CS264634B1 - Method of analysis of 1- (r-phenylcyclohexyl) piperidine nitrophenols - Google Patents

Abstract

The solution belongs to the field of clinical biochemistry, pharmaceutical analysis, chemical toxicology and chemical control. An aqueous solution of the determined 1-(1-phenylcyclohexyl)-piperidine is treated with nitrophenol of the formula [Rm.CgHn.OH] (NO2>Jc, where m = 1 to 2, η = 1 to Z, k = 1 to 3, and m+n+k=6R is a radical selected from the group including methyl, phenyl, naphthyl and hydroxyl, the mixture is extracted with an organic solvent selected from the group including benzene, chloroform, 1,1,2,2-tetrachloroethane and the color intensity of the organic solution of the associate, which is proportional to the concentration, is measured colorimetrically. The use provides the possibility of rapid evaluation of samples of 1-(1'-phenylcyclohexyl)piperidine from a limiting concentration of 1.10~6 mol.dm-3 with an accuracy of ± 5%. It meets the requirements of automation.

Description

The invention relates to a method for the analysis of 1- (1'-phenylcyclohexyl) piperidine nitrophenols.

It solves simple, sensitive spectrophotometric determination and detection of biologically active compound. It can be used in medicine, pharmacy. The invention can be incorporated into the fields of clinical biochemistry, pharmaceutical analysis, chemical toxicology and chemical control.

The previously known methods of detection, identification and determination are mainly oriented on precipitation reactions. The potentiometric method for titration with sodium tetrafenylborate to a potassium ion selective electrode has been published (VYTŘÁS, K .: Coli, Czech, Chem. Commun.

42, 1977, p. The substance can also be identified by thin-layer chromatography and detected by Dragendorf's reagent (GASPARlC, J .: Paper and thin-layer chromatography of organic compounds. SNTL Praha 1981). There are no methods of sensitive spectrophotometric determination of 1- (1'-phenylcyclohexyl) piperidine, in particular using an extraction step. This does not give the possibility to use the analysis of 1- (1'-phenylcyclohexyl) piperidine in the laboratory operation at the basic stage, the above mentioned drawbacks being removed by the method of analysis according to the invention.

The invention is a method for analysis of 1- (1'-phenylcyclohexyl) piperidine nitrophenols, which comprises 'the fact that the aqueous solution of the sample treated nitrophenol .CgH formula Cp ^ · OH] * ^N0 2>k' ^{k <m} ^ ^{e =} 1 2, n = 1 to 2, k = 1 to 3, m + n + k = 6, R is a radical selected from methyl, phenyl, naphthyl, hydroxyl, extracted with an organic solvent selected from benzene, chloroform, 1,1,2,2-tetrachloroethane and the colorimetric intensity of the organic solution of associates is measured colorimetrically.

The advantage of the elaborated procedure is the possibility to determine 1- (1'-phenylcyclohexyl) piperidine ^- β ^- 3 up to a concentration of 2.10 mol.dm. The time required to perform the analysis is 3 minutes. The use of the proposed extraction spectrophotometric method for the analysis of 1- (1'-phenylcyclohexyl (piperidine sulfophthalein) is new because the available literature does not mention its application in technical practice. phenylcyclohexyl) piperidine from a limit concentration of 2.10 ® mol.dm at the accuracy of the method, expressed in relative standard deviation of + 5%.

Example 1

3

A real operating urine sample was imitated by adding 0.1 cm -3 -3 of an aqueous solution of 1.10 mol.dm sample solution to 1.0 cm urine and adding 1.6 cm buffered citrate

-4 -3 of a solution of pH 3, 0.2 cm @ 3 of an aqueous solution of 4.10 mol.dm of 3-methyl-4-nitrophenol and shaken with 2 cm of chloroform for 1 minute. After removal of the aqueous layer, the absorbance at 380 nm was measured. The minimum detectable concentration of 1- (1'-phenylcyclohexyl) piperidine was

5.10 mol.dm. The slope of the calibration curve was 4,800 1.1.mol .cm. Does not interrupt real sample components.

Example 2

An operational blood sample was imitated by adding 3 -2 -3 to 1.0 cm of blood plasma

0.1 cm @ 3 of an aqueous solution of 1.10 mol.dm of 1- (1-phenylcyclohexyl) piperidine. From there he was after

3 -3 —3

0,4 cm pipetted and added in 0,1 cm increments of 5.10 mol.dm 2,3,6-trinitrophenol

- 3 3 and made up to 2.0 cm with buffer pfl 3. The aqueous solutions were extracted with 2.0 cm.

chloroform within one minute. The absorbance of chloroform extracts was measured at a wavelength of 6-3 nm of 400 nm. The lowest detectable concentration was 4.10 mol.dm. Of the calibration curve was 5900 l.mol '.cm ^{-' first}

Example 3

-5 -3

0.1 cm &lt; 1 &gt; mol.dm of 1- (1-phenylcyclohexyl) piperidine- ³ was pipetted in increments of 0.1 cm

-4 -3 dine and added 0.1 cm 3 of an aqueous solution of 4.10 mol.dm 3-methyl-4-nitro-1- (4-nitrophenyl) 3

-2-pyrazolin-5-one and supplemented with citrate buffer pH 5.0 per 2.0 cm. The aqueous layers were extracted with 2.0 cm of chloroform, 1,1,2,2-tetrachloroethane and benzene. Extraction to chloro form and 1,1,2,2-tetrachloroethane was carried out in 80% yield and to benzene in 48% yield. The lowest detectable concentration of 1- (1'-phenylcyclohexyl) piperidine was 1.10 ^-6 mol.dm ^-3 . The slope of the calibration curve was 15,500 1.mol ^-3 .cm ^-3 .

Example 4

A working blood solution was prepared by adding 3 -5 -3 to 1.0 cm ^{3 of} blood plasma

0.1 cm @ 3 of an aqueous solution of 5.10 mol.dm of 1- (1'-phenylcyclohexyl) piperidine. From there, 0.3 cm of the process solution solution was pipetted into 0.1 cm aqueous solution

-4 -3

4.10 mol.dm 4,6-dinitro-2-methylphenol and supplemented with citrate buffer pH 5.0.

The aqueous layers were shaken for one minute with 2.0 cm chloroform. After aspiration of the aqueous layer, organic associate solutions were measured at 415 nm. The limit of determination was

1.10 ⁶ mol.dm ³ . The slope of the calibration curve was 8,300 1.mol ^-1 .cm ^-3 .

The method of analysis according to the invention satisfies both automation and efficiency requirements, expressed in terms of the number of samples that can be processed per hour. The procedure is modified so that it can be secured by domestic chemicals and is applicable to spectrophotometers, photometers and colorimeters with which basic operating laboratories are equipped. Said method is suitable for complementing a set of methods of analysis in pharmacy, forensic medicine, clinical biochemistry, chemical toxicology and chemical control. The sensitivity which is ensured according to the method of analysis allows the method according to the invention to be used up to a limit concentration of 1.10 .mu.m.dm ^{-3 of} 1- (1'-phenylcyclohexyl) piperidine in the sample.

Claims (1)

SUBJECT OF THE INVENTION Method for the analysis of 1- (1'-phenylcyclohexyl) piperidine nitrophenols characterized in that an aqueous solution of the sample is treated with a nitrophenol of the formula C, H, OH 2 (NO _q ), where m = 1 to 2, η = 1 to 2 , rn on 2 κ k = 1 to 3, where m + n + k = 6, R is a radical selected from the group consisting of methyl, phenyl, naphthyl and OH, extracted with an organic solvent selected from the group consisting of benzene, chloroform, 1,1 2,2-tetrachloroethane and the colorimetric intensity of the organic solution of associates is measured colorimetrically.