Organochlorine Pesticides In Milk Research Articles

Au@Ag nanoflowers based SERS coupled chemometric algorithms for determination of organochlorine pesticides in milk

In this study, SERS coupled with chemometric algorithms like PLS (partial least square), Si-PLS (synergy interval-PLS), GA-PLS (genetic algorithm-PLS) and UVE-PLS (uninformative variable elimination-PLS) were applied for the detection of 2,4-D and imidacloprid in milk. The fabricated gold and silver core-shell nanoflowers (Au@Ag NFs) were used as SERS nanosensor which exhibited strong signal over the concentration range of 1.0 × 10−3 to 1.0 × 102 ng/mL. Performances of the models were evaluated based on the attained correlation coefficients of the prediction (Rp) and calibration (Rc), root mean square error in calibration (RMSECV) and prediction (RMSEP), and the ratio of sample standard deviation to RMSEP (RPD). The models exhibited improved results in the order of PLS < Si-PLS < GA-PLS < UVE-PLS. The UVE-PLS model showed superior performance, yielded Rc = 0.9801 and Rp = 0.9878 with RPD = 6.32 for 2,4-D, and Rc = 0.9732 and Rp = 0.9726 with RPD = 4.30 for imidacloprid. The strategy could be employed for safety and quality monitoring of milk.

Organochlorine pesticide residues in raw milk samples collected from dairy farms and urban areas of Lahore district, Pakistan.

The current study was employed to investigate the organochlorine pesticides (OCP) concentrations in milk, as the milk we consume, has residues of these notorious pesticides. The residual concentrations of OCP in milk have numerous harmful effects on health especially the children. Therefore, milk was analyzed using gas chromatography equipped with µECD for seven OCP residues, namely α-endosulfan, β-endosulfan, Endosulfan-sulphate, DDE, γ-HCH, Dieldrin, and DDT. Three hundred and sixty raw milk samples were collected from urban areas (10 areas of Lahore N = 300) and Dairy Farms (10 farms in Lahore N = 60) from September 2012 to September 2013. Samples were collected after an interval of 2months, for 12months. Mean values of OCPs in milk samples from urban areas were reported as α-endosulfan, β-endosulfan, Endosulfan-sulphate, DDE, γ-HCH, and Dieldrin with concentration of 17.44 ± 3.99, 35.74 ± 7.50, 20.28 ± 3.95, 2.51 ± 0.55, 0.93 ± 0.16 and 1.12 ± 0.18µgkg-1, respectively, while the milk samples from dairy farms with concentration of 26.94 ± 4.63, 59.88 ± 6.76, 32.07 ± 4.51, 4.64 ± 0.48, 1.20 ± 0.17 and 1.93 ± 0.18µgkg-1, respectively. None of the samples analyzed were found positive for the presence of DDT, just as none of the samples from area milk shops exceeded the Maximum Residual Limits (MRLs). γ-HCH and β-endosulfan were found higher in dairy farm milk samples than the MRLs. Conclusively, these pesticide residues are present in milk available in Lahore in enough quantity (some exceeding the MRLs) to threaten human health, particularly the infant and children.

Distribution and Fate of Persistent Organochlorine Pesticides on the Soil-Forage-Milk Chain in Three Transylvanian Farms

The present work follows the distribution and fate of persistent organochlorine pesticides on the soil-forage-milk chain in three Transylvanian farms. In order to achieve this goal, a new, rapid and affordable analytical method for the quantifications of organochlorine pesticides in milk samples was developed. The tracing of the persistent organochlorine pesticides in soil and milk was performed for each farm separately. On Farm 1, aldrin was identified to be the pesticide traced from soil to milk, while on Farm 2 and Farm 3, delta-benzene hexachloride (δ-BHC) was the dominant pesticide. All of the determined pesticide concentrations for the milk samples were found to be under the maximum residue limits for pesticides (MRLs) established for milk by the European Union (EU).

Risk profile and health vulnerability of female workers who pick cotton by organanochlorine pesticides from southern Punjab, Pakistan

The present study was conducted to highlight the existing level of organochlorine-pesticides (OCPs) from human milk (n = 45) and blood serum (n = 40) of female workers who pick cotton in Khanewal District, southern Punjab, Pakistan. Source apportionment, congener-specific analysis, and risk surveillance of OCPs are reported from human milk and blood samples. Levels of OCPs in milk and blood serum samples ranged from 15.7 ppb to 538.3 ppb and from 16.4 ppb to 747.1 ppb, respectively, and were lower than previously published reports from other regions of the globe. Congener-specific analysis revealed that DDTs were predominant, followed by hexachlorocyclohexane, chlordane, and hexachlorobenzene. Calculated results for source apportionment analysis suggested that contamination load was a new input of DDTs as well as the historic use of lindane in the study area. Levels of OCPs in milk and blood serum were significantly (p < 0.05) correlated with age, time period of picking cotton, and number of children. Health risk revealed that female workers had risk of cancer among 1 per million; however, noncarcinogenic risks were not considerable. Environ Toxicol Chem 2017;36:1193-1201. © 2016 SETAC.

Multiresidue analysis of 30 organochlorine pesticides in milk and milk powder by gel permeation chromatography-solid phase extraction-gas chromatography-tandem mass spectrometry

A method for simultaneous determination of the 30 organochlorine pesticides (OCP) in milk and milk powder samples has been developed. Prior to the gas chromatography-tandem mass spectrometric analysis, the residual OCP in samples were extracted with n-hexane and acetone mixture (1/1, vol/vol) and cleaned up by gel permeation chromatography and solid phase extraction. Selected reaction monitoring mode was used for gas chromatography-tandem mass spectrometric data acquisition to identify and quantify the OCP. To avoid the matrix effects, matrix-matched calibration solutions ranging from 2 to 50 ng/mL were used to record the calibration curve. Limits of quantification of all OCP were 0.8μg/kg. With the exception of endrin, limits of quantification are significantly lower than maximum residue limits set by the European Union and China. The average recoveries were in the range of 70.1 to 114.7% at 3 spiked concentration levels (0.8, 2.0, and 10.0μg/kg) with residual standard deviation lower than 12.9%. The developed method was successfully applied to analyze the OCP in commercial milk products.

Multiresidue Analysis of Organochlorine Pesticides in Milk, Egg and Meat by GC–ECD and Confirmation by GC–MS

A multiresidue method was developed and optimized for the quantification of organochlorine pesticides (OCPs) in milk, egg and meat samples. Sample extraction was performed by adopting QuEChERS principle and the extracts were cleaned-up dispersive solid-phase extraction with primary secondary amine after salting out with NaCl and MgSO(4). Analysis was carried out by gas chromatography coupled with electron capture detector and confirmation by gas chromatography-mass spectrometry. The performance of the method was investigated in terms of linearity, accuracy, precision, detection limit and quantification limit (LOQ). Good linearity was obtained, with correlation coefficients (r(2)) higher than 0.992. Mean recoveries were found in the ranges 72%-108%, 74%-101% and 75.27%-104.56% for the milk, egg and meat, respectively, RSD % turned out to range from 0.28% to 10.05%. The method developed was successfully tested on commercial milk, egg, and meat samples from the markets of Tamil Nadu (India), proving to be a useful tool in routine analysis of OCPs for monitoring purposes. None of the compounds of interest were observed above their respective LOQ.

Organochlorine pesticide residues in cows’ milk from Karlovac County, Croatia

The aim of this study was to determine the residue levels of the organochlorine pesticides in cows’ milk from Karlovac County, Croatia. The study included 48 pooled milk samples: 40 pooled samples of non-processed (raw) milk and 8 pooled samples of processed milk collected in the Karlovac County from May 2003 until April 2004. Organochlorine pesticides DDT and derivates, HCH, lindane, heptachlor and endosulfan were determined using the GC-ECD method. The detection limit was 0.01 μg kg −1 . The determined amounts of organochlorine pesticides were predominantly and significantly below the Maximum Residue Limit (MRL) set by the European Union and which Croatia has also recently adopted as its standard. The study has confirmed pesticide persistence in milk samples from our country despite the fact that some of them have been banned some thirty years ago, which indicates a high degree of dispersion of this substances in the environment. Taking into account that milk is a foodstuff of high biological value consumed frequently and in large quantities by vulnerable groups of population (children, pregnant women, elderly people), the continued monitoring and control of organochlorine pesticides in milk is therefore of great importance for public health.

A method to determine residue levels of persistent organochlorine pesticides in human milk from Indonesian women.

A method has been developed for the analysis of organochlorine pesticides in human milk using solvent extraction, Florisil solid phase extraction clean-up and analysis by gas chromatography with an electron capture detector. The recovery of analytes from spiked milk samples was in the range 53 +/- 1% to 109 +/- 7% (n = 9). A small number of samples were obtained from women in a rural and an urban area of Indonesia and analysed using the developed method. The results are reported on a milk fat basis. All samples contained detectable residues of p,p'-DDT (urban mean 0.11 +/- 0.18 mgkg(-1) (n = 5), rural mean 0.07 +/- 0.03 mg kg(-1) (n = 5)) and p,p'-DDE (urban mean 0.05 +/- 0.04 m kg(-1) (n = 5), rural mean 0.76 +/- 1.46 mg kg(-1) (n = 5)). Residues of HCB, betaHCH, alpha-endosulfan and dieldrin were also detected in some samples. There was no significant difference (at the 95% confidence level) in levels of pesticides between urban and rural areas. The levels of organochlorine pesticides in milk from Indonesian women were lower than those reported from Indonesian women exposed to DDT through malaria eradication schemes and were similar to levels reported from UK and Japan.

Assessment of risk to public health posed by persistent organochlorine pesticide residues in milk and milk products in Mumbai, India

The risk posed by the presence of organochlorine pesticides in milk and milk products was estimated for the population of Mumbai. To determine the levels of organochlorine pesticides in milk and milk products, a monitoring study was carried out in and around Mumbai City. 520 samples of milk and milk products of different brands were considered in this study. A survey was also conducted to determine the mean daily consumption of milk and milk products by different age groups and this data was used to evaluate the daily exposure to the public. Non-cancer effects were evaluated by comparing the predicted exposure distributions to the published guidance values. For chemicals identified as potential human carcinogens, cancer risk was evaluated using standard methodology. The majority of the chlorinated pesticides identified in the milk and milk product samples studied were found to be at levels which do not pose unacceptable risks to the public, with the exception of alpha-HCH. The cancer risk estimated for this chemical slightly exceeds the US EPA guidance value.

Determination of Organochlorine Pesticides in Milk by Electron Capture Capillary Gas Chromatography

AbstractThe goal of this study was to develop an analytical method to determine the organochlorine pesticides residues in milk. The samples were loaded onto the self‐packed diatomaceous earth columns, then eluted with 25 mL solvent mixture of n‐hexane‐acetone‐ethyl acetate (4+2+1, v/v/v). After collection and concentration, the extracts were cleaned up by the C18 solid‐phase extraction cartridges. Gas chromatograph/electron capture detector was used for determination. The average recoveries of milk which were spiked with 10 ng/mL of α‐BHC, lindane, heptachlor, dieldrin, p,p'‐DDD, and p,p'‐DDT were above 92%. Limits of detection between 0.5‐1.8 ng/mL were achieved.

Rapid method for the determination of organochlorine pesticides in milk

This method involved one step extraction of milk with acetate—acetone—methanol by ultrasonication. The supernatants were further cleaned-up and enriched by solid-phase extraction using octadecyl (C 18)-bonded silica catridges, then assayed by capillary gas—liquid chromatography with electron capture detection. The recoveries of eleven organochlorine pesticides (OCPs) from raw milks were quantitative, ranging from 90–110% at 10 times the limit of detection (LOD). The LOD ranged form 0.5 μ/l whole milk for α-hexachlorocyclohexane to 2.5 μg/l whole milk for 1,1,1-trichloro-2,2-bis( p-chlorophenyl)ethane. The day day-to-day variation of the method was evaluated over 7 days using 3 different pools of spiked cow miles (at the LOD, 5 and 10 times the LOD). The coefficient of variations (C.V.s) were 16±6, 10±2 and 9±3% (means S.D.), respectively. The method showed no emulsion problems common with conventional non-polar solvent extraction, and the use of solid-phase extraction considerably reduced the sample clean-up process compared with the existing method. The method also showed that OCPs in milk could be extracted quantitatively without extraction of total fat, and that OCPs spiked into cows milk could be used to construct calibration curves for human milk determinations.

Polychlorinated biphenyls and organochlorine pesticides in milk of Norwegian women during lactation

Milk samples of 14 women were analyzed for PCBs (polychlorinated biphenyls), p,p'-DDE, and HCB (hexachlorobenzene) during 11 intervals of a 120 day-lactation period. A general downward trend in residue levels was evident, and a statistically significant decline was observed for residue levels of PCBs (P less than 0.01) and HCB (P = 0.02) on the milk fat basis. Primipara (n = 9) had from 1.5 to 2.1 times higher mean residue levels than mothers nursing their second or third child (n = 9). Significant declines in residue levels during lactation of the first child were found, while no pronounced changes in residue levels were observed during lactation of the second or third child. Overall, residue levels in this study were lower than corresponding levels found earlier in Norway, and within the range of the corresponding levels found in another Norwegian human milk survey done at the same time.

Polychlorinated biphenyls and organochlorine pesticides in milk and blood of Canadian women during lactation.

Blood and breast milk samples of 16 women were analyzed for PCBs (polychlorinated biphenyls) and some organochlorine pesticides during eight intervals of a 98 day lactation period. Although a general downward trend in residue levels of blood and breast milk was evident, this trend was interrupted by sporadic increases. Most residues in breast milk showed an apparent increase during the first 30 days of lactation, which was not statistically significant. However, during lactation a statistically significant decrease was observed for the following residues, expressed on a milkfat basis: HCB (hexachlorobenzene), oxychlordane, transnonachlor (1-exo, 2-endo, 3-exo-4,5,6,7,8,8-nonachloro-3a,4,7,7a-tetrahydro-4,7-methanoindene), βHCH (hexachlorocyclohexane),p,p′-DDE andp,p′-DDT. Average milk/blood ratios for PCBs, HCB, oxychlordane(1-exo,2-endo-4,5,6,7,8,8-oc-tachloro-2,3-exo-epoxy 2,3,3a,4,7,7a-hexa-hydro-4,7-methanoindene),p,p′-DDE (2,2-bis-(p-chlorophenyl)- 1, 1-dichloroethylene), dieldrin (1,2,3,4, 10,10-hexachloro-exo-6,7-epoxy-1,4,4a,5,6,7,8,8a-octahydro- 1,4-endo- exo- 5,8-dimethanonaphthalene) and p,p′-DDT (1,l-bis-(p-chlorophenyl)-2,2,2-trichloroethane) levels were 23, 20, 9, 19, 5 and 30 respectively. Milk/blood ratios for PCB andp,p′-DDE levels remained relatively constant during lactation (coefficient of variation ∼20). Accumulation of residues in infant body fat were theoretically estimated

Pesticide Pollution in India: Organochlorine Pesticides in Milk of Woman, Buffalo, and Goat

As an index of pesticide pollution in breast feeding by Indian mothers, milks of woman, buffalo, and goat were analyzed to estimate residues of organochlorine pesticides by gas liquid chromatograph equipped with electron capture detector. Contamination in human milk was high as compared with buffalo and goat. Concentration of dichlorodiphenyl trichloroethane in human milk was 12 times higher than that of buffalo milk and 13 times higher than that of goat milk. Residues of hexachlorocyclohexane were correspondingly high in human milk.

Column switching techniques in the liquid chromatographic analysis of organochlorine pesticides in milk

A system is described for the analysis of organochlorine pesticides in milk by high-performance liquid chromatography. Sample clean-up, separation of pesticides from milk fat and quantification of both fat and pesticides are carried out on-column using column switching and backflushing techniques. The combination of liquid chromatography with electron-capture detection results in a detection limit of ∼ 0.1 ppm pesticide in milk fat.

Pesticide residues in foodstuffs in Great Britain. II. Persistent organochlorine pesticide residues in selected foods.

AbstractResidue measurements for persistent organochlorine pesticides in milk, butter, corned beef, beef fat and mutton fat, produced in or imported into Britain in 1963 and 1964 are reported. The levels in mutton fat are compared with levels found earlier; only very low residues are found in most other produce examined though some butter samples contain up to 0·1 ppm of DDT and 0·4 ppm of total DDT equivalent. Levels in the fat of grass and store‐fed animals were indistinguishable; results for milk suggest that the diet of cows in Britain contains very little γ‐BHC or dieldrin.