RU2510018C1 - Method of determining lithium ascorbate in drug formation by voltammetry - Google Patents
Method of determining lithium ascorbate in drug formation by voltammetry Download PDFInfo
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- RU2510018C1 RU2510018C1 RU2012145221/28A RU2012145221A RU2510018C1 RU 2510018 C1 RU2510018 C1 RU 2510018C1 RU 2012145221/28 A RU2012145221/28 A RU 2012145221/28A RU 2012145221 A RU2012145221 A RU 2012145221A RU 2510018 C1 RU2510018 C1 RU 2510018C1
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- lithium ascorbate
- voltammetry
- ascorbate
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- IHAQDFLGBNNAEH-RXSVEWSESA-M lithium (2R)-2-[(1S)-1,2-dihydroxyethyl]-4-hydroxy-5-oxo-2H-furan-3-olate Chemical compound O=C1C(O)=C([O-])[C@H](O1)[C@@H](O)CO.[Li+] IHAQDFLGBNNAEH-RXSVEWSESA-M 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000004832 voltammetry Methods 0.000 title claims abstract description 10
- 229940079593 drug Drugs 0.000 title description 2
- 239000003814 drug Substances 0.000 title description 2
- 230000015572 biosynthetic process Effects 0.000 title 1
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 10
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 5
- 239000001103 potassium chloride Substances 0.000 claims abstract description 5
- 238000002360 preparation method Methods 0.000 claims abstract description 4
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical class [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims abstract 2
- 239000002552 dosage form Substances 0.000 claims description 15
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 229910021397 glassy carbon Inorganic materials 0.000 abstract description 4
- 239000013583 drug formulation Substances 0.000 abstract 2
- 239000000126 substance Substances 0.000 abstract 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 6
- 229910052744 lithium Inorganic materials 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000001075 voltammogram Methods 0.000 description 3
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 235000015872 dietary supplement Nutrition 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 208000020016 psychiatric disease Diseases 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 208000017194 Affective disease Diseases 0.000 description 1
- 208000007848 Alcoholism Diseases 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 208000027465 Psychotic Affective disease Diseases 0.000 description 1
- 208000028017 Psychotic disease Diseases 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 208000024823 antisocial personality disease Diseases 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- BTZWIZOMVVQOAZ-UHFFFAOYSA-L dichlorosilver Chemical class Cl[Ag]Cl BTZWIZOMVVQOAZ-UHFFFAOYSA-L 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 208000035475 disorder Diseases 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 125000002587 enol group Chemical group 0.000 description 1
- 206010015037 epilepsy Diseases 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000000506 psychotropic effect Effects 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Description
Способ определения аскорбата лития в лекарственной форме методом вольтамперометрииMethod for determination of lithium ascorbate in dosage form by voltammetry
Изобретение относится к области количественного определения аскорбата лития с выраженными антиоксидантными свойствами в лекарственной форме. Метод определения - вольтамперометрия.The invention relates to the field of quantitative determination of lithium ascorbate with pronounced antioxidant properties in a dosage form. The determination method is voltammetry.
В настоящее время препараты лития широко используются в терапии психических заболеваний, лечении аффективных психозов. Имеются данные об эффективности лития не только при эндогенных психических расстройствах, но и у больных с органическими психозами, эпилепсией и различными психопатиями. Применяют препараты лития также для профилактики и лечения эффективных нарушений у больных хроническим алкоголизмом.Currently, lithium preparations are widely used in the treatment of mental illness, the treatment of affective psychoses. There is evidence of the effectiveness of lithium not only in endogenous mental disorders, but also in patients with organic psychoses, epilepsy, and various psychopathies. Lithium preparations are also used for the prevention and treatment of effective disorders in patients with chronic alcoholism.
На фиг. 1 представлена структурная формула аскорбата лития.In FIG. 1 shows the structural formula of lithium ascorbate.
Выявлено, что от содержания чистого компонента - аскорбата лития в лекарственной форме зависит качество препарата по проявлению антиоксидантных и психотропных свойств. В связи с этим актуальным является контроль содержания аскорбата лития в лекарственной форме.It was revealed that the quality of the drug for the manifestation of antioxidant and psychotropic properties depends on the content of the pure component - lithium ascorbate in the dosage form. In this regard, it is relevant to control the content of lithium ascorbate in the dosage form.
В настоящее время нет методик количественного определения аскорбата лития в лекарственных формах или в БАД. Существуют методы определения лития в сплавах, почвах или сточных водах (ГОСТ 8775.1-87. Литий. Методы определения). Настоящий стандарт устанавливает титриметрический метод определения лития в сплавах, почвах и сточных водах, однако его невозможно использовать для определения аскорбата лития в лекарственной форме.Currently, there are no methods for the quantitative determination of lithium ascorbate in dosage forms or in dietary supplements. There are methods for determining lithium in alloys, soils, or wastewater (GOST 8775.1-87. Lithium. Methods for determination). This standard establishes a titrimetric method for the determination of lithium in alloys, soils and wastewater, but it cannot be used to determine lithium ascorbate in a dosage form.
Для обеспечения контроля качества лекарственных форм аскорбата лития необходимо разработать вольтамперометрическую методику количественного определения аскорбата лития в лекарственных формах.To ensure the quality control of dosage forms of lithium ascorbate, it is necessary to develop a voltammetric method for the quantitative determination of lithium ascorbate in dosage forms.
Новая техническая задача - разработка способа определения аскорбата лития в таблетированной лекарственной форме методом вольтамперометрии.A new technical problem is the development of a method for determining lithium ascorbate in a tablet dosage form by voltammetry.
Способ измерений молярной концентрации аскорбата лития в пробах лекарственной формы основан на измерении вольтамперометрического сигнала окисления енольной группы аскорбата лития, используя метод добавок, в диапазоне концентраций от 2,1·10-4 до 17·10-6 моль/дм3.The method for measuring the molar concentration of lithium ascorbate in samples of the dosage form is based on measuring the voltammetric signal of the oxidation of the enol group of lithium ascorbate using the addition method in a concentration range from 2.1 · 10 -4 to 17 · 10 -6 mol / dm 3 .
Определению не мешают другие функциональные группы органических соединений лекарственной формы (-СOOH, -СН2OH, -OLi).Other functional groups of the organic compounds of the dosage form (—COOH, —CH 2 OH, —OLi) do not interfere with the determination.
Поставленная задача достигается тем, что аскорбат лития переводят из таблетированной формы в раствор и проводят вольтамперометрическое определение. Проводят анодную вольтамперометрию на индикаторном стеклоуглеродном электроде при потенциале +0,24 В относительно насыщенного хлорид-серебряного электрода на фоне хлористого калия 0,1 моль/дм3 при постояннотоковой форме развертки потенциала со скоростью 30 мВ/с с областью определяемых содержаний аскорбата лития от 2,1·10-4 до 17·10-6 моль/дм3.The problem is achieved in that the lithium ascorbate is transferred from the tablet form into the solution and voltammetric determination is carried out. Anodic voltammetry is carried out on an indicator glassy carbon electrode at a potential of +0.24 V relative to a saturated silver chloride chloride electrode on the background of potassium chloride 0.1 mol / dm 3 with a constant current potential sweep form at a speed of 30 mV / s with a range of detected lithium ascorbate contents from 2 , 1 · 10 -4 to 17 · 10 -6 mol / dm 3 .
Наглядные вольтамперограммы окисления аскорбата лития от его концентрации в ячейке в условиях постояннотоковой вольтамперометрии на стеклоуглеродном электроде приведена на фиг.2.Visual voltammograms of the oxidation of lithium ascorbate from its concentration in the cell under conditions of constant current voltammetry on a glassy carbon electrode are shown in FIG. 2.
Область прямолинейной зависимости тока окисления аскорбата лития от его концентрации в электрохимической ячейке достаточна для применения методики при оценки количественного содержания аскорбата лития в лекарственной форме.The area of the linear dependence of the oxidation current of lithium ascorbate on its concentration in the electrochemical cell is sufficient for applying the technique to assess the quantitative content of lithium ascorbate in the dosage form.
Значения пределов повторяемости, воспроизводимости и критического диапазона измерений концентрации аскорбата лития при доверительной вероятности Р=0,95 представлена в табл.1.The values of the repeatability, reproducibility, and critical range of measurements of the concentration of lithium ascorbate with a confidence probability of P = 0.95 are presented in Table 1.
Пример. Определение аскорбата лития в таблетированной лекарственной форме «Аскорбат лития».Example. Determination of lithium ascorbate in tablet dosage form “Lithium ascorbate”.
Одну таблетку растирают в ступке до получения порошка. Порошок взвешивают и переносят в колбу 50 мл, добавляют 10-15 см3 в буферном растворе хлористого калия 0,1 моль/дм3и нагревают на водяной бане при температуре 45-50°С в течение 10 минут. После этого раствор фильтруют через бумажный фильтр, который промывают буфером два раза по 5 мл. Затем в кварцевый стаканчик вместимостью 20 мл вносят 10,0 мл раствора фонового электролита в растворе хлористого калия 0,1 моль/дм3 и помещают в электрохимическую ячейку вольтамперометрического анализатора (ТА-2, г. Томск). Опускают в раствор электроды: индикаторный - стеклоуглеродный электрод, вспомогательный и электрод сравнения - насыщенные хлорид- серебряные. Регистрацию фоновой линии проводят в постояннотоковом режиме съемки при линейной скорости развертки потенциала 30 мВ/с. Отсутствие пиков на вольтамперограмме и воспроизводимые кривые свидетельствовали о чистоте фона. После получения удовлетворительных кривых фона вносят аликвоту фильтрата аскорбата лития объемом 0,1 мл. Перемешивают раствор 10 с газом азотом, успокаивают 20 с и снимают вольтамперограмму в тех же условиях. Анодный пик регистрируют в при потенциале +0,24 В. Концентрацию аскорбата лития оценивали по высоте анодного пика методом добавок аттестованных смесей аскорбата лития по общепринятой методике.One tablet is ground in a mortar to obtain a powder. The powder is weighed and transferred to a 50 ml flask, 10-15 cm 3 are added in a 0.1 mol / dm 3 potassium chloride buffer solution and heated in a water bath at a temperature of 45-50 ° C for 10 minutes. After that, the solution is filtered through a paper filter, which is washed with a buffer twice in 5 ml. Then, 10.0 ml of a background electrolyte solution in a potassium chloride solution of 0.1 mol / dm 3 is added to a quartz glass with a capacity of 20 ml and placed in the electrochemical cell of a voltammetric analyzer (TA-2, Tomsk). The electrodes are lowered into the solution: indicator - glassy carbon electrode, auxiliary and reference electrode - saturated silver chloride. The background line is recorded in constant current mode at a linear potential sweep speed of 30 mV / s. The absence of peaks in the voltammogram and reproducible curves indicated the purity of the background. After obtaining satisfactory background curves, an aliquot of 0.1 ml lithium ascorbate filtrate is added. The solution 10 is mixed with nitrogen gas, calmed for 20 seconds and the voltammogram is taken under the same conditions. The anode peak is recorded at a potential of +0.24 V. The concentration of lithium ascorbate was estimated by the height of the anode peak by the addition of certified mixtures of lithium ascorbate according to the generally accepted method.
Предложенный способ количественного определения аскорбата лития отличается простотой, не требует больших трудозатрат, значительного количества реактивов и отличается высокой экспрессностью и чувствительностью.The proposed method for the quantitative determination of lithium ascorbate is simple, does not require large labor costs, a significant number of reagents, and is characterized by high expressivity and sensitivity.
Предложенный способ может быть использован для количественного определения аскорбата лития в БАД и лекарственных формах.The proposed method can be used for the quantitative determination of lithium ascorbate in dietary supplements and dosage forms.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2224997C1 (en) * | 2002-06-06 | 2004-02-27 | Томский политехнический университет | Volt-ampere method determining summary activity of antioxidants |
| JP2006029981A (en) * | 2004-07-15 | 2006-02-02 | Taisho Pharmaceut Co Ltd | Analytical method and component of common cold drug component |
| US7998513B1 (en) * | 2007-07-10 | 2011-08-16 | Primordial Diagnostics, Inc. | Ascorbate monitoring and control system |
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2012
- 2012-10-25 RU RU2012145221/28A patent/RU2510018C1/en not_active IP Right Cessation
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2224997C1 (en) * | 2002-06-06 | 2004-02-27 | Томский политехнический университет | Volt-ampere method determining summary activity of antioxidants |
| JP2006029981A (en) * | 2004-07-15 | 2006-02-02 | Taisho Pharmaceut Co Ltd | Analytical method and component of common cold drug component |
| US7998513B1 (en) * | 2007-07-10 | 2011-08-16 | Primordial Diagnostics, Inc. | Ascorbate monitoring and control system |
Non-Patent Citations (1)
| Title |
|---|
| ГОСТ 8775.1-87. ЛИТИЙ. Методы определения лития с.1-4. * |
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