Determination of saccharin in pharmaceuticals by high performance thin layer chromatography
Određivanje saharina u farmaceutskim preparatima primenom visoko efikasne tankoslojne hromatografije
Апстракт
A simple, accurate and selective high performance thin layer chromatographic method for the determination of saccharin in pharmaceuticals has been developed. The chromatography was performed on silica-gel 60F254 plates with ethyl acetate-carbon tetrachloride-acetic acid (3 + 4 + 0.5 v/v/v) as the mobile phase. The chromatographic zones corresponding to the saccharin spots were scanned in the reflectance/absorbance mode at λ=230 mm. For the standard curves, two series of saccharin sodium salt solutions were prepared: in methanol (solvent 1) and in ethyl acetate-acetic acid (9:1, v/v) mixture (solvent 2). A linear calibration relationship was observed within the concentration range from 300-1200 ng saccharin sodium salt per spot correlation coefficients being 0.998 (solvent 1) and 0.995 (solvent 2). The relationship between the peak area and the amount of saccharin sodium salt was evaluated by linear regression analysis. The limits of detection and quantification of saccharin sodium salt... were 35 ng and 110 ng per spot (solvent 1), respectively, and 45 ng and 150 ng per spot (solvent 2) respectively. Mean recovery values of 103.5 % (solvent 1) and 102.3 % (solvent 2), and RSD values of 4.42 % (solvent 1) and 2.53 % (solvent 2) were obtained. The proposed method was applied for saccharin determination in two pharmaceutical preparations, effervescent tablets and a carbomer- based gel.
Predložena je jednostavna i selektivna metoda za određivanje saharina u farmaceutskim preparatima primenom visoko efikasne tankoslojne hromatografije. Određivanja su vršena na silika-gel pločama 60F254 koristeći kao mobilnu fazu smešu etilacetata, ugljentetrahlorida i sirćetne kiseline (3 + 4 + 0,5, v/v/v). Pripremljene su dve serije standardnih rastvora natrijumove soli saharina: u metanolu (rastvarač 1) i smeši etilacetat-sirćetna kiselina (9:1, v/v) (rastvarač 2). Kalibracione krive snimljene su na talasnoj dužini od 230 nm u opsegu nanetih količina natrijumove soli saharina (300-1200 ng), sa koeficijentima korelacije 0,998 (rastvarač 1) i 0,995 (rastvarač 2). U ispitivanom opsegu utvrđena je linearna zavisnost između površine pikova i količine natrijumove soli saharina. Limit detekcije i limit kvantifikacije saharina iznosili su redom 35 ng i 110 ng (rastvarač 1) i 45 ng i 150 ng (rastvarač 2). Dobijene su sledeće vrednosti za "recovery" i relativnu standardnu devijaciju: 103,5 % i... 4,42 % (rastvarač 1) i 102,3 % i 2,53 % (rastvarač 2). Predložena metoda je primenjena za određivanje saharina u šumećim tabletama Kalcijum® i Daktanol® gelu.
Кључне речи:
saccharin / HPTLC determination / effervescent tablets / carbomer-based gelИзвор:
Journal of the Serbian Chemical Society, 2006, 71, 6, 669-676Издавач:
- Srpsko hemijsko društvo, Beograd
DOI: 10.2298/JSC0606669C
ISSN: 0352-5139
WoS: 000240444400011
Scopus: 2-s2.0-33748930806
Институција/група
PharmacyTY - JOUR AU - Čakar, Mira AU - Popović, Gordana PY - 2006 UR - https://farfar.pharmacy.bg.ac.rs/handle/123456789/879 AB - A simple, accurate and selective high performance thin layer chromatographic method for the determination of saccharin in pharmaceuticals has been developed. The chromatography was performed on silica-gel 60F254 plates with ethyl acetate-carbon tetrachloride-acetic acid (3 + 4 + 0.5 v/v/v) as the mobile phase. The chromatographic zones corresponding to the saccharin spots were scanned in the reflectance/absorbance mode at λ=230 mm. For the standard curves, two series of saccharin sodium salt solutions were prepared: in methanol (solvent 1) and in ethyl acetate-acetic acid (9:1, v/v) mixture (solvent 2). A linear calibration relationship was observed within the concentration range from 300-1200 ng saccharin sodium salt per spot correlation coefficients being 0.998 (solvent 1) and 0.995 (solvent 2). The relationship between the peak area and the amount of saccharin sodium salt was evaluated by linear regression analysis. The limits of detection and quantification of saccharin sodium salt were 35 ng and 110 ng per spot (solvent 1), respectively, and 45 ng and 150 ng per spot (solvent 2) respectively. Mean recovery values of 103.5 % (solvent 1) and 102.3 % (solvent 2), and RSD values of 4.42 % (solvent 1) and 2.53 % (solvent 2) were obtained. The proposed method was applied for saccharin determination in two pharmaceutical preparations, effervescent tablets and a carbomer- based gel. AB - Predložena je jednostavna i selektivna metoda za određivanje saharina u farmaceutskim preparatima primenom visoko efikasne tankoslojne hromatografije. Određivanja su vršena na silika-gel pločama 60F254 koristeći kao mobilnu fazu smešu etilacetata, ugljentetrahlorida i sirćetne kiseline (3 + 4 + 0,5, v/v/v). Pripremljene su dve serije standardnih rastvora natrijumove soli saharina: u metanolu (rastvarač 1) i smeši etilacetat-sirćetna kiselina (9:1, v/v) (rastvarač 2). Kalibracione krive snimljene su na talasnoj dužini od 230 nm u opsegu nanetih količina natrijumove soli saharina (300-1200 ng), sa koeficijentima korelacije 0,998 (rastvarač 1) i 0,995 (rastvarač 2). U ispitivanom opsegu utvrđena je linearna zavisnost između površine pikova i količine natrijumove soli saharina. Limit detekcije i limit kvantifikacije saharina iznosili su redom 35 ng i 110 ng (rastvarač 1) i 45 ng i 150 ng (rastvarač 2). Dobijene su sledeće vrednosti za "recovery" i relativnu standardnu devijaciju: 103,5 % i 4,42 % (rastvarač 1) i 102,3 % i 2,53 % (rastvarač 2). Predložena metoda je primenjena za određivanje saharina u šumećim tabletama Kalcijum® i Daktanol® gelu. PB - Srpsko hemijsko društvo, Beograd T2 - Journal of the Serbian Chemical Society T1 - Determination of saccharin in pharmaceuticals by high performance thin layer chromatography T1 - Određivanje saharina u farmaceutskim preparatima primenom visoko efikasne tankoslojne hromatografije VL - 71 IS - 6 SP - 669 EP - 676 DO - 10.2298/JSC0606669C ER -
@article{ author = "Čakar, Mira and Popović, Gordana", year = "2006", abstract = "A simple, accurate and selective high performance thin layer chromatographic method for the determination of saccharin in pharmaceuticals has been developed. The chromatography was performed on silica-gel 60F254 plates with ethyl acetate-carbon tetrachloride-acetic acid (3 + 4 + 0.5 v/v/v) as the mobile phase. The chromatographic zones corresponding to the saccharin spots were scanned in the reflectance/absorbance mode at λ=230 mm. For the standard curves, two series of saccharin sodium salt solutions were prepared: in methanol (solvent 1) and in ethyl acetate-acetic acid (9:1, v/v) mixture (solvent 2). A linear calibration relationship was observed within the concentration range from 300-1200 ng saccharin sodium salt per spot correlation coefficients being 0.998 (solvent 1) and 0.995 (solvent 2). The relationship between the peak area and the amount of saccharin sodium salt was evaluated by linear regression analysis. The limits of detection and quantification of saccharin sodium salt were 35 ng and 110 ng per spot (solvent 1), respectively, and 45 ng and 150 ng per spot (solvent 2) respectively. Mean recovery values of 103.5 % (solvent 1) and 102.3 % (solvent 2), and RSD values of 4.42 % (solvent 1) and 2.53 % (solvent 2) were obtained. The proposed method was applied for saccharin determination in two pharmaceutical preparations, effervescent tablets and a carbomer- based gel., Predložena je jednostavna i selektivna metoda za određivanje saharina u farmaceutskim preparatima primenom visoko efikasne tankoslojne hromatografije. Određivanja su vršena na silika-gel pločama 60F254 koristeći kao mobilnu fazu smešu etilacetata, ugljentetrahlorida i sirćetne kiseline (3 + 4 + 0,5, v/v/v). Pripremljene su dve serije standardnih rastvora natrijumove soli saharina: u metanolu (rastvarač 1) i smeši etilacetat-sirćetna kiselina (9:1, v/v) (rastvarač 2). Kalibracione krive snimljene su na talasnoj dužini od 230 nm u opsegu nanetih količina natrijumove soli saharina (300-1200 ng), sa koeficijentima korelacije 0,998 (rastvarač 1) i 0,995 (rastvarač 2). U ispitivanom opsegu utvrđena je linearna zavisnost između površine pikova i količine natrijumove soli saharina. Limit detekcije i limit kvantifikacije saharina iznosili su redom 35 ng i 110 ng (rastvarač 1) i 45 ng i 150 ng (rastvarač 2). Dobijene su sledeće vrednosti za "recovery" i relativnu standardnu devijaciju: 103,5 % i 4,42 % (rastvarač 1) i 102,3 % i 2,53 % (rastvarač 2). Predložena metoda je primenjena za određivanje saharina u šumećim tabletama Kalcijum® i Daktanol® gelu.", publisher = "Srpsko hemijsko društvo, Beograd", journal = "Journal of the Serbian Chemical Society", title = "Determination of saccharin in pharmaceuticals by high performance thin layer chromatography, Određivanje saharina u farmaceutskim preparatima primenom visoko efikasne tankoslojne hromatografije", volume = "71", number = "6", pages = "669-676", doi = "10.2298/JSC0606669C" }
Čakar, M.,& Popović, G.. (2006). Determination of saccharin in pharmaceuticals by high performance thin layer chromatography. in Journal of the Serbian Chemical Society Srpsko hemijsko društvo, Beograd., 71(6), 669-676. https://doi.org/10.2298/JSC0606669C
Čakar M, Popović G. Determination of saccharin in pharmaceuticals by high performance thin layer chromatography. in Journal of the Serbian Chemical Society. 2006;71(6):669-676. doi:10.2298/JSC0606669C .
Čakar, Mira, Popović, Gordana, "Determination of saccharin in pharmaceuticals by high performance thin layer chromatography" in Journal of the Serbian Chemical Society, 71, no. 6 (2006):669-676, https://doi.org/10.2298/JSC0606669C . .