,4-DDT, endrin aldehyde, endosulfan
sulfate, methoxychlor and endrin ketone) in marine sediments. The method is based on the
ultrasonic solvent extraction (USE) of sediment samples. The extraction procedure was
optimised with regard to the solvent type, amount of solvent and duration of sonication steps.
Analytical determinations of the 17 OCPs were carried out by gas chromatography using
electron capture detector (GC/ECD). The highest recoveries from sediment samples spiked at
trace concentrations of 50 ng g−1 obtained when samples were extracted two times by
ultrasonication for 20 min with 5 mL of dichloromethane. Recovery studies were performed at
1, 2, 5, 10 and 50 ng g−1 fortification levels and correlation coefficients obtained ranged from
0.9652 to 0.9993 showing that the method is linear over the range assayed. The detection limits
(signal/noise = 3) for the organochlorine compounds tested in marine sediments varied from
0.1 to 1 ng g−1 dry weight. USE of OCPs from marine sediments using dichloromethane showed
satisfactory extraction efficiencies combined with simplicity of use and low solvent
consumption.

Rewritten abstract:

An effective method for the investigation of seventeen organochlorine pesticides in aquatic


sediments involves the application of ultrasonic solvent extraction and analytical assessment
by gas chromatography using electron capture detector. The solvent type, concentration of
solvent and duration of sonication steps were varied during research. The recoveries from
samples showed minute amounts of 50 ng per gram of organochlorine pesticides in the sample.
This method is simple to use with minimum solvent required and has shown pleasing extracting
results.

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Determination of organochlorine pesticides in sediment using graphitized
carbon black solid-phase extraction and gas chromatography/mass
spectrometry

Min Sun Kim, Tae Woo Kang, Hee Soo Pyo, Jun Heon Yoon, Kyong Hee Choi,
Jong Ki Hong.

Original Abstract:

An analytical method for the determination of organochlorine pesticides (OCPs) in sediment


samples involves ultrasonic extraction, solid-phase extraction (SPE), gas-chromatography
(GC)/electron-capture detection (ECD), and GC/mass spectrometry (MS). OCPs were
extracted from sediment samples by ultrasonication in mixtures of n-hexane and acetone.
Several SPE sorbents [Florisil, silica gel, C18, Oasis HLB, and graphitized carbon black
(GCB)] were evaluated as means of preliminary purification. GCB SPE cartridges successfully
removed major contaminants such as non-polar hydrocarbons when eluted with an acetone–
acetonitrile mixture. After purification, the extract was preferentially screened using GC/ECD
and confirmed and quantified using GC/MS. The percentage recovery of samples spiked with
10 or 100 ng/g OCP ranged from 73.9% to 106.0% with a relative standard deviation of 0.4–
5.7%. Detection limits ranged from 0.002 to 0.005 ng/g for GC/ECD and from 0.03 to 0.50
ng/g for GC/MS detection. The linear dynamic range extended from 0.2 to 20 ng/g, with a
correlation coefficient (R2) greater than 0.995. The method was validated using a standard
reference material (SRM 1941b) and spiked sediment samples. Real sediment samples
collected from a river near a Korean industrial area exhibited low levels of several OCPs when
analyzed using this method.

Rewritten Abstract:

Ultrasonic extraction, solid-phase extraction, gas-chromatography/mass spectroscopy, gas-


chromatography/electron capture detection and solid phase extraction are some methods that
may be used for analysis of pesticides. Ultrasonication in mixtures of n-hexane with acetone
was applied on sample. After purification from major contaminants such as non-polar
hydrocarbons, gas-chromatography/electron-capture detection was used to assess the extract

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while gas-chromatography/mass spectrometry is used to evaluate it. 100 ng/g of organochlorine
pesticides were retrieved in sediment sample.

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