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1.
The purpose of this study was to develop a method for the determination of fluroxypyr (4-amino-3,5-dichloro-6-fluro2-pyridyloxyacetic acid) residue in palm oil namely crude palm oil (CPO) and crude palm kernel oil (CPKO). The method involves the extraction of the herbicide from the oil matrix followed by low temperature precipitation and finally quantification of the residues using the high performance liquid chromatography (HPLC). The extraction efficiency of the method was evaluated by conducting recovery studies. The recovery of fluroxypyr from the fortified CPO samples ranged from 78%-111% with the relative values for the coefficient of variation ranging from 1.4 to 8.6%. Furthermore, the recovery of fluroxypyr from the spiked CPKO samples ranged from 91-107% with the relative values for the coefficient of variation ranging from 0.6 to 4.5%. The minimum detection limit of fluroxypyr in CPO and CPKO was 0.05 microg/g. The method was used to determine fluroxypyr residues from the field-treated samples of CPO and CPKO. When fluroxypyr was used for weed control in oil palm plantations no residue was detected in CPO and CPKO irrespective of the sampling interval and the dosage applied at the recommended or double the manufacturer's recommended dosage. 相似文献
2.
Halimah M Tan YA Ismail BS 《Journal of environmental science and health. Part. B》2004,39(5-6):765-777
Four methods were developed for the analysis of fluroxypyr in soil samples from oil palm plantations. The first method involved the extraction of the herbicide with 0.05 M NaOH in methanol followed by purification using acid base partition. The concentrated material was subjected to derivatization and then cleaning process using a florisil column and finally analyzed by gas chromatography (GC) equipped with electron capture detector (ECD). By this method, the recovery of fluroxypyr from the spiked soil ranged from 70 to 104% with the minimum detection limit at 5 microg/kg. The second method involved solid liquid extraction of fluroxypyr using a horizontal shaker followed by quantification using high performance liquid chromatography (HPLC) equipped with UV detector. The recovery of fluroxypyr using this method, ranged from 80 to 120% when the soil was spiked with fluroxypyr at 0.1-0.2 microg/g soil. In the third method, the recovery of fluroxypyr was determined by solid liquid extraction using an ultrasonic bath. The recovery of fluroxypyr at spiking levels of 4-50 microg/L ranged from 88 to 98% with relative standard deviations of 3.0-5.8% with a minimum detection limit of 4 microg/kg. In the fourth method, fluroxypyr was extracted using the solid liquid extraction method followed by the cleaning up step with OASIS HLB (polyvinyl dibenzene). The recovery of fluroxypyr was between 91 and 95% with relative standard deviations of 4.2-6.2%, respectively. The limit of detection in method 4 was further improved to 1 pg/kg. When the weight of soil used was increased 4 fold, the recovery of fluroxypyr at spiking level of 1-50 microg/kg ranged from 82-107% with relative standard deviations of 0.5-4.7%. 相似文献
3.
《Journal of environmental science and health. Part. B》2013,48(5-6):765-777
Abstract Four methods were developed for the analysis of fluroxypyr in soil samples from oil palm plantations. The first method involved the extraction of the herbicide with 0.05 M NaOH in methanol followed by purification using acid base partition. The concentrated material was subjected to derivatization and then cleaning process using a florisil column and finally analyzed by gas chromatography (GC) equipped with electron capture detector (ECD). By this method, the recovery of fluroxypyr from the spiked soil ranged from 70 to 104% with the minimum detection limit at 5 µg/kg. The second method involved solid liquid extraction of fluroxypyr using a horizontal shaker followed by quantification using high performance liquid chromatography (HPLC) equipped with UV detector. The recovery of fluroxypyr using this method, ranged from 80 to 120% when the soil was spiked with fluroxypyr at 0.1–0.2 µg/g soil. In the third method, the recovery of fluroxypyr was determined by solid liquid extraction using an ultrasonic bath. The recovery of fluroxypyr at spiking levels of 4–50 µg/L ranged from 88 to 98% with relative standard deviations of 3.0–5.8% with a minimum detection limit of 4 µg/kg. In the fourth method, fluroxypyr was extracted using the solid liquid extraction method followed by the cleaning up step with OASIS® HLB (polyvinyl dibenzene). The recovery of fluroxypyr was between 91 and 95% with relative standard deviations of 4.2–6.2%, respectively. The limit of detection in method 4 was further improved to 1 µg/kg. When the weight of soil used was increased 4 fold, the recovery of fluroxypyr at spiking level of 1–50 µg/kg ranged from 82–107% with relative standard deviations of 0.5–4.7%. 相似文献
4.
Method development for determination of fluroxypyr in water 总被引:2,自引:0,他引:2
Halimah M Tan YA Aini K Ismail BS 《Journal of environmental science and health. Part. B》2003,38(4):429-440
Improved methods for extraction and clean up of fluroxypyr residue in water have been established. Two methods of fluroxypyr extraction were used, namely, Direct Measurement of fluroxypyr and Concentration of fluroxypyr onto A Solid Phase Extraction (SPE) Adsorbent, followed by elution with solvent before determination of fluroxypyr. The recovery for Direct Measurement of fluroxypyr in water containing 8-100 microg L(-1), ranged from 86 to 110% with relative standard deviation of 0.7 to 2.15%. For the second method, three types of SPE were used, viz. C18, C18 end-capped and polyvinyl dibenzene (ISOLUTE ENV+). The procedure involved concentrating the analyte from fluroxypyr-spiked water at pH 3, followed by elution of the analyte with 4 mL of acentonitrile. The recovery of fluroxypyr from the spiked sample at 1 to 50 microg L(-1) after eluting through either C18 or C18 end-capped ranged from 40-64% (with relative standard deviation of 0.7 to 2.15) and 41-65% (with standard deviation of 1.52 to 11.9). The use of ISOLUTE ENV+, gave better results than the C18, C18 end-capped or the Direct Measurement Methods. The recovery and standard deviation of fluroxypyr from spiked water using ISOLUTE ENV+ ranged from 91-102% and 2.5 to 5.3, respectively. 相似文献
5.
The method of residue analysis of kresoxim-methyl and its dissipation rate in cucumber and soil in a greenhouse were studied. Residues of kresoxim-methyl were extracted from cucumber and soil matrices with acetone, purified by liquid-liquid extraction and Florisil cartridges, and then determined by GC with NP-detector. The limit of detection was estimated to be 9 x 10-12 g, and the minimum determination concentration of kresoxim-methyl in the samples was 0.005 mg kg-1. The average recoveries ranged from 89.4 to 100.2% with a coefficient variation between 2.4 and 8.9%. Dissipation study showed that the half-lives of kresoxim-methyl in cucumber were approximately 6.5 days at both the recommended and double the recommended dosage. Half-lives for both the treatments were approximately 8 days in soil. The present study revealed that the residues in cucumber were below the MRL (0.05 mg kg-1, fixed by EU) after 7 days for both treatments. 相似文献
6.
JIAN-ZHONG LI XIAN WU JI-YE HU 《Journal of environmental science and health. Part. B》2013,48(4):427-436
The method of residue analysis of kresoxim-methyl and its dissipation rate in cucumber and soil in a greenhouse were studied. Residues of kresoxim-methyl were extracted from cucumber and soil matrices with acetone, purified by liquid-liquid extraction and Florisil cartridges, and then determined by GC with NP-detector. The limit of detection was estimated to be 9× 10?12 g, and the minimum determination concentration of kresoxim-methyl in the samples was 0.005 mg kg?1. The average recoveries ranged from 89.4 to 100.2% with a coefficient variation between 2.4 and 8.9%. Dissipation study showed that the half-lives of kresoxim-methyl in cucumber were approximately 6.5 days at both the recommended and double the recommended dosage. Half-lives for both the treatments were approximately 8 days in soil. The present study revealed that the residues in cucumber were below the MRL (0.05 mg kg?1, fixed by EU) after 7 days for both treatments. 相似文献
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8.
Transfer assessment of carbendazim residues from rapeseed to oil production determined by HPLC–MS/MS
Yinghong Li Jing Hu Zhoulin Yao Qiang Wang 《Journal of environmental science and health. Part. B》2020,55(8):726-731
AbstractIt is crucial to develop practical procedures for the control and reduction of pesticide residues in oil productions from farm to dining table. In this study, the dissipation behaviors of typical fungicide from rapeseed to oil production were studied to reveal relationship among spraying stage, application dosage, household oil processing stage, and pesticide residues. In the field trials, rape plants were sprayed with carbendazim at three different dosages during flowering period. Transfer assessment of carbendazim residues from rapeseed to oil production during household oil processing via different press techniques was determined using high-performance liquid chromatography coupled with tandem mass spectrometry (HPLC–MS/MS). The recoveries of carbendazim in rapeseed samples, meals after squeezing samples, and rapeseed oil samples ranged from 82.5% to 93.6% with relative standard deviations (RSDs) <5.2%. The validation results illustrated that the methods were reliable and sensitive. The average processing factor (PF) during household oil processing via hot press technique and cold press technique was 0.15 and 0.51, respectively. This study demonstrated that household oil processing could significantly reduce the pesticide residues, especially by hot press technique. 相似文献
9.
Kiymet Gözek Ülkü Yücel Murat İlim Perihan Aysal Aydin Ş. Tunçbilek 《Journal of environmental science and health. Part. B》2013,48(3):413-429
Abstract An olive tree was treated twice in the field with 14C‐dimethoate (237.7 (μCi, 2.4 g) and 14C residues were determined in the olive fruits at harvest. The fruits were crushed and pressed to extract the crude oil, then refined by neutralization, bleaching and deodorization. The crude oil contained 14.1% of the total 14C in the olive fruits. Neutralization resulted in a reduction of 14C by about 50% of the total 14C residues in oil. Bleaching and deodorization processes further reduced the 14C residues and the refined oil contained 31.6% (which corresponds to 4.4% of I4C residues of the total 14C in olive fruits) of the total 14C in the crude oil. Industrially extracted crude oil was fortified with 14C‐dimethoate at 1.8 mg kg‐1 (0.02 μCi) level and subjected to the same refining process. A sharp decrease in the amount of 14C was observed by neutralization and the amount of 14C remaining in the refined oil was about 7.3% of the total l4C in the crude fortified oil. The data suggest that the 14C residues in the aged and the fortified oil amples were not of the same nature. The terminal 14C residue in the refined oil obtained from the field experiment did not contain dimethoate and/or its oxon. 相似文献
10.
Determination of acaricide residues in saudi arabian honey and beeswax using solid phase extraction and gas chromatography 总被引:1,自引:0,他引:1
Determination of acaricide residues of flumethrin, tau-fluvalinate, coumaphos, and amitraz in honey and beeswax was carried out using a rapid extraction method utilizing C-18 SPE cartridges and an analytical method utilizing GC with ECD, NPD, and MSD detectors for the four acaricides. Recovery percentages from the extraction method ranged from 90-102%, while the minimum detection levels ranged from 0.01-0.05 mg/kg for the acaricides. Nine of the 21 analyzed samples were found to be contaminated with the acaricides tau-fluvalinate and coumaphos. Neither flumethrin nor amitraz was detected in any of the honey or wax samples. Coumaphos was found only in honey samples in which two samples exceeded the tolerance levels set by EPA and EC regulations. It has not been detected in beeswax. Five honey samples and eight beeswax samples were found to be contaminated with tau-fluvalinate. One of the wax samples was contaminated with a relatively high residue of tau-fluvalinate and contained above 10 mg/kg. 相似文献
11.
Farag Malhat Hany Badawy Dalia Barakat Ayman Saber 《Journal of environmental science and health. Part. B》2013,48(5):331-335
A method for determination of etoxazole residues in apples, strawberries and green beans was developed and validated. The analyte was extracted with acetonitrile from foodstuff and a charcoal-celite cartridge was used for clean-up of raw extracts. Reversed phase high performance liquid chromatography with photodiode array detector (HPLC-DAD) was used for the determination and quantification of etoxazole residues in the studied samples. The calibration graphs of etoxazole in a solvent or three blank matrixes were linear within the tested intervals 0.01–2 mg L?1, with correlation coefficient of determination >0.999. The combined solid phase extraction (SPE) clean-up and the chromatographic method steps were sensitive and reliable for simultaneous determination of etoxazole residues in the studied samples. The average recoveries of etoxazole in the tested foodstuffs were between 93.4 to 102% at spiking levels of 0.01, 0.10, and 0.50 mg kg?1, with relative standard deviations ranging from 2.8 to 4.7%, in agreement with directives for method validation in residue analyses. The limit of detection (LOD) of the HPLC-DAD system was 100 pg. The limit of quantification of the entire method was 0.01 mg kg?1. 相似文献
12.
Determination of acaricide residues of flumethrin, tau-fluvalinate, coumaphos, and amitraz in honey and beeswax was carried out using a rapid extraction method utilizing C-18 SPE cartridges and an analytical method utilizing GC with ECD, NPD, and MSD detectors for the four acaricides. Recovery percentages from the extraction method ranged from 90–102%, while the minimum detection levels ranged from 0.01–0.05 mg/kg for the acaricides. Nine of the 21 analyzed samples were found to be contaminated with the acaricides tau-fluvalinate and coumaphos. Neither flumethrin nor amitraz was detected in any of the honey or wax samples. Coumaphos was found only in honey samples in which two samples exceeded the tolerance levels set by EPA and EC regulations. It has not been detected in beeswax. Five honey samples and eight beeswax samples were found to be contaminated with tau-fluvalinate. One of the wax samples was contaminated with a relatively high residue of tau-fluvalinate and contained above 10 mg/kg. 相似文献
13.
Gözek K Yücel U Ilim M Aysal P Tunçbilek AS 《Journal of environmental science and health. Part. B》1999,34(3):413-429
An olive tree was treated twice in the field with 14C-dimethoate (237.7 muCi, 2.4 g) and 14C residues were determined in the olive fruits at harvest. The fruits were crushed and pressed to extract the crude oil, then refined by neutralization, bleaching and deodorization. The crude oil contained 14.1% of the total 14C in the olive fruits. Neutralization resulted in a reduction of 14C by about 50% of the total 14C residues in oil. Bleaching and deodorization processes further reduced the 14C residues and the refined oil contained 31.6% (which corresponds to 4.4% of 14C residues of the total 14C in olive fruits) of the total 14C in the crude oil. Industrially extracted crude oil was fortified with 14C-dimethoate at 1.8 mg kg-1 (0.02 muCi) level and subjected to the same refining process. A sharp decrease in the amount of 14C was observed by neutralization and the amount of 14C remaining in the refined oil was about 7.3% of the total 14C in the crude fortified oil. The data suggest that the 14C residues in the aged and the fortified oil amples were not of the same nature. The terminal 14C residue in the refined oil obtained from the field experiment did not contain dimethoate and/or its oxon. 相似文献
14.
Vandana Tripathy Rajbir Yadav Suneeta Devi Amol Tayade Khushbu Sharma 《Journal of environmental science and health. Part. B》2019,54(5):394-406
Extraction and quantification of pesticide residue from the milk matrix at or below the established maximum residue limit (MRL) is a challenging task for both analytical chemists and the regulatory institutions to take corrective actions for the human health and safety. The main aim of the study is to develop a simple rapid and less expensive QuEChERS extraction and cleanup method for simultaneous analysis of 41 multiclass pesticide residue in milk by gas chromatography-electron capture detector (GC-ECD), followed by confirmation of the residues with gas chromatography-mass spectrometer (GC-MS). Effect of sorbent type, temperature, spiking concentration, matrix effect (ME), measurement uncertainty (MU), inter- and intra-assay repeatability, reproducibility of recovery, and trueness of the results were investigated to validate the effectiveness of the method. Limit of determination (LOD) and limit of quantitation (LOQ) for all the analytes ranged within 0.001–0.02 and 0.002–0.05 µg mL?1, respectively. The % recovery of all the pesticides ranged between 91.38 and 117.56% with relative standard deviation (RSD) below 2.79%. The MU for all the analytes was ≤29% of respective LOQs, and except for few pesticides, the ME was largely negative. The method fulfilled all the SANTE guidelines and thus can be extended for routine analysis of multiclass pesticide residue in milk. 相似文献
15.
Jessick AM Moorman TB Coats JR 《Journal of environmental science and health. Part. B》2011,46(8):735-740
Analytical methods to improve the detection of erythromycin in water and sediment were developed to optimize for erythromycin's recovery of extractable and bound residues from the aquatic environment. The objective of this study was to determine optimal recovery of erythromycin from water and sediment to improve its detection in environmental samples through solid-phase extraction (SPE) and sediment-extraction methods. SPE methods examined included previously reported methods for macrolide and sulfonamide antibiotics with erythromycin recoveries ranging from 75.5 % to 94.7 %. Extraction of erythromycin was performed from sand employing various solvents and buffers to determine the best method for extraction from two sandy loam pond sediments. Various extraction times were also examined, and all extraction procedures were performed in duplicate. The greatest recovery of (14)C-erythromycin in the Iowa sediment was 84 % using 0.3 M ammonium acetate at pH 4.2: acetonitrile (15:85, v/v) solution. The Oklahoma sediment yielded the greatest recovery of (14)C-erythromycin at 86.7 % with 0.3 M ammonium acetate at pH 7: acetonitrile (30:70, v/v) with a 60-minute shake time. The present results demonstrate improved extraction methods for enhancing the accuracy of erythromycin detection from environmental samples. 相似文献
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17.
M. D. H. Prodhan Emmanouil-N. Papadakis Euphemia Papadopoulou-Mourkidou 《Journal of environmental science and health. Part. B》2016,51(9):644-653
To estimate the variability of pesticide residue levels present in cauliflower units, a total of 142 samples were collected from a field trial of a cooperative farmer, and 120 samples were collected from different market places in Thessaloniki, Greece. The collected samples were extracted using the quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction technique, and the residues were determined by liquid chromatography–tandem mass spectrometry. The developed method was validated by evaluating the accuracy, precision, linearity, limit of detection (LOD), and limit of quantification (LOQ). The average recoveries for all the analytes, derived from the data of control samples fortified at 0.01, 0.05, 0.1, and 0.2 mg/kg, ranged from 74 to 110% with a relative standard deviation of ≤8%. The correlation coefficient (R2) was ≥0.997 for all the analytes using matrix-matched calibration standards. The LOD values ranged from 0.001 to 0.003 mg/kg, and the LOQ was determined at 0.01 mg/kg for all the sought analytes. The matrix effect was found to be at a considerable level, especially for cypermethrin and deltamethrin, amounting to +90% and +145%, respectively. For the field samples, the unit-to-unit variability factors (VFs) calculated for cypermethrin and deltamethrin were 2.38 and 2.32, respectively, while the average VF for the market basket samples was 5.11. In the market basket samples, residues of cypermethrin, deltamethrin, chlorpyrifos, and indoxacarb were found at levels ≥LOQ and their respective VFs were 7.12, 5.67, 5.28, and 2.40. 相似文献
18.
Ashley M. Jessick Thomas B. Moorman Joel R. Coats 《Journal of environmental science and health. Part. B》2013,48(8):735-740
Analytical methods to improve the detection of erythromycin in water and sediment were developed to optimize for erythromycin's recovery of extractable and bound residues from the aquatic environment. The objective of this study was to determine optimal recovery of erythromycin from water and sediment to improve its detection in environmental samples through solid-phase extraction (SPE) and sediment-extraction methods. SPE methods examined included previously reported methods for macrolide and sulfonamide antibiotics with erythromycin recoveries ranging from 75.5 % to 94.7 %. Extraction of erythromycin was performed from sand employing various solvents and buffers to determine the best method for extraction from two sandy loam pond sediments. Various extraction times were also examined, and all extraction procedures were performed in duplicate. The greatest recovery of 14C-erythromycin in the Iowa sediment was 84 % using 0.3 M ammonium acetate at pH 4.2: acetonitrile (15:85, v/v) solution. The Oklahoma sediment yielded the greatest recovery of 14C-erythromycin at 86.7 % with 0.3 M ammonium acetate at pH 7: acetonitrile (30:70, v/v) with a 60-minute shake time. The present results demonstrate improved extraction methods for enhancing the accuracy of erythromycin detection from environmental samples. 相似文献
19.
Thitinan Kitisin Pornsawan Visoottiviseth Hilmar Drechsel Pahol Kosiyachinda Natthanej Luplertlop 《Journal of environmental science and health. Part. B》2013,48(10):823-829
Local residents who habitually consume cadmium-contaminated rice (Oryza sativa L.) can be exposed to cadmium toxicity in Mae Sot District, Tak Province, Thailand. This study aimed to investigate an alternative for utilizing cadmium-contaminated rice without compromising their health with hazard risks. First, cadmium (Cd) concentration in rice grain and crude rice oil was determined (0.203 ± 0.030 and 0.007 ± 0.002 mgCd/kg dry weight, respectively). Then crude rice oil extracted from cadmium-contaminated rice grain was studied for its anti-oxidative property using the 2,2-diphenyl-1-picrylhydrazyl (DPPH) free radical scavenging approach. Next, quantitative analysis of γ-oryzanol in crude rice oil was conducted. Results indicated that the level of cadmium concentration in the rice grain could cause adverse effects on human health. However, the amount of cadmium in the crude rice oil was safe for consumption. In crude rice oil anti-oxidative property, crude rice oil extracted from cadmium-contaminated rice was significantly higher than the control (P < 0.05). The concentration of γ-oryzanol in crude rice oil extracted from cadmium-contaminated rice was significantly higher than that in the control crude rice oil (P < 0.05). This study demonstrates an alternative way to use the rice grown in cadmium-contaminated areas for crude rice oil production for its anti-oxidative properties. 相似文献
20.
The aim of this work was to comparatively assess the persistence of pirimiphos methyl residues in cereals and in their milling fractions after spray application in post harvest. An analytical method, based on a slightly modified QuEChERS extraction followed by liquid chromatography tandem mass spectrometry (LC-MS/MS) determination was validated: mean recovery was in the range 73% to 92% depending on the spiking level, and precision as RSD ranged from 11% to 16%. The analysis of treated samples revealed that pirimiphos-methyl residues were highly persistent and that no differences could be observed between wheat, durum wheat and oat. As far as the impact of the milling process on residues is concerned, pirimiphos methyl contamination was significantly reduced during both cleaning and processing, and most of the contamination was related to outer kernel fractions. 相似文献