SU859915A1 - Method of cis 7,8-epoxy-2-methyloctadecan quantitative determination - Google Patents

Description

(54) METHOD KOJU :: .CIS-7.8 -:.: Lil.

-p-dugy DEFINITIONS -: -Y;: 1IL01STADECA A

This invention relates to analytical chemistry, in particular to a method;) quantitative determination of cis-7,8-epoxy-2-methyloctadecane. A known method for the quantitative determination of cis-7,8-eloxy-2-methyl ctadecane by passing an analyte through a molecular sieve with subsequent analysis of them with a mixture of hexane: ether: 1 and treating the resulting mixture with triphenylphosphine-di-bromide, purification and chromatography of purified product l J The disadvantage of the method is the impossibility of its use for soil analysis. The closest to the proposed method is the quantitative determination of cis-7, 8-epoxy-2 methylocane decane by uptake of the sample to be analyzed with hexane, concentration of the hexane extract with nitrogen and chromatography of the concentrate 2. The slowness of the method is low sensitivity of 1 MI; d. The purpose of inventing - raising chuvs; lit.l guests. The goal is achieved by the method of determining the definition of iiiic-7, 8-zl1ox - ;; - 2-mryl-octadecane, which consists of an acetone solution, separating and evaporating the acetone solution, and treating the sodium chloride residue and treating the resulting residue hexane-S, purification, evaporation to dryness, treatment of the dry residue with hexane, and chromatography of Bioconium hydrochloride. Ost; {ostp method tested in laboratory studies, in laboratory and field experiments, the dynamics of the killer, 8epoxy-2-met1hsokta, tsekan, applied beating: on the soil. In the laboratory experiment 200 µg p.is-7, 8-epoxy-2-methyl octadecane

applied on 200 hectares of forest soil. Could be treated with cis-7,8-epoxy-2-methyl octadecane at a rate of 40 g / ha. At certain intervals, soil samples are taken and the content of cis-7,8-epoxy-2-methyloctadecane is determined. An example. 100-150 g of forest soil are placed in a homogenizer glass, 125-130 ml of acetone are poured and extracted at 3.5 thousand rpm for 2 minutes. The homogenate is filtered on a Büchner funnel under reduced pressure (water pump). The residue in the beaker and on the filter is washed with 75-100 ml of light acetone. The combined lolrate is concentrated on a rotary evaporator at 40 ° C. The aqueous residue is transferred to a separatory funnel, 1015 ml of a saturated solution of sodium chloride is added and the disparum is extracted from this mixture for 3 minutes (2 K40 ml of hexane. Hexane solution is dried with anhydrous sulfate. sodium, filtered into a flask for distillation through a cotton swab and concentrated at 40 ° C on a rotary evaporator until almost dry. The residue is dissolved in 5 ml of hexane. This solution is fed to a chromatographic column for purification. The flask is 400 mm in diameter mp 14 mm. Fill it with aluminum oxide of the Il degree of activity as follows: put a cotton swab on the bottom, a layer b / in sodium sulfate (2 cm), a layer of aluminum oxide (10 cm) and again a layer of sodium sulfate. The column is washed 25-30 ml of hexane, quantitatively transfer the solution with cis-7,8-epoxy-2-methyloctadecane and elute it from the column with hexane. The hexane fraction with cis-7,8-epoxy-2-methyloctadecane is concentrated on

859915. 4

rotary evaporator when almost dry.

The last traces of solvent are removed by air flow. The dry residue is dissolved in 0.2-1 ml of hexane, depending on the content of cis-7 8-e.pvK and-2-methyloctadecane (disparlyr J (sample. 2 μl are added to the device. The amount of disparur in the sample is calculated by the formula CT To OOO-licvV concentration of standard pheromone solution, ng / μl; injectable volume of the standard solution, μl; llj.- height of the standard solution peak, mm; - height of the solution peak with an unknown concentration, mm; V) (- inject the sample volume with unknown concentration µl; V is the final sample volume of an unknown concentration, µl. The standard solutions of disparlyur in hexane were used. For the extraction, technical acetone was used after double distillation over potassium pedmanganate. Hexane was freshly distilled. The work was performed on a Tsvet-106 chromatograph with a flame ionization detector and a 2000x4 mm glass column filled with 5% XE- 60 on NAWDMCS chromatone. Column temperature 190s, evaporator. Carrier gas flow 40 mp / min, hydrogen 40 ml / min, air 400 ml / min. In tab. data characterizing the detection limit and accuracy of the analysis are given. The sensitivity of the assay is high and is 0.01 mg / kg of soil.

5859915

Determination of dysparlura in forest soil

Claims (2)

Claim A method for the quantitative determination of cis-7,8-epoxy-2-methyl-octadecane, including hexane treatment and chromatography, characterized in that, in order to increase the sensitivity, the test sample is treated with acetone, separated and the acetone solution is evaporated, added to the aqueous sodium chloride and the resulting mixture are treated with hexane, purified, evaporated to dryness, the dry residue is treated with hexane and the hexane solution is chromatographed. Sources of information accepted for examination 40 1. Caro J.H., Bierl B.A., Treeman N.R., Sonvet R.E. ^ Journal Agric. Food-Chemistry, 1978, v. 26, ”2, p. 46J. 2. Richerson J.V., Cameron E.A. 45 ^T -Chroma tog raptyy method detection of disparlure. Envi ronmentai · .Entomology, 1974, v 3, ”3, p. 475 (prototype) ..