Optimization and Validation of a Residue Analysis Method for Glyphosate, Glufosinate, and Their Metabolites in Plant Matrixes by Liquid Chromatography with Tandem Mass Spectrometry

2017 ◽  
Vol 100 (3) ◽  
pp. 631-639 ◽  
Author(s):  
Dasharath P Oulkar ◽  
Sandip Hingmire ◽  
Arnab Goon ◽  
Manjusha Jadhav ◽  
Bharat Ugare ◽  
...  
Keyword(s):  
Residue Analysis ◽  
Direct Analysis ◽  
Field Trials ◽  
Cotton Leaf ◽  
Solvent Ratio ◽  
Extraction Solvent ◽  
Aminomethylphosphonic Acid ◽  
Cleanup Procedure ◽  
Aqueous Layer ◽  
Herbicide Glyphosate

Abstract A sensitive and accurate LC with tandem MS (MS/MS)-based method was developed and validated for the analysis of the herbicide glyphosate, its metabolite aminomethylphosphonic acid (AMPA), and glufosinate after derivatization with 9-fluorenylmethyl chloroformate (FMOC-Cl) in various plant matrixes. The method also covers direct analysis of the glufosinate metabolites 3-methylphosphinicopropionic acid (3-MPPA) and N-acetyl-glufosinate (NAG). The homogenized samples were extracted with 0.1% formic acid in water–dichloromethane (50 + 50). The aqueous layer was derivatized with FMOC-Cl, cleaned through an HLB SPE cartridge, and determined by LC-MS/MS. The sample size, extraction solvent, sample-to-solvent ratio, derivatization conditions,and cleanup procedure were thoroughly optimized, the LOQs of glyphosate, glufosinate, and AMPA were 0.5 ng/g in grape, corn (leaf and seed), and cotton (leaf, seed, and oil) and 2 ng/g in soybean and tea. The LOQs of NAGand 3-MPPA were 50 ng/g in all the test matrixes, except tea and soybean, for which the LOQ was 100 ng/g. Inall cases, average recoveries were >80%. The method successfully performed the estimation of glyphosate in incurred corn and cotton leaf samples collected from supervised field trials.

scholarly journals Effects of Glyphosate-Based and Derived Products on Sea Urchin Larval Development

2020 ◽  
Vol 8 (9) ◽  
pp. 661
Author(s):  
Davide Asnicar ◽  
Costanza Cappelli ◽  
Ahmad Safuan Sallehuddin ◽  
Nur Atiqah Maznan ◽  
Maria Gabriella Marin
Keyword(s):  
Larval Development ◽  
Sea Urchin ◽  
Marine Invertebrates ◽  
Parent Compound ◽  
Paracentrotus Lividus ◽  
Marine Species ◽  
Negative Effects ◽  
Aminomethylphosphonic Acid ◽  
Main Degradation Product ◽  
Herbicide Glyphosate

Despite the widespread use of herbicide glyphosate in cultivation, its extensive runoff into rivers and to coastal areas, and the persistence of this chemical and its main degradation product (aminomethylphosphonic acid, AMPA) in the environment, there is still little information on the potential negative effects of glyphosate, its commercial formulation Roundup® and AMPA on marine species. This study was conducted with the aim of providing a comparative evaluation of the effects of glyphosate-based and its derived chemicals on the larval development of the sea urchin Paracentrotus lividus, thus providing new data to describe the potential ecotoxicity of these contaminants. In particular, the effects on larval development, growth and metabolism were assessed during 48 h of exposure from the time of egg fertilization. The results confirm that AMPA and its parent compound, glyphosate have similar toxicity, as observed in other marine invertebrates. However, interestingly, the Roundup® formulation seemed to be less toxic than the glyphosate alone.

scholarly journals Extraction Solvents Composition Effect In Biodiesel Production From Microalgae Consortium Botryococcus Braunii And Dunaliella Sp.

Khazanah ◽  
2020 ◽  
Vol 12 (2) ◽  
Author(s):  
Tiara Nur Azizah ◽  
◽  
Alya Putri Ramadhanty ◽  
Nadya Feranika ◽  
◽  
...  
Keyword(s):  
Fossil Fuels ◽  
Production Capacity ◽  
Water Concentration ◽  
Soxhlet Extraction ◽  
Botryococcus Braunii ◽  
Solvent Mixture ◽  
Biodiesel Production ◽  
Solvent Ratio ◽  
Extraction Solvent ◽  
Biodiesel Synthesis

Indonesia has entered an energy emergency phase, proven that Indonesia is no longer a surplus oil producer due to the productivity of the wells decrease over the years and the pattern of people's consumption of fossil fuels has been exceeding the production capacity. Therefore, we need the right solution to overcome this problem, which is developing biodiesel as renewable energy based on microalgae oil. The microalgae used in this research is the consortium of microalgae Botryococcus braunii and Dunaliella sp. Microalgae were cultivated and harvested through the dewatering process with 1 g naoh/1 L water concentration. Water contents of cultivated Botryococcus braunii are 60.2505% while Dunaliella sp. Is 64.5002%. The oil from microalgae is obtained by extracted dry microalgae through the soxhlet extraction (leaching) method with mixed solvent n-hexane and ethanol as the co-solvent using a variety of solvent ratio 2:1 and 3:1. Pure microalgae consortium oil separated from the solvent using the distillation process then analyzed with GC-FID. The analysis result is trans-linoleic acid is the most dominant fatty acid contained in this oil. Transesterification process with cao (1.5% of oil weight) as a catalyst. The results obtained from this study are the oil yield 72% extracted with a solvent mixture of n-hexane and ethanol 2:1 and 60.4% for 3:1. The biodiesel synthesis resulted in the amount of yield obtained from the solvent ratio 2:1 extraction is 94.3%, while with solvent ratio 3:1 is 79.2%. The quality of both biodiesels has met the requirements of SNI 7182:2015 and ASTM D7467, except the density of biodiesel with extraction solvent composition 3:1 which is below the standard. Therefore, the best biodiesel quality is obtained from microalgae consortium’s oil with the composition of extraction solvent 2:1.

Thin-Layer Chromatography for Chlorinated Pesticide Residue Analysis without Cleanup

1964 ◽  
Vol 47 (2) ◽  
pp. 306-310
Author(s):  
H V Morley ◽  
M Chiba
Keyword(s):  
Gas Chromatography ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Plant Extracts ◽  
Residue Analysis ◽  
Rapid Screening ◽  
Pesticide Residue Analysis ◽  
Cleanup Procedure ◽  
Layer Chromatography

Abstract Thin-layer chromatography on silica gel may be used for the determination of chlorinated pesticide residues in some plant extracts without prior cleanup, thus eliminating the possible loss of pesticides during the cleanup procedure. Rapid screening of a large number of samples is thus possible with consequent saving of time and labor. When necessary, thin-layer chromatography may be used as a prior cleanup for gas chromatography.

Passive Diffusion through Polymeric Membranes: A Novel Cleanup Procedure for Analysis of Azinphos-Methyl and Azinphos-Ethyl Residues in Fruits and Vegetables

1995 ◽  
Vol 78 (6) ◽  
pp. 1450-1454 ◽  
Author(s):  
Nazir Ahmad ◽  
Lin Guo ◽  
Peter Mandarakas ◽  
Sbmeone Appleby ◽  
George Bugueno
Keyword(s):  
Fruits And Vegetables ◽  
Residue Analysis ◽  
Cost Effective ◽  
Field Evaluation ◽  
Polymeric Membrane ◽  
Gas Liquid Chromatography ◽  
Final Volume ◽  
High Lipid ◽  
Azinphos Methyl ◽  
Cleanup Procedure

Abstract A novel procedure is described for simple removal of coextractives prior to analysis of fruits and vegetables for azinphos-methyl and azinphos-ethyl residues. The solvent extract is concentrated, placed in a polymeric membrane tube, and then dialyzed in cyclohexane. Both azinphos-methyl and azinphos- ethyl diffuse into the surrounding solvent while coextractants remain inside the membrane. The dialyzing solvent is exchanged during concentration with n-hexane and analyzed without further cleanup by gas-liquid chromatography with a specific thermionic detector. The detection limit for a 25 g grape sample with final volume of extract made to 15 mL was 0.01 mg/kg. Recoveries of both residues from grapes averaged 107% (spike levels of 0.3 to 2.0 mg/kg). From a 20 g spinach sample, recoveries averaged 82% for azinphos-methyl and 72% for azinphos-ethyl when final volume of extract was made to 5 mL (spike levels of 0.1 to 1.0 mg/kg). Recoveries from 20 types of fruits and vegetables (20 g sample spiked at 1 mg/kg for both azinphos-methyl and azinphos-ethyl) were consistently greater than 70%, except for strawberries (61–67%) and avocado (28–34%). The high lipid content of avocado may impede diffusion of azinphosmethyl and azinphos-ethyl through the polymeric membrane. A field evaluation of the procedure showed a strong correlation (r = 0.957) between azinphos-methyl residues on grapes and treatments with 2 spray formulations. The membrane cleanup procedure is a simple and cost-effective alternative to other column or liquid–liquid partitioning procedures for azinphos-methyl and azinphosethyl residue analysis.

Cleanup for Residue Analysis of Some 2,4-D Esters in Potatoes

1963 ◽  
Vol 46 (5) ◽  
pp. 881-883
Author(s):  
Arthur Bevexue ◽  
Gunter Zweig ◽  
Nancy L Nash
Keyword(s):  
Residue Analysis ◽  
Cleanup Procedure

Abstract A cleanup procedure was devised for analysis of 2,4-D esters in potatoes which eliminated the interference of a halogen-containing material in the potatoes. Recoveries on fortified samples were 82-84%.

Determination of Melengestrol Acetate in Bovine Tissue: Collaborative Study

1976 ◽  
Vol 59 (3) ◽  
pp. 507-515
Author(s):  
Leo F Krzeminski ◽  
Shu Geng ◽  
Byron L Cox
Keyword(s):  
Collaborative Study ◽  
Chromatographic Determination ◽  
Extraction Solvent ◽  
Melengestrol Acetate ◽  
Cleanup Procedure ◽  
Liquid Chromatographic Determination ◽  
Fat Liver ◽  
Comparison Of The Results ◽  
Tissue Recovery ◽  
Liquid Chromatographic

Abstract Seven laboratories collaboratively studied a method for the assay of melengestrol acetate at the 0, 10, and 20 ppb levels in bovine fat, liver, muscle, and kidney. The study included fortification of tissue by each laboratory and analysis of fat samples taken from treated heifers which had endogenous levels of 0, 10, and 20 ppb melengestrol acetate. The multistep cleanup procedure used included extraction, solvent partition, column chromatography, and electron capture gas-liquid chromatographic determination. Results of the study for muscle, liver, kidney, and fat showed that the method gave satisfactory recoveries and accuracy. In fat, the most critical tissue, recovery was >93%. A statistical comparison of the results reported for fat tissue from treated heifers demonstrated that 5 of the 7 laboratories obtained similar results. The results produced by the method can be expected to be repeatable within and among laboratories. On the basis of the collaborative results the method has been adopted as official first action.

Determination of Imidacloprid, Acetamiprid, Thiabendazole and Carbendazim Residues in Edible Fungi by HPLC

2013 ◽  
Vol 781-784 ◽  
pp. 99-103 ◽  
Author(s):  
Ling Lin ◽  
Chun Liang Yang ◽  
Zheng Peng ◽  
Ming Yue Wang ◽  
Zong Qiang Zeng ◽  
...  
Keyword(s):  
Solid Phase ◽  
Residue Analysis ◽  
Correlation Coefficients ◽  
Edible Fungi ◽  
Extraction Solvent ◽  
Solid Phase Extraction Cartridge ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Straw Mushroom

A method was developed for simultaneous determination of imidacloprid,acetamiprid, thiabendazole and carbendazim in lentinus edodes, straw mushroom and oyster mushroom by HPLC. Acetonitrile was edded in the sample for extraction solvent, the sample was purified by NH2 solid phase extraction cartridge,then detected by HPLC.The results showed that a good linearity in the range of 0.05~5.0μg/mL with the linear correlation coefficients of 0.9991~0.9997, the detection limits of imidacloprid, acetamiprid, thiabendazole and carbendazim were respectively 0.002 mg/kg,0.005mg/kg, 0.003 mg/kg and 0.003 mg/kg.Tests for recovery were made by addition of four pesticidess standards at three different concentration levels (0.1, 0.5 and 1.0 mg/kg) to the blank sample.The mean recovery rates were 86.0%~105.0% , the relative standard deviations were less than 3.5%.The sensitivity, accuracy and precision of this method were able to meet the requirements for pesticide residue analysis.

Study on Technic Condition of Extracting Solanesol from Abandon Tobacco

2012 ◽  
Vol 550-553 ◽  
pp. 1623-1628
Author(s):  
Mei Yang ◽  
Zheng Gui Gu
Keyword(s):  
Organic Solvent ◽  
Petroleum Ether ◽  
Total Yield ◽  
Solvent Ratio ◽  
Extraction Temperature ◽  
Extraction Solvent ◽  
Solvent Solvent

Solanesol is an important pharmaceutical intermediate. In this paper, organic solvent is used to extract solanesol from the abandoned tobacco. The conditions of extracting the solanesol are optimized, such as extraction solvent, solvent ratio, extraction temperature and time. The extraction times are also identified. L9(34) design is selected to investigate the factors above. Finally, the optimal extraction conditions are proposed. The petroleum ether is used as solvent, the solvent ratio is 15:1(volume of solvent is 15ml, quality of leaves is 1g), the extraction temperature is 50°C and the time is 4h. The purity of solanesol reaches to 57.56% and the total yield reaches to 6.39%.

Residue analysis of fosthiazate in cucumber and soil by QuEChERS and GC-MS

2014 ◽  
Vol 68 (10) ◽  
Author(s):  
Min Wu ◽  
Jiye Hu
Keyword(s):  
Solid Phase ◽  
Residue Analysis ◽  
Field Trials ◽  
Residue Level ◽  
Gas Chromatography Mass Spectrometry ◽  
Dispersive Solid Phase Extraction ◽  
First Order ◽  
First Order Kinetics ◽  
Maximum Residue Level ◽  
Relative Standard

AbstractA convenient method was developed for the determination and validation of fosthiazate in cucumber and soil. The procedure is based on liquid partitioning with acetonitrile followed by dispersive solid phase extraction as the clean-up step, after which samples were analysed by gas chromatography-mass spectrometry (GC-MS). The average recoveries ranged from 91.2 % to 99.0 % with relative standard deviations (RSDs) of less than 6.05 %, at three fortification levels (0.02 mg kg−1, 0.1 mg kg−1, 0.5 mg kg−1) in cucumber and soil, and the limits of quantification (LOQs) for fosthiazate were all established at 0.02 mg kg−1. The proposed method was applied successfully to analyses of the dissipation and residue of fosthiazate in field trials. The dissipation rate of fosthiazate was described using pseudo-first-order kinetics with a half-life of 4.33 days and 4.08 days in soil in Beijing and Shandong, respectively. In the terminal residue experiment, fosthiazate residues in cucumber and soil were clearly below the maximum residue level (MRL, 0.2 mg kg−1) set in China.

scholarly journals Comparison of total phenolic and flavonoids contents in Malaysian propolis extract with two different extraction solvents

2019 ◽  
Vol 6 (2) ◽  
pp. 1-11
Author(s):  
Siti Umairah Mokhtar
Keyword(s):  
Colorimetric Method ◽  
Water Extract ◽  
Ethanolic Extract ◽  
Extraction Process ◽  
Total Phenolic ◽  
Solvent Ratio ◽  
Propolis Extract ◽  
Extraction Solvent ◽  
Percentage Yield

This study is aimed to prepare propolis extracts by using two different solvents which are ethanol and water via maceration method and to evaluate the total phenolic and flavonoid components of the extract. Optimization of the extraction process was done by using different solvents and sample-to-solvent ratio. The ethanolic and water extracts were analysed for the determination of Total Phenolic Content (TPC) and Total Flavonoid Content (TFC) by using Folin-Ciocalteu colorimetric method and Aluminimum chloride method, respectively. Based on sample-to-solvent ratio, it showed that 1:10 gave the highest percentage yield compared to other ratio for both solvents. Ethanolic extract resulted contains high phenolic and flavonoids content compared to water extract. The result showed that sample-to-solvent ratio 1:5 gave highest TPC and TFC in ethanolic extract which are 29.09 and 7.75 mg GAE/g, respectively. In conclusion, this study revealed that ethanol is the best extraction solvent to be used for propolis extraction compared to water. It is also demonstrated that higher volume of solvent does not leads to high values of TPC and TFC. The optimum extraction parameters and conditions are necessary to be obtained in order to extract high TPC and TFC.

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