Analysis Of Organochlorine Pesticide Residues Research Articles

Determination of organochlorine pesticide residues in food by polystyrene coated silica magnetic microspheres combined with gas chromatography-mass spectrometry

In this work, a sample pre-treatment technology, based on magnetite-silica-polystyrene (Fe3O4@SiO2@PS) composite as the adsorbent, combined with Gas Chromatography-Mass Spectrometry (GC–MS) has been developed and used for the trace analysis of organochlorine pesticide residues in food. SEM, TEM, FI-IR, VSM, XPS, BET, TGA and XRD techniques were used to characterize the synthetic adsorbent material, the adsorbent had excellent magnetic separation properties (saturation magnetization values with 32.7 emu g−1) and adsorption properties (adsorption capacity with 16.67 mg g−1 to 20.53 mg g−1), and the adsorption performance of Fe3O4@SiO2@PS aligned with the pseudo-second-order kinetics. Under the optimal conditions, the developed method showed satisfactory performance within a range of 0.01 to 4 mg L−1 (R2 ≥ 0.9971), the low detection limits (LOD) were from 0.05 to 0.20 μg kg−1, and the quantification limits (LOQ) were from 0.16 to 0.67 μg kg−1, respectively. The spiked recovery rates ranged from 74.7 % and 93.7 %, with relative standard deviations (RSD) from 2.09 % to 6.43 %. Thus, the developed adsorbent and method offer an efficient alternative to the commonly used SPE-based approach.

Determination of pesticide residues in beans using QuEChERS technique coupled to gas chromatography-mass spectrometry: Multivariate optimization of CEN and AOAC methods

The use of pesticides has led to environmental pollution and posed a global health risk, since they remain as residues on foods. Beans one of the most widely cultivated crop in Africa, and susceptible to attack by insects both on field and during storage, leading to the application of pesticides to control pests' infestation. However, misuse of these chemicals by farmers on beans has resulted in the rejection of beans exported to European countries, due to the presence of pesticide residues at concentrations higher than the maximum residues levels (MRLs). In this study, the effectiveness of the Association Official Analytical Chemists (AOAC) Official Method and the European Committee of Standardization (CEN) Standard Method, were determined using multivariate approach for the analysis of organochlorine pesticide residues in 6 varieties of beans samples. The significance of factors (mass of sample, volume of acetonitrile, mass of magnesium sulphate, sample pH, centrifugation time and speed) affecting the efficiency of extraction was estimated using Plackett-Burman design, while central composite design was used to optimize the significant factors. The following optimum factors were subsequently used for method validation, recovery tests, and real sample analysis: 4 g of sample sludge (1:1 v/v), 10 mL of acetonitrile, 4.45 g of MgSO4, and 5 min of centrifugation at 5000 rpm. The figure of merit of analytical methodology estimated using matrix-matched internal standard calibration method gave linearity ranging from 0.25 to 500 μg/kg, with correlation coefficient (R2) greater than 0.99, the recovery ranged from 75.55 to 110.41 (RSD = 0.70–16.65), with LOD and LOQ of 0.23–1.77 μg/kg and 0.76–5.88 μg/kg, respectively.

Analysis of organochlorine pesticide residues in bovine milk samples in Varanasi region, India

Analysis of organochlorine pesticide residues in bovine milk samples in Varanasi region, India

Analysis of organochlorine pesticides residues in fish from Edko Lake (North of Egypt) using eco-friendly method and their health implications for humans

Levels of organochlorine pesticides (OCPs) residues in tilapia fish and their health risk associated with the consumption of fish from Edko lake, Egypt were determined. The quick, easy, cheap, effective, rugged, and safe method (QuEChERS) was used for extraction and clean-up of 18 OCPs residues from fish followed by GC-ECD and GC-ITD analytical tools were employed for identification of OPs. Out of the 18 OCPs, only heptachlorepoxide, p,p-DDE, dieldrin, p,p-DDD, and endrin ketone were detected in muscles of fish with concentrations of 0.1144, 0.2119, 0.4352, 0.1196, and 0.1323 µg/Kg bw, respectively. Results of the risk assessment calculations showed that dieldrin had a health risk index of more than one. This means that there was a health risk to adults associated with the consumption of fish. On the other hand, heptachlorepoxide, p,p-DDE, p,p-DDD, and endrin ketone did not show any direct health risk. Contamination of fish, collected from Edko lake in Egypt, with residues of OCPs might pose health implications if fish were consumed fresh.

Analysis of Organochlorine Pesticide Residues in Various Vegetable Oils Collected in Chinese Markets.

Organochlorine pesticides (OCPs), chemicals frequently used in agriculture, are a group of highly toxic and persistent organic pollutants. This study assesses the distribution and congener profiles of residual OCPs in 11 types of vegetable oils collected from Chinese markets. All samples were extracted using the modified QuEChERS method prior to analysis by gas chromatography-triple quadrupole mass spectrometry. The sesame oil samples had the highest concentration of OCPs, within the range of 15.30-59.38 ng/g, whereas the peanut oil samples had the lowest OCP concentrations, within the range of 10.83-35.65 ng/g. The possible effect of the processing technology on the pesticide residues in these vegetable oils was also evaluated. It was found that the pressing method leaves more OCPs in vegetable oils than the aqueous extraction and cold-pressing, but the result for leaching was not obvious. In light of the obtained results, it was estimated that the average daily intake of different pesticides is between 0.01 and 2.20 ng/kg bw/day for urban and rural households. Hence, it can be affirmed that, given the amount of the concentration of OCPs detected in the vegetable oils collected from Chinese markets, there are no obvious health risks for urban and rural households by intake.

Study on The Use of QuEChERS Method for Analysis of Organochlorine Pesticides Residues in Cow's Milk.

QuEChERS stands for (Quick, Easy, Cheap, Effective, Rugged and Safe) and pronounced as (catchers) is a method that had been developed for multi-pesticide residue analyses in food. This study was conducted to investigate the efficacy of QuEChERS method for analyzing the organochlorine pesticides residues in cow's milk.Twenty organochlorine pesticide namely (Benzene, 1,3,5-trichloro, Tetrachlorobenzene, Benzene pentachloro. alfa-Lindane, Benzene hexachloro, Beta Lindane, Gammexane, Quintozene, Heptachlor, Aldrine, Heptachlor epoxide, Endosulfan-I , p,p'-DDE, Dieldrin , Endrin , Endosulfan-II , DDD , o,p' DDT , p,p'- DDT and Methoxychlor were examined.The linearity of the standard curve (r

Application of dispersive liquid–liquid microextraction followed by gas chromatography/mass spectrometry as effective tool for trace analysis of organochlorine pesticide residues in honey samples

A dispersive liquid–liquid microextraction (DLLME) method followed by gas chromatography/mass spectrometry (GC/MS) was applied for the trace determination of organochlorine pesticides in honey samples. The type and volume of organic extraction and disperser solvents, pH, effect of added salt content and centrifuging time and speed were optimized to find the appropriate extraction conditions. In DLLME, 30 µL of 1,2-dibromomethane (serving as extractant) and 1.5 mL of acetonitrile (serving as disperser) were applied. The limit of detection (3 s) and limit of quantification (10 s) for all the analytes of interest (organochlorine pesticides) varied from 0.004 to 0.07 and from 0.02 to 0.3 ng g−1, respectively. The extraction recovery ranged from 91 to 100 %, and the enrichment factors ranged from 171 to 199. The relative standard deviation was <6 % for intraday (n = 6) and <8 % interday (n = 4) measurements. The proposed DLLME–GC/MS method was confirmed to be fast, simple to perform, friendly to environment and suitable for analysis of organochlorine pesticide residues at trace levels in honey samples.

Analysis of organochlorine pesticide residues in human and cow’s milk in the towns of Asendabo, Serbo and Jimma in South-Western Ethiopia

The level of some OCPs in human and cow milk collected from Asendabo, Serbo and Jimma in South-West Ethiopia were analyzed using GC–ECD. Results of the analysis indicated that all samples contained detectable quantities of p,p′-DDT and its metabolites, p,p-DDE and p,p-DDD, but none of the other OCPs analyzed. Mean levels of total DDT in the human and cow milk samples in the three areas were 12.68 and 0.389μgg−1 respectively. The distributions of p,p-DDT, p,p-DDE and p,p-DDD in the human milk samples from the three locations followed the same trend in which the proportion of p,p-DDT was the highest in all the three cases, comprising 55–71% of total DDT, followed by p,p-DDE, 26–39%, and the least, p,p-DDD of 2–5%. The mean ratio of DDT/DDE concentration for the three areas was calculated to be 2.01. This value was much higher than the values reported from other countries in earlier studies and indicates the existence of a higher quantity of DDT from a fresh input in the three study areas. The mean estimated daily intake of DDT by infants from mother’s milk in the three locations was found to be 62.17μgkg−1 body weight, which is about three times higher than the acceptable daily intake set by WHO/FAO for total DDT, 20μgkg−1 of body weight. This alarmingly high daily intake value is a cause for concern, since children are highly susceptible to effects from such environmental contaminants. The study has revealed that people in the study areas are facing exposure to DDT from recent use. The observed contamination of mother’s milk and the possible transfer of the contaminant from mother to child is an obvious risk associated with breast-feeding in the study areas and possibly in other parts of the country too.

Comparison of two sample preparation methods for analysis of organochlorine pesticides residues in fish muscle

The aim of this study was to compare recoveries of organochlorine pesticides (heptachlor, α-HCH, β-HCH, γ-HCH, op′-DDD, pp′-DDD, pp′-DDE, op′-DDT, pp′-DDT) from fish muscle dried by two alternative methods: (i) grinding with anhydrous sodium sulphate and (ii) freeze drying. Pesticide residues content was determined by gas chromatography-mass spectrometry (GS-MS) method. For four pesticides (γ-HCH, α-HCH, heptachlor and pp;-DDD) in four of five fish species, higher recoveries were obtained from the freeze-dried samples. For five remaining pesticides, correlations between fish species and drying method were not found. The results of this study do not clearly indicate which drying method caused lower losses of analytes. Recoveries from the freeze-dried samples ranged from 69.9 to 117.6 %, while recoveries from the samples ground with sodium sulphate varied from 64.4 to 126.7 %. Either of the methods gave satisfactory recoveries and they both can be used interchangeably.

Serum Organochlorine Pesticide Residues and Risk of Testicular Germ Cell Carcinoma: A Population-Based Case-Control Study

Testicular germ cell carcinoma (TGCC) is the most common malignancy among men ages 20 to 34 years. Although the pathogenesis of TGCC is poorly understood, suboptimal androgen levels or impaired androgen signaling may play a role. Some persistent organochlorine pesticides commonly found in human tissue possess antiandrogenic properties. We examined whether the risk of TGCC is associated with serum levels of 11 organochlorine pesticides, including p,p'-DDE, and whether the p,p'-DDE-TGCC association is modified by CAG or GGN repeat polymorphisms in the androgen receptor gene. We conducted a population-based case-control study among 18- to 44-year-old male residents of three Washington State counties. Cases (n = 246) were diagnosed during 1999 to 2003 with a first, primary TGCC. Controls (n = 630) were men of similar age with no history of TGCC from the same population identified through random-digit telephone dialing. Questionnaires elicited information on demographic, medical, and lifestyle factors. A blood specimen provided serum for gas chromatography-high-resolution mass spectrometry analysis of organochlorine pesticide residues and DNA for genotyping. We observed no clear patterns between TGCC risk and concentrations of any of the organochlorines measured, nor did we observe that the risk associated with p,p'-DDE was modified by androgen receptor CAG (<23 versus > or =23 repeats) or GGN (<17 versus > or =17 repeats) genotype. This study does not provide support for the hypothesis that adult exposure to organochlorine pesticides is associated with risk of TGCC. Due to uncertainty regarding how well organochlorine levels measured in adulthood reflect exposures during early life, further research is needed using exposure measurements collected in utero or during infancy.

SPME and SPE comparative study for coupling with microwave-assisted micellar extraction in the analysis of organochlorine pesticides residues in seaweed samples

Solid-phase microextraction (SPME) and solid-phase extraction (SPE) procedures were coupling with microwave-assisted micellar extraction for organochlorine pesticides residues determination in seaweed samples. They were optimized, compared and discussed. Preliminary experiments were performed in order to study experimental conditions for the extraction of pesticides from spiked seaweed samples with microwave-assisted micellar extraction (MAME) using a non-ionic surfactant (Polyoxyethylene 10 Lauryl Ether). After that, SPME and SPE were used to clean-up and preconcentrate MAME extract prior the analysis by liquid chromatography with photodiode array (PDA) detection. Excellent results were obtained for both procedures. Average pesticide recoveries between 80.5 and 104.3% for MAME-SPME and between 73.9 and 111.5% for MAME-SPE were obtained. Relative standard deviations (RSDs) were lower than 10.3% and 5.3% respectively for all recoveries tested, and LOD between 138–348 ng g − 1 for MAME-SPME and 2–38 ng g − 1 for MAME-SPE were obtained. The method was validated using Soxhlet extraction procedure. Both methods were applied to analyse target organochlorine pesticides in several seaweed samples and results were compared. These results show the great possibilities of combining MAME-SPE-HPLC-UV for the analysis of seaweed samples, improving the selectivity and sensitivity in the determination of organochlorine pesticides analysis for this kind of samples.

Extraction and clean-up procedure for analysis of organochlorine pesticide residues in ethoxylated lanolin

In the present study an evaluation was made of a method for the determination of organochlorine pesticide residues in ethoxylated lanolin. Samples were homogenized with Celite, transferred to chromatographic columns, prepacked with silica gel deactivated to 10%. The pesticide elution was processed with n-hexane–dichloromethane and the concentrated eluate was analyzed using gas–liquid chromatography (GC) with electron capture detection (ECD). The composition of the elution solvent was a significant factor for the recovery of the pesticides. Mean recoveries obtained for fortified samples ranged from 87 to 94% for p, p′-DDE, dieldrin, endrin, p, p′-DDD and p, p′-DDT. Optimization of the experimental conditions resulted in a small-scale method that combines extraction and cleanup in a single step.

Supercritical fluid extraction and off-line clean-up for the analysis of organochlorine pesticide residues in garlic

An approach using supercritical fluid extraction (SFE) followed by clean-up with a AgNO 3-loaded Florisil column was utilized for the analysis of four organochlorine pesticides (OCPs) in garlic. The organic sulfur extracted by SFE from garlic was removed by AgNO 3 allowing OCPs to be determined by GC–electron-capture detection without interferences. All OCPs recoveries ranged from 85.0% to 110.0% and relative standard deviations were in the range of 3.9–7.2% for spiked samples. The described method may be used to analyze OCPs in garlic on a routine basis.

Analysis of Organochlorine Pesticide Residues Using Simultaneous Injection of Two Capillary Columns with Electron Capture and Electrolytic Conductivity Detectors

A system has been developed that will allow low level screening of 31 organochlorine pesticide residues using simultaneous injection on 2 dissimilar capillary columns. An electron capture detector was attached to a DB-1701 column, and an electrolytic conductivity detector in the halogen mode was attached to a DB-5 column. Chlorinated pesticide amounts ranging from 0.05 ng for gamma-BHC to 1.5 ng for decamethrin can easily be quantitated and confirmed. The system can be used in either the column programmed mode or the isothermal column mode. Good reproducibility was obtained for injections in both modes. This system can easily be retrofitted to any gas chromatograph using on column or split/splitless injectors.

Coupled LC‐GC: A new method for the on‐line analysis of organochlorine pesticide residues in fat

AbstractThis paper describes the use of coupled LC‐GC for the determination of organochlorine pesticide residues in fat samples. Organochlorine pesticide residues are preseparated from fat by LC on a short C‐18 column using an organic solvent as the mobile phase. Evaporation of the LC eluent is achieved by a modified on‐column interface, introducing an on‐line vaporizer module using the fully concurrent evaporation technique.

Rapid Screening Method for the Determination of Organochlorine Pesticide Residues in Wheat by Electron Capture Gas Chromatography

Abstract A rapid screening method, employing a gas chromatographic technique with electron capture detection, has been developed for t h e analysis of organochlorine pesticide residues in hard red spring wheat. Ground wheat is extracted by ball-milling with an ethyl etherhexane (3 + 97) extractant. After filtration, the extract is cleaned up on a partially deactivated Florisil column, using a single eluting system, ethyl ether-hexane (1 + 99). The eluate i s concentrated before gas chromatographic analysis. Sixteen organochlorine pesticide chemicals were recovered in excess of 80% from wheat samples fortified at 0.010 and 0.200 ppm. Organochlorine pesticide residues were recovered by the rapid method from 18 samples with field-incurred residues as efficiently as by t he Bertuzzi et al. method. Organochlorine pesticide residues were also recovered by t h e rapid method from 4 samples with field-incurred residues and from 2 wheat samples, spiked at 0.500 ppm as efficiently as by the total extraction method of Mumma et al. The rapid method offers a savings in time and solvents over.the Bertuzzi et al. method for the determination of organochlorine pesticide residues in wheat.