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Development of chromatographic methods for analysis of sulfamethoxazole, trimethoprim, their degradation products and preservatives in syrup

Razvoj hromatografskih metoda za analizu sulfametoksazola, trimetoprima, njihovih degradacionih proizvoda i konzervanasa u sirupu

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2014
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Authors
Perović, Ivana
Malenović, Anđelija
Vemić, Ana
Kostić, Nađa
Ivanović, Darko
Article (Published version)
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Abstract
In this paper the experimental conditions for optimal reversed-phase liquid chromatographic (RP-HPLC) determination of sulfamethoxazole, trimethoprim and preservatives, as well as degradation products of sulfamethoxazole and trimethoprim in syrup were defined. The determination of active compounds and preservatives was carried out on Zorbax Eclipse XDB-C18, 150 mm × 4.6 mm, 5 μm particle size column, mobile phase flow rate was 1.5 mL min-1, and detection at 235 nm for the active compounds and 254 nm for preservatives. Mobile phase A consisted of 150 mL of acetonitrile, 850 mL of water and 1 mL of triethanolamine (pH 5.90 adjusted with diluted acetic acid), while mobile phase B was acetonitrile. The mobile phase ratio was defined by the gradient program. For the determination of degradation products Zorbax Eclipse Plus C18, 100 mm x 4.6 mm, 3.5 μm particle size column was used, the mobile phase flow rate was 0.5 mL min-1 and detection at 210 nm for 3,4,5-trimethoxybenzoic acid and 254 n...m for sulfanilic acid and sulfanilamide. Mobile phase A was 50 mM potassium dihydrogenphosphate (pH 5.60 adjusted with a 0.5 mol L-1 potassium hydroxide), while mobile phase B was acetonitrile. The mobile phase ratio was defined by the gradient program. Through the validation of the developed methods their efficiency and reliability is confirmed and consequently the adequacy for the routine control.

U ovom radu prikazano je definisanje eksperimentalnih uslova i optimizacija metoda reverzno-fazne tečne hromatografije (RP-HPLC) za određivanje sulfametoksazola, trimetoprima i konzervanasa, odnosno degradacionih proizvoda sulfametoksazola i trimetoprima u sirupu. Određivanje sadržaja aktivnih komponenti i konzervanasa vršeno je na koloni Zorbax Eclipse XDB-C18, 150 mm × 4,6 mm, 5 μm veličine čestica, protok mobilne faze bio je 1,5 mL min-1, dok je detekcija vršena na 235 nm za aktivne komponente i 254 nm za konzervanse. Mobilna faza A sastojala se od smeše 150 mL acetonitrila, 850 mL vode i 1 mL trietanolamina (pH 5,9 podešen razblaženom sirćetnom kiselinom), a kao mobilna faza B korišćen je acetonitril. Odnos mobilnih faza tokom analize definisan je programom gradijenta. Određivanje sadržaja degradacionih proizvoda vršeno je na koloni Zorbax Eclipse Plus-C18, 100 mm × 4,6 mm, 3,5 μm veličine čestica, uz protok mobilne faze od 0,5 mL min-1 i detekciju na 210 nm za 3,4,5-trimetoksibenz...ojevu kiselinu i 254 nm za sulfanilnu kiselinu i sulfanilamid. Mobilna faza A bila je 50 mM kalijum-dihidrogenfosfat (pH 5,60 podešen sa 0,5 mol L-1 kalijum-hidroksidom), a mobilna faza B bio je acetonitril. Odnos mobilnih faza tokom analize definisan je programom gradijenta. Validacijom postavljenih metoda potvrđeno je da su efikasne i pouzdane, i kao takve pogodne za rutinsku kontrolu.

Keywords:
sulfamethoxazole / trimethoprim / preservatives / degradation products / reversed-phase liquid chromatography / Sulfametoksazol / trimetoprim / konzervansi / degradacioni proizvodi / reverzno-fazna tečna hromatografija
Source:
Arhiv za farmaciju, 2014, 64, 2, 112-127
Publisher:
  • Savez farmaceutskih udruženja Srbije, Beograd
Funding / projects:
  • Modelling of different chromatographic systems with chemometrical approach in pharmaceutical analysis (RS-172052)

DOI: 10.5937/arhfarm1402112P

ISSN: 0004-1963

Scopus: 2-s2.0-84943629457
[ Google Scholar ]
1
URI
https://farfar.pharmacy.bg.ac.rs/handle/123456789/2242
Collections
  • Radovi istraživača / Researchers’ publications
Institution/Community
Pharmacy
TY  - JOUR
AU  - Perović, Ivana
AU  - Malenović, Anđelija
AU  - Vemić, Ana
AU  - Kostić, Nađa
AU  - Ivanović, Darko
PY  - 2014
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/2242
AB  - In this paper the experimental conditions for optimal reversed-phase liquid chromatographic (RP-HPLC) determination of sulfamethoxazole, trimethoprim and preservatives, as well as degradation products of sulfamethoxazole and trimethoprim in syrup were defined. The determination of active compounds and preservatives was carried out on Zorbax Eclipse XDB-C18, 150 mm × 4.6 mm, 5 μm particle size column, mobile phase flow rate was 1.5 mL min-1, and detection at 235 nm for the active compounds and 254 nm for preservatives. Mobile phase A consisted of 150 mL of acetonitrile, 850 mL of water and 1 mL of triethanolamine (pH 5.90 adjusted with diluted acetic acid), while mobile phase B was acetonitrile. The mobile phase ratio was defined by the gradient program. For the determination of degradation products Zorbax Eclipse Plus C18, 100 mm x 4.6 mm, 3.5 μm particle size column was used, the mobile phase flow rate was 0.5 mL min-1 and detection at 210 nm for 3,4,5-trimethoxybenzoic acid and 254 nm for sulfanilic acid and sulfanilamide. Mobile phase A was 50 mM potassium dihydrogenphosphate (pH 5.60 adjusted with a 0.5 mol L-1 potassium hydroxide), while mobile phase B was acetonitrile. The mobile phase ratio was defined by the gradient program. Through the validation of the developed methods their efficiency and reliability is confirmed and consequently the adequacy for the routine control.
AB  - U ovom radu prikazano je definisanje eksperimentalnih uslova i optimizacija metoda reverzno-fazne tečne hromatografije (RP-HPLC) za određivanje sulfametoksazola, trimetoprima i konzervanasa, odnosno degradacionih proizvoda sulfametoksazola i trimetoprima u sirupu. Određivanje sadržaja aktivnih komponenti i konzervanasa vršeno je na koloni Zorbax Eclipse XDB-C18, 150 mm × 4,6 mm, 5 μm veličine čestica, protok mobilne faze bio je 1,5 mL min-1, dok je detekcija vršena na 235 nm za aktivne komponente i 254 nm za konzervanse. Mobilna faza A sastojala se od smeše 150 mL acetonitrila, 850 mL vode i 1 mL trietanolamina (pH 5,9 podešen razblaženom sirćetnom kiselinom), a kao mobilna faza B korišćen je acetonitril. Odnos mobilnih faza tokom analize definisan je programom gradijenta. Određivanje sadržaja degradacionih proizvoda vršeno je na koloni Zorbax Eclipse Plus-C18, 100 mm × 4,6 mm, 3,5 μm veličine čestica, uz protok mobilne faze od 0,5 mL min-1 i detekciju na 210 nm za 3,4,5-trimetoksibenzojevu kiselinu i 254 nm za sulfanilnu kiselinu i sulfanilamid. Mobilna faza A bila je 50 mM kalijum-dihidrogenfosfat (pH 5,60 podešen sa 0,5 mol L-1 kalijum-hidroksidom), a mobilna faza B bio je acetonitril. Odnos mobilnih faza tokom analize definisan je programom gradijenta. Validacijom postavljenih metoda potvrđeno je da su efikasne i pouzdane, i kao takve pogodne za rutinsku kontrolu.
PB  - Savez farmaceutskih udruženja Srbije, Beograd
T2  - Arhiv za farmaciju
T1  - Development of chromatographic methods for analysis of sulfamethoxazole, trimethoprim, their degradation products and preservatives in syrup
T1  - Razvoj hromatografskih metoda za analizu sulfametoksazola, trimetoprima, njihovih degradacionih proizvoda i konzervanasa u sirupu
VL  - 64
IS  - 2
SP  - 112
EP  - 127
DO  - 10.5937/arhfarm1402112P
ER  - 
@article{
author = "Perović, Ivana and Malenović, Anđelija and Vemić, Ana and Kostić, Nađa and Ivanović, Darko",
year = "2014",
abstract = "In this paper the experimental conditions for optimal reversed-phase liquid chromatographic (RP-HPLC) determination of sulfamethoxazole, trimethoprim and preservatives, as well as degradation products of sulfamethoxazole and trimethoprim in syrup were defined. The determination of active compounds and preservatives was carried out on Zorbax Eclipse XDB-C18, 150 mm × 4.6 mm, 5 μm particle size column, mobile phase flow rate was 1.5 mL min-1, and detection at 235 nm for the active compounds and 254 nm for preservatives. Mobile phase A consisted of 150 mL of acetonitrile, 850 mL of water and 1 mL of triethanolamine (pH 5.90 adjusted with diluted acetic acid), while mobile phase B was acetonitrile. The mobile phase ratio was defined by the gradient program. For the determination of degradation products Zorbax Eclipse Plus C18, 100 mm x 4.6 mm, 3.5 μm particle size column was used, the mobile phase flow rate was 0.5 mL min-1 and detection at 210 nm for 3,4,5-trimethoxybenzoic acid and 254 nm for sulfanilic acid and sulfanilamide. Mobile phase A was 50 mM potassium dihydrogenphosphate (pH 5.60 adjusted with a 0.5 mol L-1 potassium hydroxide), while mobile phase B was acetonitrile. The mobile phase ratio was defined by the gradient program. Through the validation of the developed methods their efficiency and reliability is confirmed and consequently the adequacy for the routine control., U ovom radu prikazano je definisanje eksperimentalnih uslova i optimizacija metoda reverzno-fazne tečne hromatografije (RP-HPLC) za određivanje sulfametoksazola, trimetoprima i konzervanasa, odnosno degradacionih proizvoda sulfametoksazola i trimetoprima u sirupu. Određivanje sadržaja aktivnih komponenti i konzervanasa vršeno je na koloni Zorbax Eclipse XDB-C18, 150 mm × 4,6 mm, 5 μm veličine čestica, protok mobilne faze bio je 1,5 mL min-1, dok je detekcija vršena na 235 nm za aktivne komponente i 254 nm za konzervanse. Mobilna faza A sastojala se od smeše 150 mL acetonitrila, 850 mL vode i 1 mL trietanolamina (pH 5,9 podešen razblaženom sirćetnom kiselinom), a kao mobilna faza B korišćen je acetonitril. Odnos mobilnih faza tokom analize definisan je programom gradijenta. Određivanje sadržaja degradacionih proizvoda vršeno je na koloni Zorbax Eclipse Plus-C18, 100 mm × 4,6 mm, 3,5 μm veličine čestica, uz protok mobilne faze od 0,5 mL min-1 i detekciju na 210 nm za 3,4,5-trimetoksibenzojevu kiselinu i 254 nm za sulfanilnu kiselinu i sulfanilamid. Mobilna faza A bila je 50 mM kalijum-dihidrogenfosfat (pH 5,60 podešen sa 0,5 mol L-1 kalijum-hidroksidom), a mobilna faza B bio je acetonitril. Odnos mobilnih faza tokom analize definisan je programom gradijenta. Validacijom postavljenih metoda potvrđeno je da su efikasne i pouzdane, i kao takve pogodne za rutinsku kontrolu.",
publisher = "Savez farmaceutskih udruženja Srbije, Beograd",
journal = "Arhiv za farmaciju",
title = "Development of chromatographic methods for analysis of sulfamethoxazole, trimethoprim, their degradation products and preservatives in syrup, Razvoj hromatografskih metoda za analizu sulfametoksazola, trimetoprima, njihovih degradacionih proizvoda i konzervanasa u sirupu",
volume = "64",
number = "2",
pages = "112-127",
doi = "10.5937/arhfarm1402112P"
}
Perović, I., Malenović, A., Vemić, A., Kostić, N.,& Ivanović, D.. (2014). Development of chromatographic methods for analysis of sulfamethoxazole, trimethoprim, their degradation products and preservatives in syrup. in Arhiv za farmaciju
Savez farmaceutskih udruženja Srbije, Beograd., 64(2), 112-127.
https://doi.org/10.5937/arhfarm1402112P
Perović I, Malenović A, Vemić A, Kostić N, Ivanović D. Development of chromatographic methods for analysis of sulfamethoxazole, trimethoprim, their degradation products and preservatives in syrup. in Arhiv za farmaciju. 2014;64(2):112-127.
doi:10.5937/arhfarm1402112P .
Perović, Ivana, Malenović, Anđelija, Vemić, Ana, Kostić, Nađa, Ivanović, Darko, "Development of chromatographic methods for analysis of sulfamethoxazole, trimethoprim, their degradation products and preservatives in syrup" in Arhiv za farmaciju, 64, no. 2 (2014):112-127,
https://doi.org/10.5937/arhfarm1402112P . .

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