ОПРЕДЕЛЕНИЕ ГАЛОНАЛА И БЕНЗОНАЛА В ТАБЛЕТИРОВАННЫХ ФОРМАХ ЛЕКАРСТВЕННЫХ ПРЕПАРАТОВ МЕТОДОМ ИНВЕРСИОННОЙ ВОЛЬТАМПЕРОМЕТРИИ

A possibility of applying the stripping voltammetry method for the determination of benzylated derivatives of phenobarbital (benzonal and halonal) in tableted forms of medicinal drugs was shown. The regularities of the physicochemical behavior of the barbiturates on the glassy carbon electrode depending on the pH of the solution were studied, and the following accumulation parameters with an analytical value were estimated: the range of variation in the accumulation potential and the accumulation time as well as the voltammetric mode. It was established that the character of the dependence of the magnitude of the electroreduction currents of the barbiturates studied had an adsorption character. The following working conditions were established: the background electrolyte was 0.1 M solutions of Na2SO3 or 0.1 M NaH2PO4, the accumulation potential was -0.6 V, the accumulation time was 30 s, the cathode differential-impulse sweep of the potentials was at the speed of 50 mV / s. A possible interfering effect of auxiliary substances of tableted forms on the voltammetric signal of halonal and benzonal was investigated: under the conditions of real contents of auxiliary and basic components of the tableted form the error in determining the halonal (benzonal) was 3-5% and did not exceed the error of the method. The methods of analysis of tableted forms of medicinal drugs for the content of halonal and benzonal by the method of differential-pulse voltammetry had been developed. The verification of the correctness of the developed algorithm was carried out by the " introduced-found" method. The analysis time of one sample, considering the sample preparation, did not exceed 15 minutes. The detection limit Cmin = 0.33 mg/l, limit of determination Сlim = 1.32 mg/l, and the range of determined concentrations - 2-200 mg/l were determined. The calculation of the basic metrological indices was carried out including the computation of indices of correctness, intralaboratory precision and repeatability.Keywords: Halonal, benzonal, barbituric acid, stripping voltammetry, glassy carbon electrode, dosage form, method of determination(Russian) DOI: http://dx.doi.org/10.15826/analitika.2018.22.2.011O.L. Mezentseva, G.B. Slepchenko, V.D. Filiminov, E.V. Miheeva, G.A. ArbitTomsk Polytechnic University, Lenin av., 30, Tomsk, 634050, Russian FederationПоказана возможность применения метода инверсионной вольтамперометрии для определения бензоилированных производных фенобарбитала (бензонал и галонал) в таблетированных формах лекарственных препаратов.  Изучены закономерности физико-химического поведения определяемых барбитуратов на стеклоуглеродном электроде в зависимости от рН раствора и оценены параметры накопления, имеющие аналитическое значение: диапазон изменения потенциала накопления и времени накопления, режим полярографирования. Найдено, что характер зависимости величины токов электровосстановления изучаемых барбитуратов носит адсорбционный характер. Установлены рабочие условия измерений: фоновый электролит – 0.1 М растворы Na2SO3 или 0.1 М NaH2PO4, потенциал накопления – -0.6 В, время накопления 30 с, катодная дифференциально-импульсная развертка потенциалов, со скоростью 50 мВ/с. Проведено исследование возможного мешающего влияния вспомогательных веществ таблетированных форм на вольтамперометрический сигнал галонала и бензонала: в условиях реальных содержаний вспомогательных и основных компонентов таблетированной формы, погрешность определения галонала (бензонала) составляет 3-5 % и не превышает погрешности метода. Разработаны методики анализа таблетированных форм лекарственных препаратов на содержание галонала и бензонала методом дифференциально-импульсной вольтамперометрии.  Проверка правильности разработанного алгоритма методики проведена методом «введено-найдено». Время анализа одной пробы с учетом пробоподготовки не превышает 15 минут. Определены: предел обнаружения Сmin = 0.33 мг/л, предел определения Сlim = 1.32 мг/л, диапазон определяемых концентраций – 2-200 мг/л; проведен расчет основных метрологических показателей: показатель правильности, внутрилабораторной прецизионности, повторяемости.   Ключевые слова: Галонал, бензонал, барбитуровая кислота, инверсионная вольтамперометрия, стеклоуглеродный электрод, лекарственная форма, методика определенияDOI: http://dx.doi.org/10.15826/analitika.2018.22.2.01

Determination of halonal and benzonal in tableted forms of medicinal drugs using the stripping voltammetry

A possibility of applying the stripping voltammetry method for the determination of benzylated derivatives of phenobarbital (benzonal and halonal) in tableted forms of medicinal drugs was shown. The regularities of the physicochemical behavior of the barbiturates on the glassy carbon electrode depending on the pH of the solution were studied, and the following accumulation parameters with an analytical value were estimated: the range of variation in the accumulation potential and the accumulation time as well as the voltammetric mode. It was established that the character of the dependence of the magnitude of the electroreduction currents of the barbiturates studied had an adsorption character. The following working conditions were established: the background electrolyte was 0.1 M solutions of Na2SO3 or 0.1 M NaH2PO4, the accumulation potential was -0.6 V, the accumulation time was 30 s, the cathode differential-impulse sweep of the potentials was at the speed of 50 mV / s. A possible interfering effect of auxiliary substances of tableted forms on the voltammetric signal of halonal and benzonal was investigated: under the conditions of real contents of auxiliary and basic components of the tableted form the error in determining the halonal (benzonal) was 3-5% and did not exceed the error of the method. The methods of analysis of tableted forms of medicinal drugs for the content of halonal and benzonal by the method of differential-pulse voltammetry had been developed. The verification of the correctness of the developed algorithm was carried out by the " introduced-found" method. The analysis time of one sample, considering the sample preparation, did not exceed 15 minutes. The detection limit Cmin = 0.33 mg/l, limit of determination Сlim = 1.32 mg/l, and the range of determined concentrations - 2-200 mg/l were determined. The calculation of the basic metrological indices was carried out including the computation of indices of correctness, intralaboratory precision and repeatability.Показана возможность применения метода инверсионной вольтамперометрии для определения бензоилированных производных фенобарбитала (бензонал и галонал) в таблетированных формах лекарственных препаратов. Изучены закономерности физико-химического поведения определяемых барбитуратов на стеклоуглеродном электроде в зависимости от рН раствора и оценены параметры накопления, имеющие аналитическое значение: диапазон изменения потенциала накопления и времени накопления, режим полярографирования. Найдено, что характер зависимости величины токов электровосстановления изучаемых барбитуратов носит адсорбционный характер. Установлены рабочие условия измерений: фоновый электролит - 0.1 М растворы Na2SO3 или 0.1 М NaH2PO4, потенциал накопления - -0.6 В, время накопления 30 с, катодная дифференциально-импульсная развертка потенциалов, со скоростью 50 мВ/с. Проведено исследование возможного мешающего влияния вспомогательных веществ таблетированных форм на вольтамперометрический сигнал галонала и бензонала: в условиях реальных содержаний вспомогательных и основных компонентов таблетированной формы, погрешность определения галонала (бензонала) составляет 3-5 % и не превышает погрешности метода. Разработаны методики анализа таблетированных форм лекарственных препаратов на содержание галонала и бензонала методом дифференциально-импульсной вольтамперометрии. Проверка правильности разработанного алгоритма методики проведена методом «введено-найдено». Время анализа одной пробы с учетом пробоподготовки не превышает 15 минут. Определены: предел обнаружения С min = 0.33 мг/л, предел определения С lim = 1.32 мг/л, диапазон определяемых концентраций - 2-200 мг/л; проведен расчет основных метрологических показателей: показатель правильности, внутрилабораторной прецизионности, повторяемости

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