Застосування тонкошарової хроматографії в аналізі ефавіренцу
Aim. To carry out the integrated study of visualization conditions of efavirenz on TLC-plates with aplication of standard and particular colored reagents, and the chromatographic behavior of efavirenz using standard mobile phases.Results and discussion. It has been shown that such widely used color...
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| Published in: | Журнал органічної та фармацевтичної хімії |
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| Date: | 2020 |
| Volume: | 18 |
| Issue: | 1(69) |
| Pages: | 58-62 |
| ISSN: | 2518-1548 |
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| Format: | Article |
| Language: | English |
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National University of Pharmacy
2020
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| author | Slabiak, Oksana I. Ivanchuk, Iryna M. Klimenko, Lina Yu. Mykytenko, Olena Ye. Antonenko, Olga V. |
| author_facet | Slabiak, Oksana I. Ivanchuk, Iryna M. Klimenko, Lina Yu. Mykytenko, Olena Ye. Antonenko, Olga V. |
| author_institution_txt_mv | [
{
"author": "Oksana I. Slabiak",
"institution": "Ivano-Frankivsk National Medical University",
"orcid": ""
},
{
"author": "Iryna M. Ivanchuk",
"institution": "Ivano-Frankivsk National Medical University",
"orcid": "0009-0006-4335-8119"
},
{
"author": "Lina Yu. Klimenko",
"institution": "National University of Pharmacy",
"orcid": "0000-0002-4857-5706"
},
{
"author": "Olena Ye. Mykytenko",
"institution": "National University of Pharmacy",
"orcid": "0000-0003-3178-3418"
},
{
"author": "Olga V. Antonenko",
"institution": "National University of Pharmacy",
"orcid": "0000-0002-0369-6520"
}
] |
| author_orcid_str_mv | 0009-0006-4335-8119 0000-0002-4857-5706 0000-0003-3178-3418 0000-0002-0369-6520 |
| author_sort | Slabiak, Oksana I. |
| baseUrl_str | https://ophcj.nuph.edu.ua/oai |
| collection | OJS |
| container_end_page | 62 |
| container_issue | 1(69) |
| container_start_page | 58 |
| container_title | Журнал органічної та фармацевтичної хімії |
| container_volume | 18 |
| datestamp_date | 2026-08-24T18:04:29Z |
| description | Aim. To carry out the integrated study of visualization conditions of efavirenz on TLC-plates with aplication of standard and particular colored reagents, and the chromatographic behavior of efavirenz using standard mobile phases.Results and discussion. It has been shown that such widely used color reagents as UV-light, Erdmann reagent, Froehde reagent, Liebermann reagent, sulfuric acid, Marquis reagent, Mandelin reagent, acidified iodoplatinate solution, iodine vapor can be used for efavirenz detection on chromatographic plates. Efavirenz gives the positive detection results with reagents used in the TLC-screening of extracts from the biological material for substances of basic, acid and neutral nature. The chromatographic mobility of efavirenz has been studied in 17 solvents systems; the systems are used as standard mobile phases according to the recommendations of the International Association of Forensic Toxicologists for TLC-screening of organic compounds of acid, neutral and basic nature, and as well as in the general TLC-screening of organic substances in the Ukrainian forensic toxicological laboratories.Experimental part. The chromatographic plates Sorbfil® PTLC-IIH-UV and Merck® TLC Silica gel 60G were used as thin layers.Conclusions. The behavior of efavirenz when developing on TLC-plates with two types of a substrate (plastic and glass) and with/without a luminophor with commonly used colored reagents has been studied. The Rf values of efavirenz under chromatographing conditions in the standard solvent systems used for TLC-screening of organic compounds of acid, neutral and basic nature have been set. Received: 17.12.2019Revised: 12.01.2020Accepted: 27.02.2020 |
| doi_str_mv | 10.24959/ophcj.20.197511 |
| first_indexed | 2025-07-17T13:00:43Z |
| format | Article |
| fulltext |
Journal of Organic and Pharmaceutical Chemistry. – 2020. – Vol. 18, Iss. 1 (69)
58
ISSN 2308-8303 (Print) ISSN 2518-1548 (Online)
UDC 615.281.1:543.544.5 https://doi.org/10.24959/ophcj.20.197511
O. I. Slabiak1, I. M. Ivanchuk1, L. Yu. Klimenko2, O. Ye. Mykytenko2, O. V. Antonenko2
1 Ivano-Frankivsk National Medical University, Ukraine
2 National University of Pharmacy, Ukraine
53, Pushkinska str., Kharkiv, 61002, Ukraine. E-mail: lina_klimenko@nuph.edu.ua
Application of thin layer chromatography in the analysis
of efavirenz
Aim. To carry out the integrated study of visualization conditions of efavirenz on TLC-plates with aplication of standard
and particular colored reagents, and the chromatographic behavior of efavirenz using standard mobile phases.
Results and discussion. It has been shown that such widely used color reagents as UV-light, Erdmann rea-
gent, Froehde reagent, Liebermann reagent, sulfuric acid, Marquis reagent, Mandelin reagent, acidified iodoplatinate
solution, iodine vapor can be used for efavirenz detection on chromatographic plates. Efavirenz gives the positive
detection results with reagents used in the TLC-screening of extracts from the biological material for substances of
basic, acid and neutral nature. The chromatographic mobility of efavirenz has been studied in 17 solvents systems;
the systems are used as standard mobile phases according to the recommendations of the International Association
of Forensic Toxicologists for TLC-screening of organic compounds of acid, neutral and basic nature, and as well as in
the general TLC-screening of organic substances in the Ukrainian forensic toxicological laboratories.
Experimental part. The chromatographic plates Sorbfil® PTLC-IIH-UV and Merck® TLC Silica gel 60G
were used as thin layers.
Conclusions. The behavior of efavirenz when developing on TLC-plates with two types of a substrate
(plastic and glass) and with/without a luminophor with commonly used colored reagents has been studied. The Rf
values of efavirenz under chromatographing conditions in the standard solvent systems used for TLC-screening
of organic compounds of acid, neutral and basic nature have been set.
Key words: efavirenz; thin layer chromatography; color tests
О. І. Слабяк1, І. М. Іванчук1, Л. Ю. Клименко2, О. Є. Микитенко2, О. В. Антоненко2
1 Івано-Франківський національний медичний університет, Україна
2 Національний фармацевтичний університет, Україна
Застосування тонкошарової хроматографії в аналізі ефавіренцу
Мета. Провести комплексне дослідження умов візуалізації ефавіренцу на ТШХ-пластинах із застосу-
ванням стандартних і окремих кольорових реагентів, а також хроматографічної поведінки ефавіренцу з вико-
ристанням стандартних рухомих фаз.
Результати та їх обговорення. Показано, що для виявлення ефавіренцу на хроматографічних пластинах
можна використовувати такі широко відомі проявники, як УФ-світло, реактив Ердмана, реактив Фреде, реактив
Лібермана, сульфатна кислота, реактив Маркі, реактив Манделіна, підкислений розчин йодоплатинату, пари йоду.
Ефавіренц дає позитивні результати виявлення з реактивами, що використовують в ТШХ-скринінгу витягів
з біологічного матеріалу на речовини основного, кислого і нейтрального характеру. Хроматографічну рухливість
ефавіренцу досліджено в 17 системах розчинників, серед яких рухомі фази, що застосовують як стандартні згід-
но з рекомендаціями Міжнародного комітету з систематичного токсикологічного аналізу Міжнародної асоціації
судових токсикологів для ТШХ-скринінгу органічних речовин кислого, нейтрального та основного характеру, а та-
кож у загальному ТШХ-скринінгу органічних речовин у судово-токсикологічних лабораторіях України.
Експериментальна частина. Як тонкі шари використовували пластини Sorbfil ПТСХ-ІІВ-УФ та Merck
TLC Silica gel 60G.
Висновки. Досліджено поведінку ефавіренцу при проявленні загальноприйнятими хромогенними ре-
агентами на пластинах для ТШХ з двома типами підложки (пластик та скло) та з УФ-індикатором і без
нього. Встановлено значення Rf ефавіренцу за умов хроматографування в стандартних системах роз-
чинників, що використовуються для ТШХ-скринінгу речовин кислого, нейтрального та основного характеру.
Ключові слова: ефавіренц; тонкошарова хроматографія; кольорові реакції
О. И. Слабяк1, И. М. Иванчук1, Л. Ю. Клименко2, Е. Е. Микитенко2, О. В. Антоненко2
1 Ивано-Франковский национальный медицинский университет, Украина
2 Национальный фармацевтический университет, Украина
Применение тонкослойной хроматографии в анализе эфавиренца
Цель. Провести комплексное исследование условий визуализации эфавиренца на ТСХ-пластинах с при-
менением стандартных и частных цветных реагентов, а также хроматографического поведения эфави-
ренца с использованием стандартных подвижных фаз.
Результаты и их обсуждение. Показано, что для обнаружения эфавиренца на хроматографических пласти-
нах можно использовать такие широко применяемые проявители, как УФ-свет, реактив Эрдманна, реактив
Фреде, реактив Либермана, серная кислота, реактив Марки, реактив Манделина, подкисленный раствор йодопла-
тината, пары йода. Эфавиренц дает положительные результаты обнаружения с реактивами, используемыми
в ходе ТСХ-скрининга извлечений из биологического материала на вещества основного, кислого и нейтрального
характера. Хроматографическая подвижность эфавиренца исследована в 17 системах растворителей, среди
которых подвижные фазы, применяемые в качестве стандартных согласно рекомендациям Международного
комитета по систематическому токсикологическому анализу Международной ассоциации судебных токси-
кологов для ТСХ-скрининга органических веществ кислого, нейтрального и основного характера, а также
в общем ТСХ-скрининге органических веществ в судебно-токсикологических лабораториях Украины.
Журнал органічної та фармацевтичної хімії. – 2020. – Т. 18, вип. 1 (69)
59
ISSN 2518-1548 (Online) ISSN 2308-8303 (Print)
Экспериментальная часть. В качестве тонких слоев использовали пластины Sorbfil ПТСХ-ІІВ-УФ и Merck
TLC Silica gel 60G.
Выводы. Исследовано поведение эфавиренца при проявлении общепринятыми хромогенными ре-
агентами на пластинах для ТСХ с двумя типами подложки (пластик и стекло) и с УФ-индикатором и без
него. Установлены значения Rf эфавиренца в условиях хроматографирования в стандартных системах
растворителей, используемых для ТСХ-скрининга веществ кислого, нейтрального и основного характера.
Ключевые слова: эфавиренц; тонкослойная хроматография; цветные реакции
HIV infection is usually treated with drug com-
binations consisting of at least three different anti-
retroviral medicines. Essential components of this highly
active antiretroviral therapy are non-nucleoside and
nucleoside reverse transcriptase inhibitors [1, 2].
The group of non-nucleoside reverse transcriptase
inhibitors are currently presented by five medicines
(nevirapine, delavirdine, efavirenz, etravirine and ril-
pivirine) approved by the Food and Drug Administra-
tion; four of them (nevirapine, efavirenz, etravirine
and rilpivirine) have been approved by the European
Union [3 – 5].
Efavirenz is recommended currently as a prefer-
red first-line medicine with a low pill burden, once daily
dosing, a long half-life allowing for relatively stable
plasma concentrations and some forgiveness for doses
not taken exactly on the schedule [6, 7].
Efavirenz therapy accompanies with quite a num-
ber of side effects showed by psychiatric symptoms,
including insomnia, nightmares, memory loss, depres-
sion, and anxiety. Efavirenz is characterized by defi-
nite neuropsychological symptoms in 50 % of cases;
its neurotoxicity exceeds other antiretroviral medi-
cines [8 – 10]. The studies of efavirenz showed that
in 20 – 50 % of cases the toxic concentrations of the me-
dicine in the blood were fixed [11 – 12]. There are cases
of acute poisoning due to administration of efavirenz,
including cases of suicide attempts [13]. Therefore,
in our opinion, efavirenz may be approved as a po-
tential toxic compound in forensic toxicology.
The method of thin layer chromatography (TLC)
is widely used in the process of forensic toxicological
examinations for screening and confirming investi-
gations – with the purpose of analyte detection and
identification, respectively [14, 15]. The main focus
is the chromatographic behavior of the substances
using standard mobile phases (or solvents systems),
as well as the conditions of analyte spots visualiza-
tion using standard colored reagents [14, 15].
The aim of our work was the integrated study of
visualization conditions of efavirenz on TLC-plates
using standard and particular colored reagents, as well
as the chromatographic behavior of the substances
using standard mobile phases.
To fix the results of visualization of the substances
to be analyzed 4 developing modes of TLC-plates with
two types of a substrate (plastic and glass) and with/
without a luminophor (or UV-indicator) were chosen:
1) immediately after processing the substances
with a reagent and after drying the plates at the am-
bient temperature;
2) in UV-light at two wavelengths – 254 nm and
365 nm;
3) after heating the plates for 15 min at 110 °C
(the plates are covered with glass);
4) in UV-light at two wavelengths – 254 nm and
365 nm – after heating.
A number of the reagents studied (hydrogen per-
oxide solution, Nessler reagent, perchloric acid, FPN
reagent, hydrochloric acid vapor, 1 % H8[Si(W2O7)6]
solution, 1 % H7[P(Mo2O7)6] solution, 1 % H7[P(W2O7)6]
solution, 1 % H8[Si(Mo2O7)6] solution, formaldehyde/
sulfuric acid, Forrest reagent, Dragendorff reagent,
5 % ferric chloride solution, iodoplatinate solution)
do not color efavirenz either before or after heating
the plates, and also quench the initial fluorescence
both at 254 nm and at 365 nm.
The total results of efavirenz visualization on chro-
matographic plates are presented in Table 1.
Such commonly applied developers as UV-light,
Erdmann reagent, Froehde reagent, Liebermann rea-
gent, sulfuric acid, Marquis reagent, Mandelin reagent,
acidified iodoplatinate solution, iodine vapor can be
used for the detection of efavirenz on chromatogra-
phic plates.
The positive results were recorded when develo-
ping efavirenz with the reagents used in the analysis
of barbituric acid derivatives [14] – the mercuric chlo-
ride/diphenylcarbazone reagent and cobalt nitrate/
ammonia vapor; the spots of various tints of violet
color appeared, and they disappeared when heating
the plates; in UV-light the spots were not visualized.
The most of reagents used for detection and identi-
fication of substances of basic nature, including the so-
called “generally alkaloid reagents”, allows to visua-
lize efavirenz on the TLC-plates. It is colored with
the concentrated sulfuric acid, Marquis reagent and
the mixture of formaldehyde and the concentrated
sulfuric acid, Erdmann reagent, Froehde reagent,
Liebermann reagent, Mandelin reagent, acidified iodo-
platinate solution.
We also processed efavirenz according to the scheme
of TLC-screening of the substances of basic nature.
Developing the plates with acidified potassium per-
manganate solution leads to the formation of brown
spots; and after heating the plates the spots are brown.
Application of ninhydrin solution in traditional modi-
fication for TLC-screening (acidified ninhydrin spray)
results in brown spots. Overspraying the plates with
FPN reagent and Dragendorff reagent followed by aci-
dified iodoplatinate solution does not change the pre-
vious results.
Journal of Organic and Pharmaceutical Chemistry. – 2020. – Vol. 18, Iss. 1 (69)
60
ISSN 2308-8303 (Print) ISSN 2518-1548 (Online)
Table 1
The results of efavirenz visualization on chromatographic plates
No. Reagent Stationary
phase*
Spot color/sensitivity,
mg in the sample
1 UV-light (λ = 254 nm)
А violet/0.1
В –
2 UV-light (λ = 365 nm) А, В –
3 formaldehyde vapor (for 5 min in the covered cell)
A violet (λ = 254 nm)/0.5
yellow (λ = 365 nm)/0.5
B –
4 phosphoric acid [14, p. 2464] pour on
A light blue (λ = 365 nm)/0.5
B –
5 Erdmann reagent [14, p. 485] pour on
A bright yellow/0.1
B –
6 Froehde reagent [14, p. 478] pour on
A pink-brown/0.1
B –
7 Liebermann reagent [14, p. 480] pour on A, B bright yellow/0.1
8 glacial acetic acid [14, p. 2463] pour on A, B yellow/0.5
9 mercuric chloride – diphenylcarbazone reagent
[14, p. 2463] spray A, B violet/0.5
10 cobalt nitrate spray, dry
+ ammonia vapor for 5 min in the covered cell A, B light violet/0.5
11 sulfuric acid [14, p. 488] pour on A, B light yellow (15 min at 110 °C)/0.5
12 Marquis reagent [14, p. 480] pour on A light yellow/0.5
light yellow (15 min at 110 °C) / 0.5
13 Iodine vapor for 5 min in the covered cell A, B brown/0.1
14 Mandelin reagent [14, p. 480] pour on
A light brown/0.1
light brown (15 min at 110 °C)/0.1
B pink brown/0.1
pink brown (15 min at 110 °C) / 0.1
15 formaldehyde vapor for 5 min in the covered cell
+ Mandelin reagent pour on [14, p. 612]
A light brown/0.1
light brown (15 min at 110 °C)/0.1
B pink brown/0.1
pink brown (15 min at 110 °C)/0.1
16 acidified potassium permanganate solution
[14, p. 478] spray A, B brown/0.1
17 acidified ninhydrin spray [14, p. 2464] spray A, B light brown (15 min at 110 °C)/0.5
18 + FPN reagent [14, p. 478] overspray A, B light brown/0.1
light brown (15 min at 110 °C)/0.1
19 + Dragendorff reagent [14, p. 476] overspray A, B light brown/0.1
light brown (15 min at 110 °C)/0.1
20 + acidified iodoplatinate solution [14, p. 2463] overspray A, B light brown/0.1
light brown (15 min at 110 °C)/0.1
21
Van Urk reagent (acidified
p-dimethylaminobenzaldehyde solution in ethanol)
[14, p. 476] spray
A bright yellow (15 min at 110 °C)/0.1
B yellow (15 min at 110 °C)/0.1
22 + 5 % ferric chloride solution [14, p. 478] overspray
A bright yellow (15 min at 110 °C)/0.1
B yellow (15 min at 110 °C)/0.1
23 acidified iodoplatinate solution [14, p. 2463] spray A, B dark brown (15 min at 110 °C)/0.1
Notes: * – А – Sorbfil® PTLC-IIH-UV; В – Merck® TLC Silica gel 60G
Журнал органічної та фармацевтичної хімії. – 2020. – Т. 18, вип. 1 (69)
61
ISSN 2518-1548 (Online) ISSN 2308-8303 (Print)
Processing the plates directly with iodoplatinate
solution does not lead to visible results. Acidified iodo-
platinate solution after heating causes the formation
of dark brown spots.
Developing efavirenz according to the scheme of
TLC-screening of the substances of acid and neutral
nature leads to the positive results (yellow spots after
heating) with Van Urk reagent. Overspraying the plates
with 5 % ferric chloride solution does not change the pre-
vious results.
The chromatographic mobility of efavirenz was
studied in 17 solvents systems (Table 2); the systems
1 – 9 were used as standard mobile phases according
to the recommendations of the International Asso-
ciation of Forensic Toxicologists (TIAFT) for TLC-scre-
ening of organic compounds of acid, neutral and basic
nature [14]; systems 10 – 12 were used in the general
TLC-screening of organic substances in the Ukrainian
forensic toxicological laboratories; systems 13 – 17 were
studied with the purpose of choosing the optimal in-
dividual solvents systems for research of efavirenz.
When using the mobile phases 3A, 7A, 8A, 9A
the studies were carried out on the plates processed
previously with 0.1 mole/L KOH solution in methanol
and then dried at 110°С for 30 min. For the mobile
phase 6 application the plates were previously pro-
cessed with 0.1 mole/L NaBr solution.
The results are presented in Table 2.
Experimental part
Efavirenz was of pharmacopoeial purity. Chloro-
form (≥99 %, anhydrous, contains 0.5 – 1.0 % of etha-
nol as a stabilizer), ethyl acetate (99.8 %, anhydrous),
methanol (≥99.8 %, puriss. p.a., ACS reagent), ammo-
nium hydroxide solution (≥25 % NH3 in H2O, puriss.
p.a. plus) were purchased from Sigma-Aldrich Co. LLC
(USA). All other reagents were of analytical grade.
The reference solution 1 (1000 μg/mL) was pre-
pared by dissolving 50.0 mg of efavirenz in methanol;
the solution was diluted to 50.0 mL with the same
solvent. The reference solution 2 (100 μg/mL) was
prepared by diluting 5.00 mL of the reference solu-
tions 1 to 50.0 mL with methanol.
The color reagents were prepared according to [14].
The chromatographic plates Sorbfil® PTLC-IIH-UV
(silica gel STC-1HP, PETP, luminophor, silica sol, the frac-
tion of 8÷12 μm, the layer thickness of 100 μm) were
purchased from IMID LLC (Russia). The chromatogra-
phic plates Merck® TLC SILICA GEL 60 (silica gel 60,
glass, gypsum, the fraction of 9.5÷11.5 μm, the layer
thickness of 140÷160 μm) were purchased from Merck
Group (Germany).
The part of plates was previously processed with
0.1 mole/L potassium hydroxide solution in metha-
nol and then dried at 110°С for 30 min. The part of
plates was previously processed with 0.1 mole/L so-
dium bromide solution [14].
To choose the developing color reagents in 10 mL
of the reference solution 1 were applied on the pla-
tes of both types, and then the reagents were sprayed
or poured onto the plates. The results were fixed vi-
sually at once and after drying the plate, then the pla-
tes were developed in UV-light with the wavelength
of 254 nm and 365 nm. At the next stage the plates
were heated for 15 min at 110 °C (the plates were co-
vered with a glass plate), and after that colors of spots
were fixed in visible and UV-light one more time.
To determine sensitivity of the developing color rea-
gents the same experiments were carried out using 1
and 10 mL of the reference solutions 2 of the substances.
Table 2
The Rf values for efavirenz
Mobile phase
Rf of efavirenz
(n = 3)
Sorbfil®
PTLC-PH-
UV
Merck®
TLC
Silica
gel 60G
1 chloroform – acetone (8:2) 0.65 0.67
2 ethyl acetate 0.85 0.89
3 chloroform – methanol (9:1) 0.76 0.71
3А* chloroform – methanol (9:1) 0.70 0.72
4 ethyl acetate – methanol –
25 % NH3 (85:10:5) 0.18 0.11
5 methanol 0.87 0.82
6 methanol – n-butanol (6:4)** 0.90 0.87
7 methanol – 25 % NH3 (100:1,5) 0.84 0.89
7А* methanol – 25 % NH3 (100:1,5) 0.76 0.74
8 cyclohexane – toluene –
diethylamine (75:15:10) 0.05 0.07
8А* cyclohexane – toluene –
diethylamine (75:15:10) 0.00 0.00
9 acetone 0.84 0.85
9А* acetone 0.90 0.92
10
chloroform – dioxane –
acetone – 25 % NH3
(47,5:45:5:2,5)
0.35 0.39
11 toluene – acetone – ethanol –
25 % NH3 (45:45:7,5:2,5) 0.82 0.85
12 chloroform – n-butanol –
25 % NH3 (70:40:5) 0.90 0.93
13 chloroform 0.00 0.00
14 chloroform – methanol (1:1) 0.85 0.89
15 toluene – CH3COOH
conc. (3:1) 0.10 0.15
16 chloroform – methanol –
CH3COOH conc. (90:10:1) 0.25 0.29
17 toluene – methanol –
CH3COOH conc. (9:1:1) 0.85 0.83
Notes: * – 0.1 M KOH in CH3OH, 110°С, 30 min; ** – 0.1 M NaBr
Journal of Organic and Pharmaceutical Chemistry. – 2020. – Vol. 18, Iss. 1 (69)
62
ISSN 2308-8303 (Print) ISSN 2518-1548 (Online)
Chromatographing was carried out in cells with
the volume of 500 mL; 50 mL of the corresponding
TLC-systems were placed into them. The cell was
saturated for 30 min. In 10 mL of the reference so-
lutions 1 of the substance to be researched were
applied on the start line in the distance of 1 cm from
the plate edge. The solvent path length was 8 cm.
After reaching the finish line by the mobile phase
the plate was taken out from the cell, dried at the am-
bient temperature and developed with the correspon-
ding reagents.
Conclusions
The behavior of efavirenz when developing with
commonly used colored reagents on TLC plates with
two types of a substrate (plastic and glass) and with/
without a luminophor (or UV-indicator) has been stu-
died. The results of efavirenz development with rea-
gents used for TLC-screening of organic compounds of
acid, neutral and basic nature are presented. The Rf va-
lues for efavirenz have been determined using diffe-
rent types of TLC-plates for solvent systems used as
standard mobile phases according to the recommen-
dations of the International Association of Forensic
Toxicologists for TLC-screening of organic compounds
of acid, neutral and basic nature, and also in the ge
neral TLC-screening of organic substances in the
Ukrainian forensic toxicological laboratories.
Conflict of interests: authors have no conflict of
interests to declare.
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Received: 17. 12. 2019
Revised: 12. 01. 2020
Accepted: 27. 02. 2020
The research was carried out according to the budget themes of the Ministry of Public Health of Ukraine “Study of organizational,
marketing, pharmacoeconomic, technological, pharmacological and qualitative aspects of medicines of natural and synthetic origin”
(the state registration No. 0113U004136; research period 2013 – 2020) and “Chemical and toxicological analysis of biologically active
substances and medicines” (the state registration No. 011411000958; the research period 2014 – 2020).
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| id | oai:ojs.journals.uran.ua:article-197511 |
| institution | Journal of Organic and Pharmaceutical Chemistry |
| issn | 2518-1548 |
| keywords_txt_mv | |
| language | English |
| last_indexed | 2026-08-25T01:01:44Z |
| publishDate | 2020 |
| publisher | National University of Pharmacy |
| record_format | ojs |
| resource_txt_mv | ophcjnupheduua/da/af96e3a073bce64a648c7e30339bb2da.pdf |
| spelling | oai:ojs.journals.uran.ua:article-1975112026-08-24T18:04:29Z Application of thin layer chromatography in the analysis of efavirenz Применение тонкослойной хроматографии в анализе эфавиренца Застосування тонкошарової хроматографії в аналізі ефавіренцу Slabiak, Oksana I. Ivanchuk, Iryna M. Klimenko, Lina Yu. Mykytenko, Olena Ye. Antonenko, Olga V. эфавиренц тонкослойная хроматография цветные реакции УДК 615.281.1 543.544.5 ефавіренц тонкошарова хроматографія кольорові реакції УДК 615.281.1 543.544.5 efavirenz thin layer chromatography color tests UDC 615.281.1 543.544.5 Aim. To carry out the integrated study of visualization conditions of efavirenz on TLC-plates with aplication of standard and particular colored reagents, and the chromatographic behavior of efavirenz using standard mobile phases.Results and discussion. It has been shown that such widely used color reagents as UV-light, Erdmann reagent, Froehde reagent, Liebermann reagent, sulfuric acid, Marquis reagent, Mandelin reagent, acidified iodoplatinate solution, iodine vapor can be used for efavirenz detection on chromatographic plates. Efavirenz gives the positive detection results with reagents used in the TLC-screening of extracts from the biological material for substances of basic, acid and neutral nature. The chromatographic mobility of efavirenz has been studied in 17 solvents systems; the systems are used as standard mobile phases according to the recommendations of the International Association of Forensic Toxicologists for TLC-screening of organic compounds of acid, neutral and basic nature, and as well as in the general TLC-screening of organic substances in the Ukrainian forensic toxicological laboratories.Experimental part. The chromatographic plates Sorbfil® PTLC-IIH-UV and Merck® TLC Silica gel 60G were used as thin layers.Conclusions. The behavior of efavirenz when developing on TLC-plates with two types of a substrate (plastic and glass) and with/without a luminophor with commonly used colored reagents has been studied. The Rf values of efavirenz under chromatographing conditions in the standard solvent systems used for TLC-screening of organic compounds of acid, neutral and basic nature have been set. Received: 17.12.2019Revised: 12.01.2020Accepted: 27.02.2020 Цель. Провести комплексное исследование условий визуализации эфавиренца на ТСХ-пластинах с применением стандартных и частных цветных реагентов, а также хроматографического поведения эфавиренца с использованием стандартных подвижных фаз.Результаты и их обсуждение. Показано, что для обнаружения эфавиренца на хроматографических пластинах можно использовать такие широко применяемые проявители, как УФ-свет, реактив Эрдманна, реактив Фреде, реактив Либермана, серная кислота, реактив Марки, реактив Манделина, подкисленный раствор йодоплатината, пары йода. Эфавиренц дает положительные результаты обнаружения с реактивами, используемыми в ходе ТСХ-скрининга извлечений из биологического материала на вещества основного, кислого и нейтрального характера. Хроматографическая подвижность эфавиренца исследована в 17 системах растворителей, среди которых подвижные фазы, применяемые в качестве стандартных согласно рекомендациям Международного комитета по систематическому токсикологическому анализу Международной ассоциации судебных токсикологов для ТСХ-скрининга органических веществ кислого, нейтрального и основного характера, а также в общем ТСХ-скрининге органических веществ в судебно-токсикологических лабораториях Украины.Экспериментальная часть. В качестве тонких слоев использовали пластины Sorbfil ПТСХ-ІІВ-УФ и Merck TLC Silica gel 60G.Выводы. Исследовано поведение эфавиренца при проявлении общепринятыми хромогенными реагентами на пластинах для ТСХ с двумя типами подложки (пластик и стекло) и с УФ-индикатором и без него. Установлены значения Rf эфавиренца в условиях хроматографирования в стандартных системах растворителей, используемых для ТСХ-скрининга веществ кислого, нейтрального и основного характера. Received: 17.12.2019Revised: 12.01.2020Accepted: 27.02.2020 Мета. Провести комплексне дослідження умов візуалізації ефавіренцу на ТШХ-пластинах із застосуванням стандартних і окремих кольорових реагентів, а також хроматографічної поведінки ефавіренцу з використанням стандартних рухомих фаз.Результати та їх обговорення. Показано, що для виявлення ефавіренцу на хроматографічних пластинах можна використовувати такі широко відомі проявники, як УФ-світло, реактив Ердмана, реактив Фреде, реактив Лібермана, сульфатна кислота, реактив Маркі, реактив Манделіна, підкислений розчин йодоплатинату, пари йоду. Ефавіренц дає позитивні результати виявлення з реактивами, що використовують в ТШХ-скринінгу витягів з біологічного матеріалу на речовини основного, кислого і нейтрального характеру. Хроматографічну рухливість ефавіренцу досліджено в 17 системах розчинників, серед яких рухомі фази, що застосовують як стандартні згідно з рекомендаціями Міжнародного комітету з систематичного токсикологічного аналізу Міжнародної асоціації судових токсикологів для ТШХ-скринінгу органічних речовин кислого, нейтрального та основного характеру, а також у загальному ТШХ-скринінгу органічних речовин у судово-токсикологічних лабораторіях України.Експериментальна частина. Як тонкі шари використовували пластини Sorbfil ПТСХ-ІІВ-УФ та Merck TLC Silica gel 60G.Висновки. Досліджено поведінку ефавіренцу при проявленні загальноприйнятими хромогенними реагентами на пластинах для ТШХ з двома типами підложки (пластик та скло) та з УФ-індикатором і без нього. Встановлено значення Rf ефавіренцу за умов хроматографування в стандартних системах розчинників, що використовуються для ТШХ-скринінгу речовин кислого, нейтрального та основного характеру. Received: 17.12.2019Revised: 12.01.2020Accepted: 27.02.2020 National University of Pharmacy 2020-03-05 Article Article application/pdf https://ophcj.nuph.edu.ua/article/view/ophcj.20.197511 10.24959/ophcj.20.197511 Journal of Organic and Pharmaceutical Chemistry; Vol. 18 No. 1(69) (2020); 58-62 Журнал органической и фармацевтической химии; Том 18 № 1(69) (2020); 58-62 Журнал органічної та фармацевтичної хімії; Том 18 № 1(69) (2020); 58-62 2518-1548 2308-8303 en https://ophcj.nuph.edu.ua/article/view/ophcj.20.197511/198323 Copyright (c) 2020 Oksana I. Slabiak, Iryna M. Ivanchuk, Lina Yu. Klimenko, Olena Ye. Mykytenko, Olga V. Antonenko https://creativecommons.org/licenses/by/4.0 |
| spellingShingle | ефавіренц тонкошарова хроматографія кольорові реакції УДК 615.281.1 543.544.5 Slabiak, Oksana I. Ivanchuk, Iryna M. Klimenko, Lina Yu. Mykytenko, Olena Ye. Antonenko, Olga V. Застосування тонкошарової хроматографії в аналізі ефавіренцу |
| title | Застосування тонкошарової хроматографії в аналізі ефавіренцу |
| title_alt | Application of thin layer chromatography in the analysis of efavirenz Применение тонкослойной хроматографии в анализе эфавиренца |
| title_full | Застосування тонкошарової хроматографії в аналізі ефавіренцу |
| title_fullStr | Застосування тонкошарової хроматографії в аналізі ефавіренцу |
| title_full_unstemmed | Застосування тонкошарової хроматографії в аналізі ефавіренцу |
| title_short | Застосування тонкошарової хроматографії в аналізі ефавіренцу |
| title_sort | застосування тонкошарової хроматографії в аналізі ефавіренцу |
| topic | ефавіренц тонкошарова хроматографія кольорові реакції УДК 615.281.1 543.544.5 |
| topic_facet | эфавиренц тонкослойная хроматография цветные реакции УДК 615.281.1 543.544.5 ефавіренц тонкошарова хроматографія кольорові реакції УДК 615.281.1 543.544.5 efavirenz thin layer chromatography color tests UDC 615.281.1 543.544.5 |
| url | https://ophcj.nuph.edu.ua/article/view/ophcj.20.197511 |
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