CS264989B1 - Method of quantitative analysis of trace amounts of N- (1-formamido-2,2,2-trichloroethyl) morpholine in plant materials - Google Patents

Abstract

The invention relates to the field of mechanical engineering, where the guidance of bodies is mainly solved during simultaneous tilting. In order to reduce the sliding diameter of a guided body having the length and width of the guiding surfaces, a solution is presented that reduces the unfavorable ratio of length "L" to width "B" up to the limit of g by creating a system of tilting surfaces belonging essentially to one plane, with at least one pair of tilting surfaces belonging to the guiding body and the other pair to the guided body.

Description

264989 2

The invention relates to a method for the quantitative analysis of the trace amounts of N- (1-formamido-2,2,2-trichloroethyl) morpholine / trimorphamide) in plant materials. N- (1-formamido-2,2,2-trichloroethyl) morpholine, known under the generic name of trimorphamide, is a polar Czechoslovak systemic fungicide (CS 193 659), which is formulated into a suitable formulation for the control of powdery mildew in grape, barley, cucumbers, tobacco, apple trees, spouts and other cultures.

To readily assess the level of trimorphamide residues in the treated cultures at the time of harvest, as well as its biodegradation in individual environmental compartments, a rapid analytical procedure for quantitative analysis of the active ingredient content with the required evidence and yield is essential. Gas-chromatographic method for determination of trimorphamide residues in the mentioned crops, used so far in relation to the study of its residue dynamics (Kováč J .; Kovačičova J., Bátora V .: 5th International Congress on Pesticides Chemistry, Kyoto Japan, 20, 8-4 1982, Vol. 4, 201-205. Pergamon Press, Oxford - New York - Toronto - Sydney - Paris, Frankfurt, 1983, Kovac J., Koprda V, Radiochem. , (1987);

Kováč J., Grambličková A., Minářová E., Kurucová M .: Agrochemistry 26/3, 88-90 (1986); CS 254 674) is due to the separation process of vegetable co-extracts based on their partial separation in an organic solvent-water system and final purification by thin layer chromatography. Time-consuming, especially in protracted separating emulsions at the organic solvent-water phase boundaries, as well as in slow filtration phases during multiple extraction. In addition to the above, the procedures are also demanding with the consumption of organic solvents of the required analytical purity.

These drawbacks are overcome by a method of quantitatively analyzing the trace amounts of N- / 1-formamido-2,2,2-trichloroethyl / morpholine in plant materials by the gas chromatographic method of the present invention, wherein the co-extracts are separated with the silica through which the mobile phase is passed under pressure and the N- [1-formamido-2,2,2-trichloroethyl / norfoline content is evaluated in the concentrated fraction collected by the gas chromatography method.

The method of the present invention does not require a completely, oen and instrumentally demanding device for high performance liquid chromatography, with only a high pressure pump being controlled by a flowable mobile phase flow coupled through the dosing loop to the column. The separation process is very efficient and fast and solvent consumption is at least ten times lower than in the previously used methods. The simplicity, speed and accuracy of the method of the invention predetermine it for use in serial analyzes of a large number of samples for trimor Famid content in biological substrates.

The following example illustrates the invention. Example

Quantitative analysis of N- (1-dimmamido-2,2,2-trichloroethyl) morpholine (trimorphamide) in plant materials. All chemicals and solvents used were of analytical purity, the solvents were pre-distilled, leaving a one-third of the distillation residue relative to the total volume of the distilled solvent. The following equipment was used: an electric homogenizer with a coffee grinder attachment, a dosing pump - a liquid chromatographic accessory (possibly another analogue pressure dosing pump with a minimum pressure of 6 MPa), □ 3 dosing loop (50 mm), blunt dosing syringe needle (100 mm), 40 x 4 mm pre-column with silica gel filling (30 µm), 2 x 150 x 2 mm column filled with spherical silica gel (5 µm), combined in series, mobile phase: n-hexane: ethyl alcohol (92: 8 v) / v), flow rate: 1 cm3.min-1, pressure: 5.2 MPa, gas chromatograph packed column 10% diethylene glycol succinate porous polymer carrier of styrene-divinylbenzene copolymer (80/100), detector

Claims (1)

3 264989 electron capture ^ 3Ni (250 ° C), carrier gas: argon - 60 cm3.min column temperature: 160 ° C, injector: 250 ° C, detector: 270 ° C. After washing the chromatographic columns with mobile phase n-hexane-ethyl alcohol and equilibrating the 3 conditions, the retention time of the trimorphamide is determined as follows: a 3-chloroform solution of the trimorfamide standard (conc. 2 µg.cm) is metered into the above-mentioned chromatographic columns (provided with a precolumn) with a dosing slide (50 mm) and eluting with a mobile phase using a pressure pump of 1 cm / min. The retention time of trimorphamide (in this case 12 min) is determined by monitoring the content of trimorphamide in the collected fractions (1 cm 3) flowing out of the gas phase mobile phase method. At the same time, extracts can be prepared. To 25 g of homogenised plant material 100 cm 3 of chloroform are added and extracted on a mechanical shaker in a 250 cm 3 bottle with cap for 15 minutes. Then add 50 g of anhydrous sodium sulfate and shake vigorously for a further 30 minutes. From the extract, 5 cm 3 is pipetted into a calibration vessel and concentrated with a stream of air at a water bath temperature of 55 ° C to a volume of 1 cm 3. Inject 50 mm of the chromatographic column from the concentrated 3-chloroform extract of the sample and collect the mobile phase fraction corresponding to a time interval of 10.5 to 13.5 min (3 cm 3) in a 3 cm conical flask of 5 cm. at the end tapered, calibrated to a volume of 100 mm and with a closeable glass stopper. The collected fraction is concentrated to a volume of 100 cm 3 in a water bath (55 ° C), 3 cm 3 of ethyl acetate is added and concentrated again to a volume of 100 cm 3. 3 From this solution, inject 5 mm into the gas chromatograph. Trimorphamide content is determined by absolute calibration, by direct comparison of trimorfamid wave heights in calibration solution and in sample, Method yield, verified on model experiments of fortified samples of cucumber, barley, tobacco, apple, terrible, green matter of barley leaves, ranging from 80 to 90% The limit of determination of the method is 0.05 mg.kg. SUBJECT OF THE INVENTION A method of quantitative analysis of the trace amounts of N- / 1-formamido-2,2,2-trichloro-ethyl / morpholine in plant materials by a gas chromatography method, characterized in that separated on a silica column through which the mobile phase is passed through a vacuum and the N / 1-formamido-2,2,2-trichloroethyl / morpholine content is evaluated in a concentrated fraction of the mobile phase collected by gas chromatography.