Кількісне визначення оксациліну методами кінетико-спектрофотометрії та окисно-відновного титрування
The search for new analytical reactions and finding out the optimal conditions for their course, which can be used as the basis for quantitative analytical determinations of penicillins, is a very urgent task.Aim. To develop methods for the quantitative determination of Oxacillin.Materials and metho...
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| Datum: | 2023 |
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Journal of Organic and Pharmaceutical Chemistry| _version_ | 1874364445512171520 |
|---|---|
| author | Karpova, Svetlana P. Ivashura, Maryna M. Koval, Alla O. Kolisnyk, Yulia S. |
| author_facet | Karpova, Svetlana P. Ivashura, Maryna M. Koval, Alla O. Kolisnyk, Yulia S. |
| author_institution_txt_mv | [
{
"author": "Svetlana P. Karpova",
"institution": "National University of Pharmacy of the Ministry of Health of Ukraine",
"orcid": ""
},
{
"author": "Maryna M. Ivashura",
"institution": "National University of Pharmacy of the Ministry of Health of Ukraine",
"orcid": ""
},
{
"author": "Alla O. Koval",
"institution": "National University of Pharmacy of the Ministry of Health of Ukraine",
"orcid": ""
},
{
"author": "Yulia S. Kolisnyk",
"institution": "National University of Pharmacy of the Ministry of Health of Ukraine",
"orcid": ""
}
] |
| author_sort | Karpova, Svetlana P. |
| baseUrl_str | https://ophcj.nuph.edu.ua/oai |
| collection | OJS |
| container_end_page | 20 |
| container_issue | 2 |
| container_start_page | 15 |
| container_title | Журнал органічної та фармацевтичної хімії |
| container_volume | 21 |
| datestamp_date | 2026-08-23T19:38:20Z |
| description | The search for new analytical reactions and finding out the optimal conditions for their course, which can be used as the basis for quantitative analytical determinations of penicillins, is a very urgent task.Aim. To develop methods for the quantitative determination of Oxacillin.Materials and methods. The study object was Oxacillin sodium salt powder in vials for preparing a solution for injections(0.5 g). Peroxomonosulfate acid as triple potassium salt 2КНSO5∙КНSO4∙K2SO4 (Oxone®) of “extra pure” grade was used as an oxidant. The methods of kinetic spectriphotometry and redox titration were used.Results and discussion. A simple procedure for the quantitative determination of the Oxacillin pure substance by the kinetic spectrophotometry and redox titration methods using potassium hydrogen peroxomonosulfate (KHSO5) has been developed. The results of the drug analysis obtained by newly developed and current methods are in good agreement with each other; δ (correctness) = (0.45 – 0.86) %.Conclusions. Using the methods of kinetic spectrophotometric and redox titration, two independent procedures for thequantitative determination of oxacillin in the substance and the drug product have been developed using potassium hydrogen peroxomonosulfate as an analytical reagent (KHSO5). A relative standard deviation RSD = (1.24 – 2.17) %. |
| doi_str_mv | 10.24959/ophcj.23.273654 |
| first_indexed | 2025-07-23T04:43:13Z |
| format | Article |
| fulltext |
ISSN 2308-8303 (Print) / 2518-1548 (Online) 15
Original Research
http://ophcj.nuph.edu.ua
UDC 547.732:543.242.3:543.42.062:543.257
S. P. Karpova, M. M. Ivashura, A. O. Koval, Yu. S. Kolisnyk
National University of Pharmacy of the Ministry of Health of Ukraine,
53, Pushkinska str., Kharkiv, 61002, Ukraine
The Quantitative Determination of Oxacillin Using
Kinetiс-Spectrophotometric and Redox Titration Methods
Abstract
The search for new analytical reactions and finding out the optimal conditions for their course, which can be used as the
basis for quantitative analytical determinations of penicillins, is a very urgent task.
Aim. To develop methods for the quantitative determination of Oxacillin.
Materials and methods. The study object was Oxacillin sodium salt powder in vials for preparing a solution for injections
(0.5 g). Peroxomonosulfate acid as triple potassium salt 2КНSO5∙КНSO4∙K2SO4 (Oxone®) of “extra pure” grade was used as an
oxidant. The methods of kinetic spectriphotometry and redox titration were used.
Results and discussion. A simple procedure for the quantitative determination of the Oxacillin pure substance by the kinetic
spectrophotometry and redox titration methods using potassium hydrogen peroxomonosulfate (KHSO5) has been developed.
The results of the drug analysis obtained by newly developed and current methods are in good agreement with each other;
δ (correctness) = (0.45 – 0.86) %.
Conclusions. Using the methods of kinetic spectrophotometric and redox titration, two independent procedures for the
quantitative determination of oxacillin in the substance and the drug product have been developed using potassium hydro-
gen peroxomonosulfate as an analytical reagent (KHSO5). A relative standard deviation RSD = (1.24 – 2.17) %.
Keywords: oxacillin; potassium hydrogen peroxomonosulfate; iodometry; kinetic spectrophotometry
С. П. Карпова, М. М. Івашура, А. О. Коваль, Ю. С. Колісник
Національний фармацевтичний університет Міністерства охорони здоров’я України,
вул. Пушкінська, 53, м. Харків, 61002, Україна
Кількісне визначення оксациліну методами кінетико-спектрофотометрії та окисно-відновного
титрування
Анотація
Мета. Пошук нових аналітичних реакцій та з’ясування оптимальних умов їх перебігу, які можуть бути покладені в основу
кількісних аналітичних визначень пеніцилінів, є вельми актуальним завданням. Метою цієї роботи було розробити
методики кількісного визначення оксациліну.
Матеріали та методи. Обʼєктом дослідження був Оксацилін – порошок натрій оксациліну у флаконах для приготуван-
ня розчину для ін’єкцій (0,5 г). Як окисник використовували потрійну калієву сіль 2КНSO5∙КНSO4∙K2SO4 кваліфікації “ex-
tra pure” (Oxone®). У дослідженні було задіяно методи кінетико-спектрофотометрії та окисно-відновного титрування.
Результати та їх обговорення. Розроблено процедуру кількісного визначення оксациліну методами кінетико-спектро-
фотометрії та йодометричного титрування з використанням калій гідрогенпероксомоносульфату. Результати аналізу
препарату, одержані за новоопрацьованими та чинними методиками, добре узгоджуються між собою; δ (правиль-
ність) = (0.45 – 0.86) %.
Висновки. За допомогою методів кінетико-спектрофотометрії та йодометричного титрування розроблено дві неза-
лежні методики кількісного визначення оксациліну в субстанції та лікарському препараті з використанням калій гід-
рогенпероксомоносульфату як аналітичного реагенту (KHSO5). Відносне стандартне відхилення RSD (1,24 – 2,17) %.
Ключові слова: оксацилін; калій гідрогенпероксомоносульфат; йодометрія; кінетико-спектрофотометрія
ISSN 2308-8303 (Print) / 2518-1548 (Online) 16
Журнал органічної та фармацевтичної хімії 2023, 21 (2)
Citation: Karpova, S. P.; Ivashura, M. M.; Koval, A. O.; Kolisnyk, Yu. S. The Quantitative Determination of Oxacillin Using Kinetiс-
Spectrophotometric and Redox Titration Methods. Journal of Organic and Pharmaceutical Chemistry 2023, 21 (2), 15 – 20.
https://doi.org/10.24959/ophcj.23.273654
Received: 28 September 2022; Revised: 10 November 2022; Accepted: 29 November 2022
Copyright© 2023, S. P. Karpova, M. M. Ivashura, A. O. Koval, Yu. S. Kolisnyk. This is an open access article under the CC BY license
(http://creativecommons.org/licenses/by/4.0).
Funding: The work is a part of the research of the National University of Pharmacy on the topic “Organic synthesis and analysis
of biologically active compounds, drug development based on synthetic substances” (the state registration No. 01144000943;
the research period of 2019 – 2024).
Conflict of interests: The authors have no conflict of interests to declare.
■ Introduction
Despite the emergence of new groups of anti-
microbial agents, antibiotic drugs of the penicil-
lin series continue to occupy a significant place
in pharmacy. In particular, hydrolysis-resistant
ampicillin preparations have become widespread.
To determine the activity of penicillin prepa-
rations, as well as other antibiotics, biological,
chemical, and physicochemical methods are used.
The basic method for the quantitative deter-
mination of the content of penicillins is the clas-
sical method of iodometry of hydrolysis products.
Its disadvantage is the duration of at least 40 min,
the need to use standard samples and standar-
dization of the determination conditions, as well
as its dependence on temperature [1 – 3].
According to the literature data, various me-
thods are used for the quantitative determinations
of antibiotics: chromatographic methods [4 – 7],
chemiluminescent, spectrophotometric [8 – 11], fluo-
rimetric [12], kinetic [13], voltammetric, methods
using ion-selective electrodes, capillary electro-
phoresis, extraction method [14, 15].
Spectrophotometric methods are also known.
They are based on the interaction of penicillins
with copper (II) salts. These procedures allow de-
termining penicillins in drugs in the presence of
various additional substances.
Despite the fact that many methods are used
in the practice of analysis, the task of improv-
ing the known and developing new methods for
the quantitative determination of penicillins re-
mains relevant. The well-known pharmacopoe-
ial methods for determining drugs of this series
are quite difficult, require a lot of time for prep-
aration, and the use of complex equipment [16].
We have developed methods for the quantita-
tive determination of antibiotic oxacillin by two
alternative procedures of iodometry and kinetic
spectrophotometry using potassium hydrogen
peroxomonosulfate (KHSO5) as an analytical
reagent.
■ Materials and methods
Substances and solutions
For the research, oxacillin sodium salt of phar-
macopoeial purity (3-phenyl-5-methyl-4-isoxazo-
lylpenicillin sodium salt monohydrate), a dry ste-
rile powder in vials (0.5 g) “OXACILIN-KMP” pro-
duced by AT “Kyivmedpreparat”, Kyiv, Ukraine
was used. Potassium hydrogen peroxomonosul-
fate was obtained from commercial sources and
used as an oxidant in the form of a triple potassium
salt (2КНSO5∙КНSO4∙K2SO4, “Oxone”) of “extra
pure” grade with an active oxygen content of 4.5 %.
The choice of the reagent was due to its availabil-
ity, fairly good solubility and stability in aqueous
solutions, and a relatively high oxidizing ability.
Working solution of potassium hydrogen per-
oxomonosulfate 2×10–2 mol L–1.
A weighed portion of 0.6148 g of the salt was
dissolved in 100.0 mL of double-distilled water
at 20 °C. The solution concentration was con-
trolled by iodometric titration.
As a standard sample of oxacillin sodium salt,
we used the substance of Oхаcillin of pharmaco-
poeial purity with the content of the main sub-
stance of 99.1 %.
Standard sample solution of Oxacillin (Oxa),
500 mg mL-1. A weighed portion of 0.05 g of Work-
ing solution of Oxа was dissolved in 100.00 mL
of distilled water at 20 °C.
Working solutions of Oxa. Seven aqueous so-
lutions of the following concentrations: 80 %; 85 %;
90 %; 95 %; 100 %; 110 %; 120 % were prepared
in 100 mL volumetric flasks; the corresponding
portions of 0.2289 g; 0.2433 g; 0.2576 g; 0.2718 g;
0.2862 g; 0.3147 g; 0.3433 g of the Oxa substance
were weighed.
Sodium thiosulfate solution, 2×10–2 mol L–1.
An ampoule of a standard titer of sodium thio-
sulfate with an exact concentration of 0.1 mol L–1
was diluted five times with distilled water.
Solution of potassium iodide, 5 %. A weighed
portion of 5.0 g of potassium iodide was dissolved
ISSN 2308-8303 (Print) / 2518-1548 (Online) 17
Journal of Organic and Pharmaceutical Chemistry 2023, 21 (2)
in 50 mL of distilled water, and the solution was
diluted to the volume in a 100 mL volumetric flask
at 20 °C.
Sodium hydroxide solution, 6.1×10–3 mol L-1.
The sodium hydroxide solution was prepared ac-
cording to Hillebrant by diluting the saturated
solution with freshly distilled water.
Sulfuric acid, 0.1 mol L–1. An ampoule of a
standard titer of sulfuric acid with an exact con-
centration of 0.1 mol L–1 was diluted with dis-
tilled water.
Equipment
Spectrophotometry. The spectra of solutions
of Oxa and its oxidation products were recorded,
and the light absorption of solutions in a quartz
cuvette per 1 cm was measured on an Evolu-
tion 60S UV-Visible Spectrophotometer Thermo-
Scientific (USA) against the solution without Oxa
or double-distilled water (compensation solution).
Titration. The titer of the Oxa solution stud-
ied was determined using a 10 mL microburette
with an accuracy of ±0.01 mL filled with a titrant
to the zero mark.
Procedures
Kinetic Spectrophotometric Method. 65 mg (accu-
rate weight) of the powder of the Oxa sodium salt
studied was transferred into a 100 mL volumet-
ric flask, dissolved in 50 mL of distilled water,
the solution was diluted to the volume, and the
content was mixed. 5.00 mL of the solution ob-
tained was transferred into a 50 mL volumetric
flask, 3.0 mL of a 0.02 mol L–1 KHSO5 solution
and 3.0 mL of NaOH with the concentration of
6.1×10–3 mol L–1 were added. The resulting solu-
tion was exposed to photometric measurements
for 10 min in a 1 cm quartz cuvette at 282 nm
using distilled water as a compensation solu-
tion.
Reduction-oxidation (redox) titration method.
450 mg (accurate weight) of the powder of the
Oxa sodium salt studied was dissolved in 75 mL
of water in a 100 mL volumetric flask at 20 °C,
and diluted to the volume. Using a pipette, 10 mL
of the resulting Oxa solution was taken and trans-
ferred to a 100 mL volumetric flask, 10.0 mL of
a 0.02 mol L–1 KHSO5 solution was added with
stirring, and diluted to the volume with distilled
water at 20 °C. Using a pipette, 10 mL of the
reaction mixture was taken and transferred to a
100 mL flask, acidified with 1 mL of a 0.1 mol L–1
H2SO4 solution, and 2 mL of a 5 % potassium io-
dide solution was added with vigorous stirring.
The displaced iodine was immediately titrated
with a standard 0.02 mol L–1 sodium thiosulfate
solution. In parallel, under the same conditions,
a control experiment is carried out (without the
Oxa solution studied).
■ Results and discussion
Kinetic Spectrophotometric Method
As a result of the study, it was found that the
order of mixing the solutions significantly affected
the kinetics and the yield of the reaction pro-
duct: the highest rate of the product formation
was after the preliminary mixing of the Oxa so-
lution with KHSO5 (the stage of the Oxa sulfox-
ide formation).
Figure 1 shows the electronic light absorption
spectra of the reaction product of the alkaline hy-
drolysis and perhydrolysis of Oxa during the reac-
tion in the A (optical density) – λ (wavelength, nm)
Figure 1. Electronic light absorption spectra of the reaction product of alkaline hydrolysis and Oxa perhydrolysis
of the sodium salt over time. c(NaOH) = 6.1×10–3 mol L–1; c(КНSO5) = 1.2×10–3 mol L–1; c(Oxa) = 30 mg mL– 1
ISSN 2308-8303 (Print) / 2518-1548 (Online) 18
Журнал органічної та фармацевтичної хімії 2023, 21 (2)
coordinates. The maximum absorption of the pro-
duct formed was observed at 282 nm. Therefore,
at the given wavelength, the kinetics of the ana-
lytical reaction was studied.
The optimal concentrations of alkali and KHSO5
were 6.1·10–3 mol L–1 and 0.02 mol L–1, respecti-
vely, at which the reaction rate of the perhydroly-
sis product formation was the highest.
Without KHSO5 under the above conditions,
no reaction product was formed for 30 min.
The necessary excess of KHSO5 can be explained
by the influence of further hydrolytic decomposi-
tion of S-oxide Oxa in the alkaline medium (nuc-
leophilic catalysis of the hydrolysis of the β-lactam
and thiazolidine cycles). Due to the alpha effect,
KHSO5 is a stronger nucleophile than hydroxide
ion by many times (Figure 2). PMS-induced oxi-
dation of β-lactam antibiotics was proposed to
proceed through a non-radical mechanism in-
volving direct two-electron transfer along with
the heterolytic cleavage of the PMS peroxide
bond. The product analysis indicated oxidation
of β-lactam antibiotics to two stereoisomeric sul-
foxides [17].
Plotting a calibration graph. Using a micro-
burette, 0.50; 2.50; 3.00; 4.00; 5.00; 7.50 mL sam-
ples of the standard Oxa solution were added
to 50 mL volumetric flasks followed by 5 mL of
2·10–2 mol L–1 KHSO5 solution put to each flask,
and the content was shaken thoroughly. 5.0 mL
of 6.1×10–3 mol L–1 NaOH solution were sequen-
tially poured into each flask; the solution was
diluted to the volume with distilled water and
thoroughly mixed. After adding alkali to the so-
lution, the stopwatch was started. The resulting
solutions were photometered in a quartz cuvette
with a thickness of 1 cm at 282 nm against dis-
tilled water (compensation solution) for 10 minu-
tes every minute at 20 °C, and kinetic curves of
the dependence of the optical density on time were
plotted. According to the slope of the linear sec-
tions of the kinetic curves, a calibration depend-
ence of tgα on the concentration of Oxa (C, μg mL–1)
was constructed.
Figure 3 shows a calibration graph for deter-
mining Oxa, according to which, the dependence
of concentration on tgα is linear in the range of
5 to 50 μg mL–1. This makes it possible to deter-
mine the quantitative content of Oxa in the giv-
en concentration range by the standard method.
The content of С19Н19N3O4S, in mg in one vial,
(ХOxa) was calculated by the formula:
X =
a tg w ast· · 0.9094·α·
Oxa a tg· αst
where: аst – is the mass of a standard sample of
oxacillin sodium salt, mg;
tgαst – is the tangent of the angle of the slope of
the kinetic curve in the study with the standard
solution of oxacillin sodium salt, min–1;
w – is the content of С19Н19N3O4S oxacillin sodi-
um salt in the standard sample of Oxa, in mass
fractions;
S
N
H
N
R
O
Me
Me
CO2H
HSO5
S
N
H
N
R
O
Me
Me
CO2H
O
R =
HN
S
NH
R
Me
Me
CO2H
O
O
O
O
N
SO2
NH
R
Me
Me
CO2
O
O
NH
R
O
O
O
H
H3N
SO2
Me
Me
CO2
+
O
N
�max = 282 nm
H
HSO5
HO
HSO5
HO
Ph
Me
O
HO
HN
SO2
NH
R
Me
Me
CO2
O
O
Figure 2. The scheme of coupled reactions of peroxyacid oxidation and perhydrolysis of sulfon Oxa with the formation of a substituted
derivative of N-acryl-β-penicylamine sulfate
ISSN 2308-8303 (Print) / 2518-1548 (Online) 19
Journal of Organic and Pharmaceutical Chemistry 2023, 21 (2)
а – is the weighed portion of the powder of oxa-
cillin sodium salt studied, mg;
a – is the average weight of the drug in the vial, mg;
tgα – is the tangent of the angle of the slope of
the kinetic curve in the study with the test solu-
tion of oxacillin sodium salt, min–1;
0.9094 – is the calculation coefficient of oxacillin
sodium salt to oxacillin.
The results of the analysis of the Oxa drug by
kinetic spectrophotometric method are shown in
Тable 1. The relative standard deviation did not
exceed 1.7 % (δ = –1.35 %).
Redox titration method
By the method of reverse iodometric titra-
tion of the KHSO5 excess, it was found that in
the reaction studied 1 mol of KHSO5 was con-
sumed by 1 mol of Oxa, and the interaction be-
tween them occurred for 1 min. The analytical
reaction underlying the method is shown in Fi-
gure 4.
tg = 1.25α C – 1.14
r = 0.999
0
10
20
30
40
50
60
70
0 10 20 30 40 50 60
tgα,
10
–3
min
–1
C, g mLμ
–1
Figure 3. The calibration graph for the quantitative determination of Oxa, с(КНSO5) = 2×10–3 mol L–1; с(NaOH) = 6.1×10–3 mol L–1
Table 1. Results of the quantitative determination
of oxacillin by the kinetic spectrophotometric method
in the Oxa drug according to the reaction with potassium
hydrogen peroxomonosulfate (Р = 0.95, n = 7)
Oxacillin
taken, mg
Found Results of processing
statistical datamg %
503.1[a]
494.2 98.8
x = 496.3 (99.3 %)
S = ± 8.41580
Sx = ± 3.18087
Δx ± 7.79314
RSD = ± 1.7 %
ε = ± 1.57 %
δ[b] = –1.35 %
491.7 98.3
495.3 99.1
505.8 101.2
498.1 99.6
506.6 101.3
482.2 96.4
Note: [a] The Oxa content indicated in the quality certificate (m);
[b] δ = x – µ) × 100 % × µ–1
KHSO5
- KHSO4
N
S
O
O
O
H
N
O
O
N
Me
Me
Me
H
N
S
O
O
O
H
N
O
O
N
Me
Me
Me
H
O
Na Na
Figure 4. The scheme of S-oxidation of Oxa by Potassium hydrogen peroxomonosulfate
Table 2. Results of the quantitative determination
of oxacillin by redox titration in the Oxa drug by the reaction
with Potassium hydrogen peroxomonosulfate
(P = 0.95, n = 7)
Oxacillin
taken, mg
Found Results of processing
statistical datamg %
503.1[a]
498.5 99.7
x = 500.1 (100.02 %)
S = ± 1.43228
Sx = ± 0.54135
Δx = ± 1.32631
RSD = ± 0.29 %
ε = ± 0.27 %
δ[b] = –0.60 %
501.2 100.2
499.3 99.9
502.1 100.4
499.6 99.9
501.4 100.3
498.7 99.7
Note: [a] The Oxa content indicated in the quality certificate;
[b] δ = x – µ)×100 %×µ–1
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Журнал органічної та фармацевтичної хімії 2023, 21 (2)
The content of С19Н19N3O4S (Х, in %) was cal-
culated by the formula:
X =
0.02· K 423.43· ( – )· 100· 100 %· V V0
2· 1000· · (100 – )m ws H O2
where V0 – is the volume of sodium thiosulfate
solution in the control experiment, mL;
V – is the volume of sodium thiosulfate solution
studied, mL;
423.43 – is the molar mass of oxacillin (anhy-
drous), g mol–1;
K – is the correction coefficient for the concentra-
tion of sodium thiosulfate solution to 0.0200 mol L–1;
ms – is the weighed portions of Oxa, g.
The results of the analysis of the Oxa drug
by redox titration are shown in Table 2. The re-
lative standard deviation did not exceed 0.3 %
(δ = –0.60 %).
■ Conclusions
Using the methods of kinetic spectropho-
tometric and redox titration, two independent
procedures for the quantitative determination
of oxacillin in the substance and the drug pro-
duct have been developed using potassium hy-
drogen peroxomonosulfate as an analytical rea-
gent (KHSO5).
■ References
1. The United States Pharmacopeia USP38; United States Pharmacopeial Convention: Rockville, MD, 2015.
2. The British Pharmacopeia; The Stationery Office: London, 2014.
3. The United States Pharmacopeia USP30, the national formulary NF25; United States Pharmacopeial Convention: Rockville, MD, 2008.
4. Wang, P.; Liu, H. L.; Wang, B.; Cheng, X. W.; Chen, Q. H.; Fu, H. A Method for Determination of Penicillin G Residue in Waste
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Information about the authors:
Svitlana P. Karpova (corresponding author), Ph.D. in Pharmacy, Associate Professor of the General Chemistry Department,
National University of Pharmacy of the Ministry of Health of Ukraine; https://orcid.org/0000-0001-7274-7750;
e-mail for correspondence: za9594506@gmail.com; tel. +380982008557.
Maryna M. Ivashura, Ph.D. in Agricultural Science, Associate Professor of the General Chemistry Department,
National University of Pharmacy of the Ministry of Health of Ukraine; http://orcid.org/0000-0003-3427-6024.
Alla O. Koval, Ph.D. in Pharmacy, Associate Professor of the General Chemistry Department, National University
of Pharmacy of the Ministry of Health of Ukraine; https://orcid.org/0000-0001-9491-0459.
Yulia S. Kolisnyk, Ph.D. in Pharmacy, Associate Professor of the General Chemistry Department, National University
of Pharmacy of the Ministry of Health of Ukraine; https://orcid.org/0000-0002-6057-3447.
|
| id | oai:ojs.journals.uran.ua:article-273654 |
| institution | Journal of Organic and Pharmaceutical Chemistry |
| issn | 2518-1548 |
| keywords_txt_mv | |
| language | English |
| last_indexed | 2026-08-24T01:00:31Z |
| publishDate | 2023 |
| publisher | National University of Pharmacy |
| record_format | ojs |
| resource_txt_mv | ophcjnupheduua/db/d201323dcad02941d430bb0311476bdb.pdf |
| spelling | oai:ojs.journals.uran.ua:article-2736542026-08-23T19:38:20Z The Quantitative Determination of Oxacillin Using Kinetiс-Spectrophotometric and Redox Titration Methods Кількісне визначення оксациліну методами кінетико-спектрофотометрії та окисно-відновного титрування Karpova, Svetlana P. Ivashura, Maryna M. Koval, Alla O. Kolisnyk, Yulia S. оксацилін калій гідрогенпероксомоносульфат йодометрія кінетико-спектрофотометрія oxacillin potassium hydrogen peroxomonosulfate iodometry kinetic spectrophotometry The search for new analytical reactions and finding out the optimal conditions for their course, which can be used as the basis for quantitative analytical determinations of penicillins, is a very urgent task.Aim. To develop methods for the quantitative determination of Oxacillin.Materials and methods. The study object was Oxacillin sodium salt powder in vials for preparing a solution for injections(0.5 g). Peroxomonosulfate acid as triple potassium salt 2КНSO5∙КНSO4∙K2SO4 (Oxone®) of “extra pure” grade was used as an oxidant. The methods of kinetic spectriphotometry and redox titration were used.Results and discussion. A simple procedure for the quantitative determination of the Oxacillin pure substance by the kinetic spectrophotometry and redox titration methods using potassium hydrogen peroxomonosulfate (KHSO5) has been developed. The results of the drug analysis obtained by newly developed and current methods are in good agreement with each other; δ (correctness) = (0.45 – 0.86) %.Conclusions. Using the methods of kinetic spectrophotometric and redox titration, two independent procedures for thequantitative determination of oxacillin in the substance and the drug product have been developed using potassium hydrogen peroxomonosulfate as an analytical reagent (KHSO5). A relative standard deviation RSD = (1.24 – 2.17) %. Мета. Пошук нових аналітичних реакцій та з’ясування оптимальних умов їх перебігу, які можуть бути покладені в основу кількісних аналітичних визначень пеніцилінів, є вельми актуальним завданням. Метою цієї роботи було розробити методики кількісного визначення оксациліну.Матеріали та методи. Обʼєктом дослідження був Оксацилін – порошок натрій оксациліну у флаконах для приготування розчину для ін’єкцій (0,5 г). Як окисник використовували потрійну калієву сіль 2КНSO5∙КНSO4∙K2SO4 кваліфікації “extra pure” (Oxone®). У дослідженні було задіяно методи кінетико-спектрофотометрії та окисно-відновного титрування.Результати та їх обговорення. Розроблено процедуру кількісного визначення оксациліну методами кінетико-спектрофотометрії та йодометричного титрування з використанням калій гідрогенпероксомоносульфату. Результати аналізу препарату, одержані за новоопрацьованими та чинними методиками, добре узгоджуються між собою; δ (правильність) = (0.45 – 0.86) %.Висновки. За допомогою методів кінетико-спектрофотометрії та йодометричного титрування розроблено дві незалежні методики кількісного визначення оксациліну в субстанції та лікарському препараті з використанням калій гідрогенпероксомоносульфату як аналітичного реагенту (KHSO5). Відносне стандартне відхилення RSD (1,24 – 2,17) %. National University of Pharmacy 2023-08-30 Article Article application/pdf https://ophcj.nuph.edu.ua/article/view/273654 10.24959/ophcj.23.273654 Journal of Organic and Pharmaceutical Chemistry; Vol. 21 No. 2 (2023); 15-20 Журнал органической и фармацевтической химии; Том 21 № 2 (2023); 15-20 Журнал органічної та фармацевтичної хімії; Том 21 № 2 (2023); 15-20 2518-1548 2308-8303 en https://ophcj.nuph.edu.ua/article/view/273654/274430 Copyright (c) 2023 Svetlana P. Karpova, Maryna M. Ivashura, Alla O. Koval, Yulia S. Kolisnyk http://creativecommons.org/licenses/by/4.0 |
| spellingShingle | оксацилін калій гідрогенпероксомоносульфат йодометрія кінетико-спектрофотометрія Karpova, Svetlana P. Ivashura, Maryna M. Koval, Alla O. Kolisnyk, Yulia S. Кількісне визначення оксациліну методами кінетико-спектрофотометрії та окисно-відновного титрування |
| title | Кількісне визначення оксациліну методами кінетико-спектрофотометрії та окисно-відновного титрування |
| title_alt | The Quantitative Determination of Oxacillin Using Kinetiс-Spectrophotometric and Redox Titration Methods |
| title_full | Кількісне визначення оксациліну методами кінетико-спектрофотометрії та окисно-відновного титрування |
| title_fullStr | Кількісне визначення оксациліну методами кінетико-спектрофотометрії та окисно-відновного титрування |
| title_full_unstemmed | Кількісне визначення оксациліну методами кінетико-спектрофотометрії та окисно-відновного титрування |
| title_short | Кількісне визначення оксациліну методами кінетико-спектрофотометрії та окисно-відновного титрування |
| title_sort | кількісне визначення оксациліну методами кінетико-спектрофотометрії та окисно-відновного титрування |
| topic | оксацилін калій гідрогенпероксомоносульфат йодометрія кінетико-спектрофотометрія |
| topic_facet | оксацилін калій гідрогенпероксомоносульфат йодометрія кінетико-спектрофотометрія oxacillin potassium hydrogen peroxomonosulfate iodometry kinetic spectrophotometry |
| url | https://ophcj.nuph.edu.ua/article/view/273654 |
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