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DEPENDENCE OF PURIFIED RUTIN QUALITY ON ACTIVATED CARBON BRAND
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DEPENDENCE OF PURIFIED RUTIN QUALITY ON ACTIVATED CARBON BRAND
UDK 66 Химическая технология. Химическая промышленность. Родственные отрасли
Averyanova E V 1
Shkolnikova M N 2
Frolov A V 3
Authors:
1.  Biysk Institute of Technology (branch), Polzunov Altai State Technical University

2.  Biysk Institute of Technology (branch), Polzunov Altai State Technical University

3.  Biysk Institute of Technology (branch), Polzunov Altai State Technical University

Type:
Article
DOI:
https://doi.org/10.21179/2308-4057-2017-1-165-173
Pages:
from 165 to 173
Status:
Published
Received:
29.06.2017
Accepted:
29.06.2017
Published:
29.06.2017
Subject area:
UDK 66 Химическая технология. Химическая промышленность. Родственные отрасли
Language:
English
Keywords:
Grass buckweat, rutin raw, activated carbon, purification, method of preparative chromatography
Abstract and keywords
Abstract (English):
The main problem of implementation of technology of rutin extraction from grass buckwheat Fagopyrum sagittatum Gilib. lies in purification of rutin raw. In this connection the following research object is determined: consideration of the possibility to use for rutin raw purification different commercial carbon brands as adsorbents by the method of preparative chromatography and assessment of their effectiveness to achieve the maximum degree of purification with minimum duration of the elution process. The article presents experimental data on purification of rutin raw sample, extracted from grass buckweat green material by the preparative chromatography method using wood- and coconut-based activated carbons of different brands as sorbents; besides, the following items are presented in the article: dependence of rutin sample melting temperature, qualitative and quantitative flavonoid content, authenticity on chlorophyll and red pigments content depending on sorbent layer height and elution duration in comparison with the GSO [State Standard Samples] control sample. To confirm the reliability of the obtained results, statistical processing of experimental data is conducted using the methods of correlation and regression analysis, as well as using the two-parameter normal distribution of values. It is demonstrated that the use of the following carbon brands, indicated in decreasing effectiveness order, can provide the best purity and stability of parameters values, characterizing the product: NWC-P, NWM-P, OU-A, OU-B; the conducted calculations indicate that the best correlation between the sorbent layer height in a column and the rutin samples quality parameter was achieved when the carbons of the brands NWM-P, OY-A and OY-B were used. Depending on the tasks, rutin purification degree may be regulated by sequential use of NWC-P and NWM-P carbons. When rutin is purified from proximate admixtures, chlorophyll and red pigments, NWC-P adsorbent allows to get a comparable result even when the layer height is from 50 to 70 mm respectively.

Keywords:
Grass buckweat, rutin raw, activated carbon, purification, method of preparative chromatography
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INTRODUCTION Nowadays, a special place in the pharmaceutical market is occupied by medicines and dietary supplements of plant origin, containing flavonoids, one of the most important qualities of which is the ability to increase strength of the capillary walls. P-vitamin activity of these medicines is associated with the antioxidant effect that is important in the treatment of chronic venous insufficiency, hypertension and other cardiovascular diseases, associated with the increased permeability of blood capillaries. The clearest representative of this group of substances is rutin, which not only has a pronounced capillary- strengthening, antioxidant and hepatoprotective action [1, 2], but also improves the treatment of various disorders, associated with physical fatigue [3]. Today the main industrial source of rutin is the buds of Japanese pagoda tree (Styphnolobium japonicum L.), however, there is no raw material base of this plant in our country. A promising domestic source of rutin and other flavonoids may be grass buckwheat (Fagopyrum sagittatum Gilib.), widely cultivated as a valuable food crop in the Russian Federation. It is known that the rutin content in the cultivated buckwheat sorts is from 2.0 to 8.7% on a dry basis. However, the sorts, the rutin content in which may be 12%, are selected [4, 5]. Despite the broad prospects of the use of grass buckwheat as a raw material for the rutin production, the main difficulty of the implementation of technology of rutin extraction lies in the stage of rutin raw purification and obtaining a product, suitable for use in pharmaceutical industry and dietary supplements production [6]. In view of this, studies have been conducted on the use of commercial carbons of different brands as adsorbents, used for rutin purification, by the method of preparative chromatography, as well as the assessment of their effectiveness to achieve the maximum degree of purification with minimum duration of the elution process was conducted. Copyright © 2017, Averyanova et al. This is an open access article distributed under the terms of the Creative Commons Attribution 4.0 International License (http://creativecommons.org/licenses/by/4.0/ ), allowing third parties to copy and redistribute the material in any medium or format and to remix, transform, and build upon the material for any purpose, even commercially, provided the original work is properly cited and states its license. This article is published with open access at http://frm-kemtipp.ru. OBJECTS AND METHODS OF STUDY The study objects were rutin raw samples, extracted by the above-mentioned method [7, 8] and purified by the method of preparative chromatography on a layer of wood- and coconut-based activated carbon of six brands. Physical and chemical parameters of the carbons are indicated in Table 1. Sample melting temperature was measured with the device PTP (M), qualitative and quantitative flavonoid content in the samples was measured by the method of HPLC on high performance liquid chromatograph Milikhrom A-02 with UV radiation and a chromatographic column from stainless steel O 2? 75 mm, filled with a reversed-phase sorbent ProntoSIL 120-5C18 AQ, with a software package. The solution of 0.1% acetic acid and acetonitrile was used as an eluent. Flavonoid retention time is 25 minutes. Chlorophyll and red pigments content was measured by spectrometric method. The readings were taken from the devices Shimadzu UV-2401 PC UV- VIS RECORDIGPHOTOMETER (Japan) at wave length of 560 nm, 590 nm, 620 nm, 655 nm and 690 nm in a cuvette with the layer thickness of 1 cm. Isopropyl alcohol was used as a comparison solution. Microscopic examination of rutin samples was conducted with the electron microscope SK 14 28804. Table 1. Physical and chemical parameters of activated carbons of different brands [9] Carbon brands Appearance Adsorption activity by methylene blue, mg/g Ash mass fraction, % Moisture mass fraction, % Bulk density, g/dm3 Abrasion capacity, % OU-A (GOST 4453-74) Black fine- grained powder 225.0 4.6 4.7 270 60 OU-B (GOST 4453-74) Black fine- grained powder 75.0 10.0 10.0 290 60 BAU-A (GOST 6217-74) Black grains 60.0 6.0 10.0 240 60 BAU-MF (GOST 6217-74) Black grains 70.0 10.0 10.0 Not regulated 60 NWC-P, FCC specification Black powder 300.0 5.0 15.0 300 > 99 NWM-P, FCC specification Black powder 280.0 10.0 15.0 300 > 96 RESULTS AND DISCUSSION Rutin raw was extracted from grass buckweat green material by double extraction with ethanol solution of 70%. The output was 4.44 ± 0.05% (on absolute dry substance), contain of main substance in a sample was 75.74%, melting point was 162°С, crystals were gray- and-green. According to regulating documentation requirements, the rutin content shall be at least 95.0% (State Pharmacopoeia XI); in the GSO [State Standard Sample] sample it was at least 98.5%. For purification of rutin raw we offered the method of preparative chromatography on a layer of activated carbons of different brands - ОU-А, OU-В, BAU-A, BAU-MF, NWC-P, NWM-P [10]. 99.5%-methanol was used as a solvent and eluent for chromatography. In a column with a height of 360 mm and diameter of 15 mm activated carbon is placed (layer height is from 10 to 100 mm). Rutin raw solution is applied to the prepared sorbent layer, eluent feed to the column is produced at a speed of 1 drop in a second. Sorbent layer height in a column corresponds with the number of the sample of purified rutin. After rutin raw purification with the use of activated carbons of different brands, the rutin samples were analyzed for compliance with the melting temperature, the content of flavonoids and authenticity on the presence of chlorophyll and red pigments in comparison with the GSO [State Standard Samples] control sample. All the used brands of carbons are activated and represented in 87-97 mas.% of composition of elements by carbon. The main structural element of the activated carbon sorption space at the organization molecular level is the graphite basal face, which is formed by carbon atoms in the state of sp2-hybridization with delocalized fourth electron. Non-specific physical adsorption is realised on them by means of universal forces of dispersion interaction. Besides, non-specific electrostatic induction forces are expressed in carbon like in conductor by means of dipole direction in the sorbate molecule. Their intensity is determined by polarization capacity. Carbons express capacity to sorption by means of addition of these forces. At the same time, oxigenated functional groups and Bronsted acids are present on the surface initially and appear during activation process by overheated moisture vapour. They are represented by hydroxyl, phenol, carboxyl, carbonyl and lactone groupings, content and balance of which are different for different carbon brands [11]. It should be noted that acidic properties of the carbon surface change in the following sequence: NWM-P
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