CS263333B1 - Method for the analysis of diethyllysergamide sulfophthalein - Google Patents

Abstract

The reaction is in the field of clinical biochemistry, pharmaceutical analysis, chemical toxicology and chemical control. The analysis of diethyllysergamide sulfophthalein is carried out by treating the aqueous or methanolic solution of diethyllysergamide with sulfophthalein of the formula ## STR2 ## G6H (2-4) * OH (1-2) ^ (1-2) 0 Wherein x is a halogen atom selected from the group consisting of chlorine, bromine, iodine and the ionic aspirate is extracted with a solvent selected from the group consisting of benzene, chloroform, 1,1,2,2-tetrachloroethane, xylene or toluene, and after removal of the aqueous the color intensity of the solution of the diethyllysergamide and sulfophthalein ionic associate is colorimetrically measured. The use of the process provides for the possibility of express evaluation of samples containing lyophilizate, for example diethyllysergamide, from a limiting concentration of 1 · 10 ° mol.l · 1 · · · · · · · · · · · · · · · · · · · · · · · · · · · · · • • • • Meets automation requirements.

Description

The invention relates to a method for the analysis of diethyllysergamide sulfophthaleins of the formula ^C 6 ^B (2-4) *

OH (1-2) * ^A (1 - 2) ^ 3 s ₃ h.

The invention solves the simple, expressive, sensitive spectrophotometric determination and detection of a group of biologically active compounds that find use in medicine, pharmacy, can also be misused as drugs and agents in diverse events or for terrorist attacks. Thus, the invention may be included in the fields of clinical biochemistry, pharmaceutical analysis, chemical toxicology, chemical control.

Hitherto known methods for the detection, identification and determination of lysergic acid derivatives, including lysergamides, are based on classical color reactions with sulfuric acid and formaldehyde / WEBER, Q., W., A. - HEERAU, J., E., J. Pharm. Sci 62, 1973, p. 1174], by modifications according to the Winkler reaction (FRIEDMAN, M. FINLEY, J., W., J. Agr. Food Chem, 19, 1971, p. 626, Keller reactions (CONCON, J., M., Anal. Biochem. 67, 1975, p. 206, FAUBERT, M. J. Pharm. Pharmacol., 26, 1974, 637].

Other physicochemical methods of identification, detection or determination have been developed for the analysis of diethyllysergamide and other lysergic acid derivatives. Thin-layer and column chromatography including mass spectrometry is suitable and reliable. Less suitable is gas chromatography / SPEILING, A., J .: J. Chromatogr. Sci. 10, 1972, p. Volumetric methods are suitable for semi-quantitative methods of analysis. It is necessary to work with a solution volume of at least 5 cni and a concentration above 5.10 mol.dm. A suitable method for potentiometric titration of generally organic bases with sodium tetrafenylborate to a potassium ion selective electrode has been published / VYTŘÁS, K.: Coll. Czech. Chem. Commun. 42, 1977, 3168]. Spectrofluorimetry methods have also been developed for the analysis of lysergamides / BAUDOT, Ph. - ANDRE, J., C .; Analyt. Letters A 15, 1982, p. 471), infrared spectrometry.

/ CROM, C., C. - TURNEY, F., G.I. Forensic. Sci. 15, 1970, p. 530], mass spectrometry (BELIMAN, S., W .: J. Assoc. Offic. Analyt. Chem. 51, 1968, pp. 164 /.

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These methods of analysis are time-consuming, requiring qualified staff and special analytical equipment. This does not give the possibility to use it in the laboratory operation at the basic stage, where only the thin-layer chromatography is available from the mentioned methods. The above drawbacks are overcome by the analysis method of the invention.

The present invention is a method of analyzing diethyllysergamidu sulfophthaleines, which comprises, from the aqueous solution diethyllysergamidu treated with an aqueous or methanolic solution sulfophthaleines formula (C ₆ H _(a _ _4). 0H ₍₁ _ _2). X _{(l. 2)} J ₃ deg. SOjH. _{Μβ χ} is a halogen atom selected from chlorine, bromine, iodine and the ion associate is extracted with a solvent selected from benzene, chloroform, 1,1,2,2-tetrachloroethane, carbon tetrachloride, toluene or xylene and, after removal of the aqueous phase was measured colorimetrically by the color intensity of the solution of the ionic associate diethyllysergamide and sulfophthalein.

The advantage of the elaborated ‘‘ procedure is the possibility to determine diethyllysergamide up to a concentration of 1.10 mol mol.dm ’ The time required to perform the analysis is 3 to 5 minutes. It has been verified that it is possible to distinguish lysergic acid derivatives, including lysergamides, in addition to structurally close indole alkaloids, strychnine, brucine and physostigmine up to a 100 fold excess.

The use of the proposed oxtraction spectrophotometric method for the analysis of diethyllysergamide is novel. Available literature does not mention its application in technical practice. The use of the method of analysis according to the invention is beneficial in the possibility of expressing the evaluation of a sample which contains diethyllysergamide from a limit concentration of 1.10 < -1 > mol.dm at a precision. The resulting associate has the formula:

BH> 31 ^C 6 ^H

OH (1-2) (1-2)] ₃ c.s};

8) where

OH,

X is BH proionizovaná form diethyllysergamidu ^(5θ Η (2-4) + (1-2) · • ^x (2j-l | ^c 3 ^S0 3 sulfof talein ^and (S) ₍₂ _G) of solvated molecules of an organic solvent selected from benzene, chloroform, 1,1,2,2-tetrachloroethane, carbon tetrachloride, xylene or toluene.

- 3 Example 1

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-4 3

An aqueous solution of a 1.10 mol.dm sample of diethylly3 sergamide was prepared. A 0.1 cm sample solution was pipetted and 3 was added

1.9 cm 3, 3,5,5-tetrabromocresol 3 sulfophthalein buffer citrate pH 2 and shaken with 2.0 cm chloroform for 1 minute.

After the aqueous layer was removed, the absorbance at 415 nm was measured. The minimum detectable concentration was 1.81.10 -3 -3 mol.dm, which corresponds to 600 ng.cm · The slope of the calibration curve -1 -1 was 18,000 l.m & l .cm. The determination is disturbed by the others for the toned organic bases which need to be separated from the sample in advance *

Example 2

-5 -3 3

An aqueous solution of 1.10 mol.dm diethyllysergamide was pipetted after 0.4 cm and 0.1 cm of a methanol solution of 3.3.5.5 * 3 was added.

- triple bromophenolsulfophthalein and make up to 2,0 cm with buffer o

pH 2.5. The aqueous mixtures were shaken with 2.0 cm chloroform in one minute. Absorbance of chloroform extracts was measured at 420 nm. The lowest detectable con-6 -3 -3 centration was 1.00.10 mol.dm or 378 ng.cm. Guideline

-1 -1 of the calibration curve It was 5000 l.mol .cm.

Example 3

Q

The real operating sample was imitated so that to 1 cm of blood plasma

-4 * 3 was pipetted 0.1 cnr of an aqueous solution of 1.00 “mol.dm” diethyl3 of 3 lysergamide, taken in increments of 0.1 cm and added in 0.1 cm increments of aqueous • 4 -3 # solution of 4.10 'mol.dm' 3,3-dibromothymolsulfophthalein and supplemented with citrate buffer pH 5.0 per 2.0 cm ³ . The aqueous layers were extracted with 2.0 cm of chloroform, 1,1,2,2-tetrachloroethane, carbon tetrachloride, benzene, toluene and xylene. Extraction into chloroform and 1,1,2,2-tetrachloroethane proceeded with 100% efficiency, carbon tetrachloride 64%, benzene 59%, toluene 48%, xylene 41%. The lowest detectable concentration at 100% efficacy-3 ~ 3 extractivity was 1.96.10 “mol.dm”, ie 634 ng.cm ”·

At the lowest efficiency, there was a decrease in the value of the extraction nroconta, but also the molar absorption coefficient, and therefore the limit of determination here was 2.04.10 mol.dm, which is 660 ng.cm.

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Calibration curve guidelines of ionic associates of the formula © KaiiD

M ^(C 6 ^H L (2.4) * ^W "(L-2) · ^x (L-2j3 * ^{B '3]} f ^S) (2-8) amounted to extraction with chloroform and 1,1,2,2- tetrachloroethane

OH,

SO,

000l.mol ¹ .cm ” ¹ ,

520 1.mol ” ¹ .cm ¹

620 lmol 7 380 lmol ¹ cm cm benzene, 8 xylene.

tetrachloroethane, 600 l.mol ^{1 1} of toluene and .cm

Example 4

The process sample was imitated by adding 5 cm of a 5 cm 3 flow of 5.10 diethyllysergamide to 25 cm of urine. From there, 0.4 cm of the sample operating solution was pipetted and 0.1 cm methanol of cresolsulfophthalein methanol added and citrate buffer pH 3 added. 0. The aqueous layers were shaken for one minute with 2.0 cm chloroform. After aspiration of the aqueous layer, associate solutions were measured at 405 nm. The limit of determination of 6 -3-3 -3 was 3.6.10 mol.dm or 1.2 yug.cm. The slope of the calibration curve was 7,800 l.mol ¹ .cm ¹ .

Example 5

A real sample of diethyllysergamide was imitated so that 1.0 g of sucrose was homogenized with 100 mg of diethyllysergamidium tartrate.

A 10 mg sample was weighed, dissolved in water and made up to 50 ml

3

100,0 cm. For the determination, 0.1 cm was pipetted, 0.1 cm methanol solution of 1.10 mol.dm -3,3-dibromocresols sulfophthalein was added and the citrate buffer was adjusted to 2.0 cm. Chloroform extracts were measured at 410 nm. The relative standard deviation was - 4.37%.

The method of analysis according to the invention meets the requirements of automation and efficiency, expressed in terms of the number of samples that can be processed per hour, in terms of methodological arrangements. 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 up to A Q to be used up to a limit concentration of 1.10 mol.dm diethyllysergamide in the sample

Claims (1)

A method for the analysis of diethyllysergamide sulf of taleins, characterized in that an aqueous or methanolic solution of diethyllysergamide is treated with an eulfophthalein of formula ^C 6 ^H (2-4) · ^OH (1-2) * ^X (1-2) J 3 ^C ' ^SO 3 ^H wherein X is a halogen atom selected from chlorine, bromine, iodine and the ion associate is extracted with a solvent selected from benzene, chloroform, 1,1,2,2-tetrachlorethaa, carbon tetrachloride, xylene or toluene, and after removing the aqueous phase The color intensity of the solution of the ionic association of diethyllysergamide and sulfophthalein is measured colorimetrically.