SU859889A1 - Method of 1-methyl-4-(n-methylpyrrolidil-1)- -carbolene hydrochloride quantitative determination - Google Patents

Method of 1-methyl-4-(n-methylpyrrolidil-1)- -carbolene hydrochloride quantitative determination Download PDF

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SU859889A1
SU859889A1 SU802871050A SU2871050A SU859889A1 SU 859889 A1 SU859889 A1 SU 859889A1 SU 802871050 A SU802871050 A SU 802871050A SU 2871050 A SU2871050 A SU 2871050A SU 859889 A1 SU859889 A1 SU 859889A1
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USSR - Soviet Union
Prior art keywords
hydrochloride
methyl
methylpyrrolidil
carbolene
quantitative determination
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SU802871050A
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Russian (ru)
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Анатолий Алексеевич Хабаров
Людмила Пантелеймоновна Хабарова
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Читинский Медицинский Институт
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  • Investigating Or Analysing Biological Materials (AREA)

Description

1 мл полученного состава прибавл ют 9 мл дистшшированнсЛ воды и 3 капли концентрированной азотной кислоты, перегмешивают и флуориметируют по отношению к стандартному водному раствору с сод жанием 5 мгк/мл бревиколлина гидрохлор ода к 10 мл которого гфибавлено 3 капли ксжцентрированной азотной кислоты, и флуориметрируют одновремен но с- испытуемыми растворами. Результаты определени  бревиколлина гидрохлорида в 1%-ном растворе представ лены в табл. 1. Пример 2. Определение бревиколлина гидрохлорида в крови и моче. К 1 мл плазмы крови или 1 мл мочи прибавл ют 2 капли ОД н.раствора едкоГ натра и 10 мл эфира и экстраг1фуют в течение 2 мин. Эфирный слой спивают в выпарительную чашку. Экстракцию повтор ют дважды. Эфир отгон ют на вод ной бане. К остатку прибавл ют 10мл дистиллированной воды, 3 кацли кониентриро шной азотной кислоты, перемешивают и флуориметрируют по отношению стандартных растворов с содержанием 0,5:1:3 или 5мкг/мл бреви коллина гидрохлорида. Дл  этого к 1О мл 8 94 стандартного раствора прибавл ют 3 капли концентрированной азотной кислоты и флуориметрируют одновременно с испытуемыми растворами. В искусственных смес х, при содержании более ОД мкг/мл бревиколлина гидрохлорида , си определ етс  полностью (100%). Спектр возбуждени  флуоресценции полученного раствора находитс  в области 28О -.430 нм с максимумом 380 нм, а спектр излучени  флуоресценции находитс  в области 400-520 нм с максимумом 44О нм. Пр молинейна  зависимость между интенсивностью флуоресценции и концентрацией бревиколлина гидрохлорида находитс  от 0,О1.до 8 мкг/мл (табл. 2 и 3). Интенсивность флуоресценции не измен етс  в течение 2ч. В лекарственной форме сопутствующие ингредиенты не вли ют на интенсивность флуоресценции. При содержании 0,1мкг/мп бревиколлин гидрохлорид в крови или моче открьшаетс  полностью (1ОО%), т.е. компоненты крови и мочи не вли ют на интенсивность флуоресценции. Чувствительность известного метода 0,5 мкг/мл, предлагаемого - О,01кмг-мл.1 ml of the resulting composition was added 9 ml of distributive water and 3 drops of concentrated nitric acid, stirred and fluoridated with respect to a standard aqueous solution containing 5 mcc / ml of Brevicollin hydrochloride, 10 ml of which was filled with 3 drops of concentrated nitric acid, and fluoridated simultaneously but with test solutions. The results of determination of brevicolline hydrochloride in a 1% solution are presented in Table. 1. Example 2. Determination of brevicolline hydrochloride in blood and urine. To 1 ml of blood plasma or 1 ml of urine, add 2 drops of OD of sodium hydroxide solution and 10 ml of ether and extract them for 2 minutes. The ether layer is drunk in a evaporation cup. Extraction is repeated twice. The ether is distilled in a water bath. To the residue was added 10 ml of distilled water, 3 batches of conentric nitric acid, stirred and fluoridated using standard solutions with a content of 0.5: 1: 3 or 5 µg / ml brevicollin hydrochloride. To this end, 3 drops of concentrated nitric acid are added to 1O ml of 894 standard solution and fluoridated simultaneously with the test solutions. In artificial mixtures, with a content of more than OD µg / ml of brevicolline hydrochloride, si is determined completely (100%). The fluorescence excitation spectrum of the solution obtained is in the region of 28O-430 nm with a maximum of 380 nm, and the fluorescence emission spectrum is in the region of 400-520 nm with a maximum of 44O nm. The linear relationship between fluorescence intensity and the concentration of brevicolline hydrochloride is from 0, O1 to 8 µg / ml (Tables 2 and 3). The fluorescence intensity does not change for 2 hours. In the dosage form, the concomitant ingredients do not affect the fluorescence intensity. With a content of 0.1 µg / mp, brevicolline hydrochloride in the blood or urine is completely cleared (1OO%), i.e. blood and urine components do not affect the fluorescence intensity. The sensitivity of the known method of 0.5 µg / ml, proposed - Oh, 01kmg-ml.

Флусриметрйческое определение бревиколлина гидрохлорида в 1%-«ом растворе (на исследование вз то По 0,3 мл 1%-ного раствора).Fluusimetric determination of brevicolline hydrochloride in 1% - ом om solution (for the study taken 0.3 ml of 1% solution).

0,0098 О,О098 О,О1ОО О,О098 О,ОО96 0,ОО96 О,0098 О,ОО98 0,ОО96 О,ОО980,0098 О, О098 О, О1ОО О, О098 О, ОО96 0, ОО96 О, 0098 О, ОО98 0, ОО96 О, ОО98

Таблица ITable I

0,О097 2. Ю0, O097 2. U

.-.-

IlOIlo

.-4.-four

0,ОО97 Ila0, GO97 Ila

85988968598896

Завйснмосгь ингенснвносги фпуоресценцив бреви- коплина гидрохлорида ( мкг/мл) ог конпентрач-, ции азогмой кислоты,Investigating the inhibition of fluorescence of brevicopline hydrochloride (µg / ml) og concentration, azoma acid,

Количество капель концентрированной азотной кислотыThe number of drops of concentrated nitric acid

II

2;2;

3 43 4

5 Зависимость интенсивности флуоресценции от в растворе азотной кислоты5 The dependence of the fluorescence intensity on the solution of nitric acid

Таблица 2table 2

Относительна  интенсивность флуоресценцииRelative fluorescence intensity

62 85 90 90 76 t Таблица 3 концентрации бреваколлнна гвдрохлорида .62 85 90 90 76 t Table 3 Concentrations of brevacolline hydrochloride.

Claims (1)

Формула изобретенияClaim Способ количественного определения 1-метил-4-(Ν-метилпирролидил-1)-(1 - . -карболки гидрохлоридапутем обработки анализируемой пробы химическим реагентом, отличающийся тем, что, с целью повышения чувствительности и избирательнортй определения, в качестве химического реагента используют азотную СоставитеMethod for the quantitative determination of 1-methyl-4- (Ν-methylpyrrolidyl-1) - (1 -.-Capsules with hydrochloride adapting to the test sample by a chemical reagent, characterized in that, in order to increase the sensitivity and selectivity of determination, a nitrogen reagent is used as a chemical reagent
SU802871050A 1980-01-17 1980-01-17 Method of 1-methyl-4-(n-methylpyrrolidil-1)- -carbolene hydrochloride quantitative determination SU859889A1 (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1991014184A1 (en) * 1990-03-16 1991-09-19 Board Of Regents, The University Of Texas System Beta carbolines as vital stains for neurotransmitter systems
WO1998006719A1 (en) * 1996-08-09 1998-02-19 Boehringer Ingelheim Pharmaceuticals, Inc. 4-substituted beta-carbolines as immunomodulators
MD4009C2 (en) * 2008-07-15 2010-08-31 Институт Химии Академии Наук Молдовы Use of 1-methyl-4-(N-methylaminobutyl-4)-b-carboline as antituberculous remedy

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1991014184A1 (en) * 1990-03-16 1991-09-19 Board Of Regents, The University Of Texas System Beta carbolines as vital stains for neurotransmitter systems
WO1998006719A1 (en) * 1996-08-09 1998-02-19 Boehringer Ingelheim Pharmaceuticals, Inc. 4-substituted beta-carbolines as immunomodulators
US6093723A (en) * 1996-08-09 2000-07-25 Boehringer Ingelheim Pharmaceuticals, Inc. 4-substituted beta-carbolines and analogs thereof
MD4009C2 (en) * 2008-07-15 2010-08-31 Институт Химии Академии Наук Молдовы Use of 1-methyl-4-(N-methylaminobutyl-4)-b-carboline as antituberculous remedy

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