scholarly journals Optimization and Validation of an Extraction Method for Endosulfan Lactone on a Solid Substrate

Processes ◽  
2021 ◽  
Vol 9 (2) ◽  
pp. 284
Author(s):  
Paola T. Vázquez-Villegas ◽  
Rocío Meza-Gordillo ◽  
María C. Luján-Hidalgo ◽  
Abumalé Cruz-Salomón ◽  
Víctor M. Ruíz-Valdiviezo ◽  
...  
Keyword(s):  
Ethyl Acetate ◽  
Extraction Method ◽  
Agricultural Soil ◽  
Parent Compound ◽  
Solid Substrate ◽  
Response Surface Design ◽  
Surface Design ◽  
Quantification Limit ◽  
The One

Endosulfan lactone is a metabolite obtained from the biological oxidation of the insecticide endosulfan by action of the microorganisms present in the soil. This metabolite is more toxic and persistent than the parent compound. Therefore, it is extremely important to be able to determine the presence of this metabolite in the soil. However, accessible methods for extraction of endosulfan lactone in soil were not found in published literature. For this reason, the aim of this study was to evaluate two conventional methods of liquid–solid extraction for the determination of endosulfan lactone in solid substrate using two solvents (ethyl acetate and acetonitrile) and HPLC UV-VIS. The acetonitrile and rotary agitation extraction method was the one with the highest efficiency (97%), optimized using a factorial 32 response surface design, and validated in terms of linearity and precision. The linearity shown was r > 0.999 in a wide spike level (0.15–100 mg kg−1), with the detection limit (DL) of 0.045 mg kg−1 and quantification limit (QL) of 0.15 mg kg−1. The extraction of endosulfan lactone in solid substrate using acetonitrile was more efficient than that used with ethyl acetate, so this method could be used to extract and quantify endosulfan lactone in agricultural soil.

Fast Cleanup of Difficult Substrates for Determination of Fenitrothion and Some Derivatives

1981 ◽  
Vol 64 (6) ◽  
pp. 1470-1473
Author(s):  
Patrick Haché ◽  
René Marquette ◽  
Gilles Volpé ◽  
Victorin N Mallet
Keyword(s):  
Liquid Chromatography ◽  
Ethyl Acetate ◽  
Parent Compound ◽  
Chicken Liver ◽  
Gas Liquid Chromatography ◽  
Fast Recovery ◽  
Simple Method ◽  
Flame Photometric Detector ◽  
Derivatives Of

Abstract A simple method is described for the fast recovery of fenitrothion, an organophosphorus insecticide, from soil, chicken liver, urine, clams, and pine needles. The substrate is homogenized with acetonitrile or methanol, diluted with water, and passed through a column containing Amberlite XAD-7. Fenitrothion is recovered quantitatively by eluting with 4 portions of 25 mL ethyl acetate. After evaporation, the compound is determined quantitatively by gas-liquid chromatography with a flame photometric detector. The procedure is also suitable for some derivatives of fenitrothion, namely, fenitrooxon and S-methylfenitrothion. As low as 0.05 ppm of the parent compound may be determined.

scholarly journals Extraction Method for the Determination of Atrazine, Deethylatrazine, and Deisopropylatrazine in Agricultural Soil Using Factorial Design

2013 ◽  
Author(s):  
Maristela F. Amadori ◽  
Gilcélia A. Cordeiro ◽  
Caio C. Rebouças ◽  
Patricio G. Peralta-Zamora ◽  
Marco T. Grassi ◽  
...  
Keyword(s):  
Factorial Design ◽  
Extraction Method ◽  
Agricultural Soil

Heteronuclear Nucleobase Complexes as Tools for the Isolation of the Minor Rotamer of the Parent Compound: Synthesis and Crystal Structure Determination of Head-Head and Head-Tail Forms of trans-[(CH3NH2)2Pt(1-MeC-N3)2]2+ (1-MeC = 1-methylcytosine)

1995 ◽  
Vol 50 (11) ◽  
pp. 1767-1776 ◽  
Author(s):  
Dagmar Holthenrich ◽  
Imre Sóvágó ◽  
Gerd Fusch ◽  
Andrea Erxleben ◽  
Edda C. Fusch ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Parent Compound ◽  
Crystal Structure Analysis ◽  
Rapid Crystallization ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Compound Synthesis ◽  
The One ◽  
Solid State Structures

The two rotamers (head-tail, 1, and head-head, 2) of the bis(1-methylcytosine)complex of trans-(CH3NH2)2Pt(II), have been crystallized as ClO4- (1, 2a) and PF6- (2b) salts and characterized by X-ray crystal structure analysis and 1H and 195Pt NMR spectroscopy. In aqueous solution, 1 is preferred over 2 by 70:30. Upon slow crystallization from H2O, 1 is obtained as the only product. Isolation of 2a and 2b has now been accomplished via formation of the heteronuclear derivative trans-[(CH3NH2)2Pt(1-MeC--N3,N4)2Hg]2+, in which the deprotonated 1-methylcytosinato ligands (1-MeC-) are oriented head-head, precipitation of Hg(II) by thiourea, and rapid crystallization of the parent compound. The solid state structures of 1 and 2b differ markedly in a number of aspects. Isolation of pure 1 and 2 permits a detailed study of the kinetics and thermodynamics of the interconversion of the two rotamers. From comparison with the behavior of 1 and 2 in H2O on the one hand and DMSO and DMF on the other a clear solvent effect on the rotamer distribution is seen which most likely relates to differences in H bonding between solvent and solute.

scholarly journals Extraction method for the determination of atrazine, deethylatrazine, and deisopropylatrazine in agricultural soil using factorial design

2013 ◽  
Vol 24 (3) ◽  
pp. 483-491 ◽  
Author(s):  
Maristela F. Amadori ◽  
Gilcélia A. Cordeiro ◽  
Caio C. Rebouças ◽  
Patricio G. Peralta-Zamora ◽  
Marco T. Grassi ◽  
...  
Keyword(s):  
Factorial Design ◽  
Extraction Method ◽  
Agricultural Soil

Use of alumina columns to prepare plasma samples for liquid-chromatographic determination of catecholamines.

1987 ◽  
Vol 33 (2) ◽  
pp. 286-287 ◽  
Author(s):  
P F Maycock ◽  
K N Frayn
Keyword(s):  
Sample Preparation ◽  
Extraction Method ◽  
Plasma Catecholamines ◽  
Chromatographic Determination ◽  
Plasma Samples ◽  
Improved Method ◽  
Liquid Chromatographic Determination ◽  
The One ◽  
Liquid Chromatographic

Abstract We describe an improved method of sample preparation for liquid chromatographic determination of plasma catecholamines. The catecholamines are extracted from plasma by using small, cheaply-made columns of alumina, with or without prior clean-up on commercially available ion-exchange columns. Advantages of this technique over the conventional batch-extraction method of using alumina are speed, convenience, and improved sample clean-up. In particular, the one-stage method we describe allows results to be reported within 20 min of receiving the sample.

Two-Stage Procedure for the Quantitative Determination of Autoprothrombin III Concentration and Some Applications

1967 ◽  
Vol 18 (01/02) ◽  
pp. 198-210 ◽  
Author(s):  
Ronald S Reno ◽  
Walter H Seegers
Keyword(s):  
Prothrombin Time ◽  
Factor Vii ◽  
Two Stage ◽  
Pronounced Increase ◽  
One Stage ◽  
Assay Procedure ◽  
Bovine Plasma ◽  
The One ◽  
Autoprothrombin C

SummaryA two-stage assay procedure was developed for the determination of the autoprothrombin C titre which can be developed from prothrombin or autoprothrombin III containing solutions. The proenzyme is activated by Russell’s viper venom and the autoprothrombin C activity that appears is measured by its ability to shorten the partial thromboplastin time of bovine plasma.Using the assay, the autoprothrombin C titre was determined in the plasma of several species, as well as the percentage of it remaining in the serum from blood clotted in glass test tubes. Much autoprothrombin III remains in human serum. With sufficient thromboplastin it was completely utilized. Plasma from selected patients with coagulation disorders was assayed and only Stuart plasma was abnormal. In so-called factor VII, IX, and P.T.A. deficiency the autoprothrombin C titre and thrombin titre that could be developed was normal. In one case (prethrombin irregularity) practically no thrombin titre developed but the amount of autoprothrombin C which generated was in the normal range.Dogs were treated with Dicumarol and the autoprothrombin C titre that could be developed from their plasmas decreased until only traces could be detected. This coincided with a lowering of the thrombin titre that could be developed and a prolongation of the one-stage prothrombin time. While the Dicumarol was acting, the dogs were given an infusion of purified bovine prothrombin and the levels of autoprothrombin C, thrombin and one-stage prothrombin time were followed for several hours. The tests became normal immediately after the infusion and then went back to preinfusion levels over a period of 24 hrs.In other dogs the effect of Dicumarol was reversed by giving vitamin K1 intravenously. The effect of the vitamin was noticed as early as 20 min after administration.In response to vitamin K the most pronounced increase was with that portion of the prothrombin molecule which yields thrombin. The proportion of that protein with respect to the precursor of autoprothrombin C increased during the first hour and then started to go down and after 3 hrs was equal to the proportion normally found in plasma.

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