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1

An eco-friendly micellar HPLC method for the simultaneous determination of triamterene and xipamide in active pharmaceutical ingredients and marketed tablet dosage form

Ayad Magda M, Hosny Mervat M., Ibrahim Adel Ehab, El-Abassy Omar M., Belal Fathalla F.

Acta Chromatographica

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2021

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Vol. 33, no. 1

51--56

EN

In the last few years, the use of surfactants as mobile phase additives in reversed phase liquid chromatography (RPLC) has been steadily developing and improving. Surfactants modify the polarity of the stationary phase which in turn decreases the amount of organic solvent required for elution of the analytes rendering the methodologies linked to them greener and more eco-friendly. Brij-35 is a fatty alcohol ethoxylates non ionic surfactant, which is less widely used as mobile phase additive. Brij-35 can decrease stationary phase polarity while remaining neutral. In this research, Brij-35 was studied in the separation and determination of marketed antihypertensive combination therapy composed of triamterene (TRM) and xipamide (XIP). TRM and XIP are diuretics used for treatment of essential hypertension and associated edema conditions. Chromatographic separation was achieved on RP-C18 column (Kinetix®, 5 mm, 15 cm 3 4.6 mm) at flow rate 1 mL min1 and UV-detection at 254 nm. Isocratic elution was performed using mobile phase composed of 0.1 M Brij-35: methanol (MeOH) (60:40, v/v). The analytes were well separated and quantified within linearity ranges of 5–50 mg mL1 for both drugs in short retention time (2.6 and 5.3 min. for TRM and XIP, respectively). Since claiming greenness is not enough, Green Analytical Procedure Index (GAPI) was used to demonstrate the superiority of the proposed method over the previously reported methods. GAPI is a new metric for evaluation of the ecological impact of analytical procedures. The proposed method was validated according to ICH guidelines and applied successfully for simultaneous determination of the drugs in their co-formulated tablets.

2

Chemometrically optimized micellar liquid chromatographic method for the simultaneous determination of cetirizine dihydrochloride in its combined dosage forms. Application to biological fluids and pharmacokinetic studies

Sharaf El Din M. K., Ibrahim F., Eid M. I., Wahba M. E. K.

Acta Chromatographica

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2013

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Vol. 25, no. 1

59--77

EN

An accurate, simple, sensitive, and selective micellar liquid chromatographic method has been developed for the simultaneous determination of cetirizine dihydrochloride in two of its combined pharmaceutical preparations with psudoephedrine hydrochloride and/or paracetamol. The chemometrics approach was applied for the optimization of separation of the studied drugs to optimize their separation; the effect of six experimental parameters on retention was investigated by means of multivariate analysis. Separation was conducted using an ODS C18 (150 × 4.6 mm id) stainless steel column at ambient temperature with UV-detection at 250 nm. A mobile phase composed of 0.135 M sodium dodecyl sulphate, 11% 1-propanol, 0.3% tri-ethylamine in 0.02 M phosphoric acid, and adjusted to pH 3.3 has been used at a flow rate of 1 mL/min. Regression models were characterized by both descriptive and predictive ability (R2 ≥ 98.8% and R2cv ≥ 94.5%) and allowed the chromatographic separation of the drugs with a good resolution and a total analysis time within 6 min.The calibration curves were rectilinear over the concentration ranges of 0.05–1.0, 0.07–4.0, and 1.0–10.0 μg/mL for cetirizine dihydrochloride, psudoephedrine hydrochloride, and paracetamol respectively; with detection limits of 0.01, 0.05, and 0.08 μg/mL, and quantification limits of 0.04, 0.09, and 1.02 μg/mL, respectively. The results obtained were in good agreement with those obtained by the comparison method. Furthermore, the method was applied for the determination of the drugs in spiked human plasma and used to reveal the pharmacokinetic characters in a healthy volunteer treated with oral administration of the studied two combined dosage forms of cetirizine.

3

Sole sodowe kwasów cholowych jako chiralne modyfikatory fazy ruchomej w układzie wysokosprawnej chromatografii cieczowej

Kowalczyk M., Asztemborska M.

Camera Separatoria

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2011

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Vol. 3, No. 1

161--184

PL

W pracy opisano zastosowanie cholanu sodu i deoksycholanu sodu, jako modyfikatorów fazy ruchomej w wysokosprawnej chromatografii cieczowej. Własności enancjoseparacyjne micelarnych faz chiralnych dla optycznie czynnych pochodnych binaftyli: fosforanu- 1,1’- -binaftylo-2,2’-diylu oraz 1,1’-binaftylo-2,2’-diolu. Zbadano proces adsorpcji cholanu i deoksycholanu sodu na fazie C18. Zbadano wpływ stężenia i typu surfaktantu, jak również rodzaj i stężenie dodatku organicznego (n-alkohol) na proces rozpoznania chiralnego przez badane układy micelarne.

EN

In the paper the application of sodium cholate and sodium deoxycholate as modifiers of mobile phase in high performance liquid chromatography was described. Enantioseparation properties of micellar chiral phases were studied for optically active derivatives of binaphthyls: 1,1'-binaphthyl-2,2'-diyl hydrogenphosphate and 1,1'-binaphthalene-2,2'-diol. The process of adsorption of sodium cholate and sodium deoxycholate on C18 phase was studied. The influence of type and concentration of surfactant as well as type and concentration of organic additive (n-alcohol) on process of chiral recognition was investigated. It has been found that enantiorecognition of bile salts micelle increase with the increase of the chain length of n-alcohol.

4

Retention mechanism of sulfonamides in micellar reversed phase liquid chromatography

Szymański A.

Ars Separatoria Acta

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2011

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No. 8

69-80

EN

A mechanism of retention of sulfonamides in the micellar liquid chromatography, based on similar models verified for other compounds, was proposed. The magnitudes of hydrophobic and electrostatic interactions of sulfonamides were estimated for different concentrations of surfactant in the mobile phase and at varied pH. With increasing SDS concentrations and at a constant pH, a decrease in the hydrophobic interaction intensity was noted. When pH is varied, the values of the constant, describing the hydrophobicity of the sulfonamides, remained at an approximately same level (taking into account the standard deviation values). Greater differences were observed in the constants related to the electrostatic interactions informing about the increase or decrease in retention, following from ionic interactions. For each sulfonamide, the molar fraction of the ionic fractions present in the mobile phase was calculated from the formula derived, which permitted determination of the type of electrostatic interactions, varying with the eluent’s changing pH. On the basis of the chromatographic data collected, it was established that retention of sulfonamides in the SDS micellar system depends on the hydrophobic and electrostatic interactions. For varied pH values, the hydrophobic interactions of sulfonamides did not change significantly, all changes in the retention of the sulfonamides were attributed to changes in the electrostatic interactions.

5

Relationship between micellar liquid chromatography retention of sulfonamides and the pH and concentration of surfactants and organic modifiers in the mobile phase

Szymański A.

Ars Separatoria Acta

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2011

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No. 8

51-67

EN

The paper presents an attempt to adapt a retention model suggested and verified by classic RP LC in micellar liquid chromatography, MLC. Instead of hydrophobic interactions with ODS groups and electrostatic interactions with silanol residues in C-18 packing, hydrophobic interactions with alkyl groups and ionic interactions with anionic moieties of the SDS-modified stationary phase were considered. Due to the different characteristics of the stationary phase in the MLC depending on the pH of the mobile phase, the equation used to determine the contribution of electrostatic interactions to retention was modified. Theoretical curves for the relationship between retention and SDS micelle concentration in the mobile phase, organic modifier concentration and eluent pH were determined. For comparison, curves based on data obtained in basic sulfonamide studies were plotted in the same coordinate systems and units. A complete qualitative similarity was noted between the theoretical curves predicting retention changes with changing micellar mobile phase parameters and the curves determined based on experimental results for the sulfonamides. The qualitative similarity involves a similar shape of the respective curves and identical tendencies. In general, a larger reduction of sulfonamide retention with respect to the predicted value is noted. The deviation results from changes in the sulfonamide property with changing pH of the mobile phase.

6

Simultaneous determination of sulf amethazine and sulfadimethoxine in meat, milk and egg by liquid-liquid. Extraction and micellar liquid chromatography

Szymański A.

Chemia i Inżynieria Ekologiczna

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2004

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Vol. 11, nr 11

1259-1265

EN

The method of high-pressure liquid chromatography with micellar mobile phase has been applied for simultaneous determination of sulfamethazine and sulfadimethoxine in food products of animal origin. Preliminary extraction and concentration of analyte have prepared samples for analyses by the liquid-liquid extraction. The linear range of the calibration curves for sulfamethazine and sulfadimethoxine was determined as from 50 to 500 [mu]g/kg (dm3) of the concentrations of the products analysed. The detection limit of both sulfonamides was 25 [mu]g per 1 kg of meat and eggs (1 dm3 milk). The method proposed is characterised by good precision and accuracy. The accuracy of measurements in meat was 3.0 to 12.8%, in milk 2.0 to 4.0%, in eggs 2.0 to 3.3%. The precision did not exceed 6.0% for meat, 4.1% for milk and 5.7% for eggs. The recovery of sulfonamides introduced into the food products studied was determined to vary in the range 87.2% for sulfadimethoxine to 104% for sulfadimethoxine in milk.

PL

Technikę wysokociśnieniowej chromatografii cieczowej z micelarną fazą ruchomą wykorzystano do jednoczesnego oznaczania sulfametazyny i sulfadimetoksyny w środkach spożywczych pochodzenia zwierzęcego. Próbki do analizy przygotowywano, wykorzystując metodę wstępnego wydzielania i zatężania analitu za pomocą ekstrakcji ciecz-ciecz. Zbadano prostoliniowy przebieg krzywych wzorcowych dla sulfametazyny i sulfadimetoksyny w przedziale stężeń od 50 do 500 [mu]g/kg (dm3) analizowanych produktów. Limit detekcji dla obu sulfonamidów wynosił 25 [mu]g na 1 kg mięsa i jaj (l dm3 mleka). Proponowana metoda charakteryzuje się dobrą precyzją i dokładnością. Dokładność dla badanych leków w mięsie przyjmowała wartości od -3.0 do 12.8%, w mleku od -2.0 do 4.0%, natomiast dla jaj wynosiła od -2.0 do 3.3%. Precyzja nie przekraczała 6.0% dla mięsa oraz 4.1% i 5.7% odpowiednio dla mleka i jaj. Wyznaczono również odzysk sulfonamidów wprowadzonych do badanych środków spożywczych. Mieścił się on w przedziale od 87.2% dla sulfadimetoksyny w mięsie do 104% dla sulfadimetoksyny w mleku.

7

Micellar liquid chromatography for the determination of sulfonamide residues in milk and eggs

Szymański A.

Chemia Analityczna

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2003

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Vol. 48, No. 3

429-438

EN

The micellar liquid chromatography for the determination of sulfonamide residues in milk and eggs was coupled with different methods of the sample pre-treatment: direct injection and extractive condensation of the analyte in the solid-solid and liquid-liquid system. The detection limit for the concentration range studied was 0.10 ug mL(-1) (direct sample injection DSJ), 0.05 ug ml/1 (solid-phase extraction SPE), and 0.025 ug ml/1 (liquid-liquid extraction LLE), for milk, and 0.025 ug mL(-1) (SPE and LLE) for eggs. The method provided high precision and accuracy. RSD value did not exceed 8% for milk and eggs, and the accuracy defined as the percentage difference between the mean amount found and that added varied from -2.0 to 5.0. The recovery of the spiked sulfonamides from milk and eggs was in the range from 96% to 105%.

PL

Przeprowadzono badania nad zastosowaniem micelarnej chromatografii cieczowej do oznaczania pozostałości sulfonamidów w mleku i jajach wykorzystując różne sposoby przygotowania próbki do analizy: bezpośredni nastrzyk próbki, ekstrakcyjne zatężenie analitu w układzie ciecz-ciało stałe i w układzie ciecz-ciecz. Granica detekcji w badanym zakresie stężeń w mleku wynosi 0.10 ug ml/1 dla DSI, 0.05 ug ml/1 dla SPE i 0.025 ug ml/(-1) dla LLE oraz w jajach 0.025 ug mL(-1) dla SPE i LLE. Opracowana metoda charakteryzuje się wysoką dokładnością i precyzją; wartość RSD nie przekracza 8% dla mleka i jaj, a dokładność określona jako procentowa różnica pomiędzy wielkością znalezioną, a dodaną do próbki, zmienia się od-2 do 5. Odzysk sulfonamidów wprowadzonych do mleka i jaj mieścił się w przedziale od 96 do 105%.