SU1337739A1 - Method of determining amitryptelene in medicinal compounds - Google Patents

Abstract

The invention relates to analytical chemistry, in particular the determination of amitrile titration in medicinal preparations. The analysis is carried out by processing the sample with potassium bichromate in a solution of conc. with subsequent measurement of the relative fluorescence intensity, the method increases the detection sensitivity by a factor of 20, and the fluorescence intensity of the solution does not change within 24 hours. 3 tab. (L with h with SO

Description

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The invention relates to analytical chemistry, namely to methods for determining amitriptyline 5- (3-dimethylaminopropylide) -10, 1 1-dihydrodibenzocycloheptene, and can be used in the analysis of drug preparations containing amitriptyline.

The purpose of the invention is to increase the sense of vitality of the definition.

Example 1. A qualitative definition of amitriptyline,

To a grain of finely divided tablets, a drop of amitriptyline solution or a grain of powder, 1 ml of glacial acetic acid is added and shaken. Then to the resulting solution was added 1.5 ml of concentrated sulfuric acid and 0.2 ml of 0.1 N. solution of potassium dichromate. When the resulting solution was irradiated with ultraviolet light from a long wavelength of 360 nm, a pale orange fluorescence was observed, indicating the presence of amytryptine in the sample under study.

PRI mme R 2. Quantitative determination of amitriptyline in powder.

0.001 g (exact weight) of amitriptyline powder is quantitatively transferred to a 100 ml volumetric flask, 70-80 ml of glacial acetic acid are added, and shaken until the preparation is dissolved. The volume of the solution is adjusted to the mark with the same solvent. To 1 ml of the resulting solution. 1.5 ml of concentrated sulfuric acid and 0.2 ml of 0.1 N are added. potassium dichromate solution, shake. The volume is made up to 10 ml with distilled water. The relative intensity of the solution is measured. A standard solution of amitriptyline prepared in the same way is used as a comparison solution.

The quantitative content of amitriptyline powder calculated by the formula:

for G7 - i l-I-fisI-Sli02

    (H, - HJ m where X (%) is the percentage

amitriptyline powder; a is the weight of the standard amitriptyline, g; m is the sample of the amitriptyline powder under study, g; H. H, H., - Electrofluorometer readings for the test

5 about 5

Q 39

test, standard test and single experience.

The results of the determination of amitriptyline powder are given in Table 1.

The determinations are carried out using a KIAN-130 electro-fluorometer.

PRI me R 3. Quantitative determination of amitriptyline in pills of 0.025 g.

0.04 g (exact weight) of powdered dragee powder is transferred to a 100 ml volumetric flask, 70 to 80 ml of glacial acetic acid is added, and shaken for 10 minutes. The volume of the solution is made up to the mark with the same acid. The resulting solution of the analyte is filtered through a folded filter, discarding the first 10-15 ml of filtrate. To 1 ml of the obtained solution add 1.5 ml of concentrated sulfuric acid and 0.2 ml of 0.1N. potassium dichromate solution. Shake the mixture. The volume of the solution is made up to 10 ml with distilled water. The fluorescence intensity of the resulting solution is measured relative to a similarly prepared standard solution of amitriptyline.

The mass of amitriplitin contained in 1 g of dragees is calculated by the formula: .a

X

(H, - H „)

five

0

five

0

five

 about where X is the content of amitriptyline in

I g dragee, g; in - the average weight of dragee, g; a - sample of amitriptyline standard, taken for analysis, g; c - a portion of amitriptyline dragee powder, g;

H ,, Hj, Nd - readings of an electrofluorometer, respectively, for the test solution, standard solution, and blank.

The results of the determination of amitriptyline in pills of 0.025 g are shown in Table 2.

PRI me R 4. Quantitative determination of amitrigtiline in 1% solution for injection.

1 ml of the solution of amitri 1-thylin for injection is transferred into a 100-ml volumetric flask and brought to about 1 ml of the solution up to the mark of ice acetic acid. The mixture is thoroughly mixed. To 1 ml of the obtained solution was added 1.5 ml of concentrated nano-acid and 0.2 ml of 0.1 N. raso rnojia potassium dichrome

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that The volume of the solution is adjusted to the mark with distilled water. The fluorescence intensity of the resulting solution is measured relative to a solution of a standard sample of amitriptyline prepared in a similar manner. Parallel set blank experience.

The content of amitriptyline in 1 ml of injection solution is calculated by the formula:

V 1H, - But) a

(N, - H „) where a is the standard sample weight

amitriptyline, g;

Hf, Hj, readings of an electrofluorimeter for the test solution of the standard blank solution.

The results of the determination of amitriptyline in ampoules are shown in Table 3.

Preparation of the standard solution of amitriptyline 0.01 g (exact weight) of the standard amitriptyline-peroxide is quantitatively transferred to a 100 ml volumetric flask, and 70-80 ml of glacial acetic acid is added. Shake until the substance is dissolved, after which the volume of the solution is made up to the mark with the same solvent. 1.5 ml of concentrated sulfuric acid and 0.2 ml of 0.1 N were added to the 1 ml solution obtained. potassium dichromate solution and shake. The volume of the solution is made up to 10 ml with distilled water.

0,0123

0,0118

0,0102

0,0137

0,0101

0,0098

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The intensity of the fluoroscale is not PCRM - for 24 hours.

The sensitivity of the previous method of determining the amitriptyline in medicinal preparations is 20 times higher than the sensitivity of the known method, based on the ratio of the limits of the linear dependence of the gauge

. , IlO µg / ml,

graphs (r- -rr;) t In addition,

0.05 µg / ml

the method is carried out by simple operations, does not require expensive reagents, which generally determines the feasibility of its use in the practice of control and analytical laboratories engaged in quality control of drugs.

Claims (1)

DETAILED DESCRIPTION A method for determining amitriptyline in medicinal preparations by dissolving an analyzed sample, treating it with a chemical reagent, followed by analyzing the resulting solution, characterized in that, in order to increase the sensitivity of the determination, dissolution is carried out in glacial acetic acid, the chemical reagent is used potassium dichromate, they are processed in the presence of concentrated sulfuric acid and the analysis is carried out by measuring the relative intensity of fluorescence. Table X 99.33%, 24 S 1.11 From 0.45 1.16 a 99.33% + 1.16% Sample amitriptilina, g 0.02537 0.02487 0.02519 0.02521 0.02563 0.02543 Table 3 Defined Defined Metrological-amitripti-amytryptics characteristics, glic,% tics 0.0097597.5I 98.35% 0.01025102.5S 4.76 0.0098898.8S 2.18 0.0097597, 9 2.29 0.00963 96.3 a 98.35 ± 0.00975 97.5 2.29% Compiled by L.Rusanova Editor L.Pcholinska Tehred M.Hodanich Proofreader S.Shekmar  i - .. gp- - t-t-. g-gtd gd - -.ju-imi mm -i t-yy .. Order 4122/40 Circulation 776 Subscription VNIIPI USSR State Committee for inventions and discoveries P3035, Moscow, Zh-35, Raushsk nab., 4/5 Production and printing company, Uzhgorod, st. Project, 4 table 2 Metrological characteristics X 101.3% S 1,069 S 1,034  0.9G 1,085 a 10J, 13 + ± 1,085%