The present study is aimed to study the host-guest inclusion complexation of the naturally occurring cyclodextrins (CDs), namely; (α-CD,β-CD, and γ-CD) with mitiglinide (MIT).
Capillary electrophoresis coupled with a capacitively coupled contactless conductivity detector (CE-C(4)D) has been employed for the determination of the β-blocker drugs (atenolol and amiloride) in pharmaceutical formulations. 150 mM acetic acid was used as background electrolyte. The influence of several factors (detector excitation voltage and frequency, buffer concentration, applied voltage, capillary temperature, and injection time) was studied. Non-UV absorbing L-valine was used as an internal standard; the analytes were all separated in less than 7 min. The separation was carried out in normal polarity mode at 28 °C, 25 kV, and using hydrodynamic injection (25 s). The separation was effected in a bare fused-silica capillary 75 μm × 52 cm. The CE-C(4)D method was validated with respect to linearity, limit of detection and quantification, accuracy, precision, and selectivity. Calibration curves were linear over the range 5-250 μg mL(-1) for the studied analytes. The relative standard deviations of intra- and inter-day precisions of migration times and corrected peak areas were less than 6.0%. The method showed good precision and accuracy and was successfully applied to the simultaneous determination of the β-blocker drugs in different pharmaceutical tablets.
Binding constants for the enantiomers of modafinil with the negatively charged chiral selector sulfated-β-CD (S-β-CD) using CE technique is presented. The calculations of the binding constants employing three different linearization plots (double reciprocal, X-reciprocal and Y-reciprocal) were performed from the electrophoretic mobility values of modafinil enantiomers at different concentrations of S-β-CD in the BGE. The highest inclusion affinity of the modafinil enantiomers were observed for the S-enantiomer-S-β-CD complex, in agreement with the computational calculations performed previously. Binding constants for each enantiomer-S-β-CD complex at different temperatures, as well as thermodynamic parameters for binding, were calculated. Host-guest binding constants using the double reciprocal fit showed better linearity (r(2)>0.99) at all temperatures studied (15-30°C) and compared with the other two fit methods. The linear van't Hoff (15-30°C) plot obtained indicated that the thermodynamic parameters of complexation were temperature dependent for the enantiomers.
A capillary electrophoretic method for the separation of the enantiomers of both ofloxacin and ornidazole is described. Several parameters affecting the separation were studied, including the type and concentration of chiral selector, buffer pH, voltage and temperature. Good chiral separation of the racemic mixtures was achieved in less than 16 min with resolution factors Rs=5.45 and 6.28 for ofloxacin and ornidazole enantiomers, respectively. Separation was conducted using a bare fused-silica capillary and a background electrolyte (BGE) of 50 mM H(3)PO(4)-1 M tris solution; pH 1.85; containing 30 mg mL(-1) of sulfated-beta-cyclodextrin (S-beta-CD). The separation was carried out in reversed polarity mode at 25 degrees C, 18 kV, detection wavelength at 230 nm and using hydrodynamic injection for 15 s. Acceptable validation criteria for selectivity, linearity, precision, and accuracy were studied. The limits of detection (LOD) and limits of quantitation (LOQ) of the enantiomers (ofloxacin enantiomer 1 (OF-E1), ofloxacin enantiomer 2 (OF-E2), ornidazole enantiomer 1 (OR-E1) and ornidazole enantiomer 2 (OR-E2)) were (0.52, 0.46, 0.54, 0.89) and (1.59, 1.40, 3.07, 2.70) microg mL(-1), respectively. The proposed method was successfully applied to the assay of enantiomers of both ofloxacin and ornidazole in pharmaceutical formulations. The computational calculations for the enantiomeric inclusion complexes rationalized the reasons for the different migration times between the ofloxacin and ornidazole enantiomers.
A three-phase hollow fiber liquid-phase microextraction (HF-LPME) coupled either with capillary electrophoresis (CE) or high performance liquid chromatography (HPLC) with UV detection methods was successfully developed for the determination of trace levels of the anti-diabetic drug, rosiglitazone (ROSI) in biological fluids. The analyte was extracted into dihexyl ether that was immobilized in the wall pores of a porous hollow fiber from 10 mL of aqueous sample, pH 9.5 (donor phase), and was back extracted into the acceptor phase that contained 0.1M HCl located in the lumen of the hollow fiber. Parameters affecting the extraction process such as type of extraction solvent, HCl concentration, donor phase pH, extraction time, stirring speed, and salt addition were studied and optimized. Under the optimized conditions (extraction solvent, dihexyl ether; donor phase pH, 9.5; acceptor phase, 0.1M HCl; stirring speed, 600 rpm; extraction time, 30 min; without addition of salt), enrichment factor of 280 was obtained. Good linearity and correlation coefficients of the analyte was obtained over the concentration ranges of 1.0-500 and 5.0-500 ng mL(-1) for the HPLC (r(2)=0.9988) and CE (r(2)=0.9967) methods, respectively. The limits of detection (LOD) and limits of quantitation (LOQ) for the HPLC and CE methods were (0.18, 2.83) and (0.56, 5.00) ng mL(-1), respectively. The percent relative standard deviation (n=6) for the extraction and determination of three concentration levels (10, 250, 500 ng mL(-1)) of ROSI using the HPLC and CE methods were less than 10.9% and 13.2%, respectively. The developed methods are simple, rapid, sensitive and are suitable for the determination of trace amounts of ROSI in biological fluids.
Capillary zone electrophoresis coupled with a capacitively coupled contactless conductivity detector (CE-C(4)D) has been employed for the determination of atenolol and amiloride in pharmaceutical formulations. Acetic acid (150 mm) was used as background electrolyte. The influence of several factors (detector excitation voltage and frequency, buffer concentration, applied voltage, capillary temperature and injection time) was studied. Non-UV-absorbing L-valine was used as internal standard; the analytes were all separated in less than 7 min. The separation was carried out in normal polarity mode at 28 degrees C, 25 kV and using hydrodynamic injection (25 s). The separation was effected in an uncoated fused-silica capillary (75 microm, i.d. x 52 cm). The CE-C(4)D method was validated with respect to linearity, limit of detection and quantification, accuracy, precision and selectivity. Calibration curves were linear over the range 5-250 microg/mL for the studied analytes. The relative standard deviations of intra- and inter-day migration times and corrected peak areas were less than 6.0%. The method showed good precision and accuracy and was successfully applied to the simultaneous determination of atenolol and amiloride in different pharmaceutical tablet formulations.
Capillary zone electrophoresis methods for the simultaneous determination of the beta-blocker drugs, atenolol, chlorthalidone and amiloride, in pharmaceutical formulations have been developed. The influences of several factors (buffer pH, concentration, applied voltage, capillary temperature and injection time) were studied. Using phenobarbital as internal standard, the analytes were all separated in less than 4 min. The separation was carried out in normal polarity mode at 25 degrees C, 25 kV and using hydrodynamic injection (10 s). The separation was effected in an uncoated fused-silica capillary (75 mum i.d. x 52 cm) and a background electrolyte of 25 mm H(3)PO(4) adjusted with 1 m NaOH solution (pH 9.0) and detection at 198 nm. The method was validated with respect to linearity, limit of detection and quantification, accuracy, precision and selectivity. Calibration curves were linear over the range 1-250 microg/mL for atenolol and chlorthalidone and from 2.5-250 microg/mL for amiloride. The relative standard deviations of intra- and inter-day migration times and corrected peak areas were less than 6.0%. The method showed good precision and accuracy and was successfully applied to the simultaneous determination of atenolol, chlorthalidone and amiloride in various pharmaceutical tablets formulations.
Purpose: To determine and quantify vinblastine in different varieties of Catharanthus roseus using reversed-phase HPLC method. Methods: The liquid chromatographic separation was performed using a reversed phase C18, Microsorb - MV column (250 mm x 4.6 mm, 5 µm) at room temperature and eluted with a mobile phase containing methanol - phosphate buffer (5 mM, pH 6.0) - acetonitrile with different proportion gradient elution at a flow rate of 2.0 mL min-1 and detection at 254 nm. Results: The HPLC method was utilized for the quantification of vinblastine in purple, red and white varieties of Catharanthus roseus leaves. The separation was achieved in less than 8 min. The peak confirmation was done based on the retention times and UV spectra of the reference substance. The method was validated with respect to linearity, precision, recovery, limit of detection and quantification. Results showed that the purple variety gives 1.2 and 1.5 times more vinblastine concentration compared to the white and pink varieties, respectively. Conclusion: The obtained results from different varieties are thus useful for the purpose of vinblastine production from Catharanthus roseus plant.
The aim of the current study was to develop a simple, precise, and accurate capillary zone electrophoresis method for the determination of zolpidem tartrate in tablet dosage form. Separation was conducted in normal polarity mode at 25°C, 22 kV, using hydrodynamic injection for 10 s. Separation was achieved using a background electrolyte of 20 mM disodium hydrogen phosphate adjusted with phosphoric acid (85%), pH at 5.50, and detection at 254 nm. Using the above optimized conditions, complete determination took place in less than 3 min using amiloride HCl as the internal standard. The method was linear over the range of 3-1000 μg mL(-1) with a correlation coefficient of 0.9999. Forced degradation studies were conducted by introducing a sample of zolpidem tartrate standard and pharmaceutical sample solutions to different forced degradation conditions, being neutral (water), basic (0.1 M NaOH), acidic (0.1 M HCl), oxidative (10% H2O2), temperature (60°C in oven for 3 days), and photolytic (exposure to UV light at 254 nm for 2 h). Degradation products resulting from the stress studies did not interfere with the detection of zolpidem tartrate and the assay can be considered stability-indicating.
A simple micellar electrokinetic chromatography (MEKC) method for the simultaneous determination of 2-furfural (2-F), 3-furfural (3-F), 5-methylfurfural (5-MF), 5-hydroxymethylfurfural (5-HMF), 2-furoic acid (2-FA) and 3-furoic acid (3-FA) in honey and vegetable oils is described. Parameters affecting the separation such as pH, buffer and surfactant concentrations, applied voltage, capillary temperature, injection time and capillary length were studied and optimized. The separation was carried out in normal polarity mode at 20 °C, 22 kV and using hydrodynamic injection (17 s). The separation was achieved in a bare fused-silica capillary (46 cm × 50 μm i.d.) with a background electrolyte of 75 mM phosphoric acid (pH 7.3), containing 200 mM of sodium dodecyl sulphate (SDS). The detection wavelengths were at 200 nm (2-FA and 3-FA) and 280 nm (2-F, 3-F, 5-MF, 5-HMF). The furfurals were well separated in less than 20 min. The method was validated in terms of linearity, limit of detection and quantitation, precision and recoveries. Calibration curves of the six furfurals were well correlated (r(2)>0.991) within the range 1-25 μg mL(-1). Relative standard deviations of intra- and inter-day migration times and corrected peak areas ≤9.96% were achieved. The limit of detection (signal:noise, 3) was 0.33-0.70 μg mL(-1) whereas the limit of quantitation (signal:noise, 10) was 1.00-2.12 μg mL(-1). The method was applied to the determination of furanic compounds in honeys and vegetable oils (palm, walnut, grape seed and rapeseed). The effects of thermal treatment and gamma irradiation on the formation of the furanic compounds in honey were also investigated.
A micellar electrokinetic chromatography method for the determination of sumatriptan succinate in pharmaceutical formulations was developed. The effects of several factors such as pH, surfactant and buffer concentration, applied voltage, capillary temperature, and injection time were investigated. Separation took about 5 min using phenobarbital as internal standard. The separation was carried out in reversed polarity mode at 20 °C, 26 kV and using hydrodynamic injection for 10s. Separation was achieved using a bare fused-silica capillary 50 μm×40 cm and background electrolyte of 25 mM sodium dihydrogen phosphate-adjusted with concentrated phosphoric acid to pH 2.2, containing 125 mM sodium dodecyl sulfate and detection was at 226 nm. The method was validated with respect to linearity, limits of detection and quantification, accuracy, precision and selectivity. The calibration curve was linear over the range of 100-2000 μg mL(-1). The relative standard deviations of intra-day and inter-day precision for migration time, peak area, corrected peak area, ratio of corrected peak area and ratio of peak area were less than 0.68, 3.48, 3.28, 2.97 and 2.83% and 2.01, 5.50, 4.46, 4.92 and 4.07%, respectively. The proposed method was successfully applied to the determinations of the analyte in tablet. Forced degradation studies were conducted by introducing a sample of sumatriptan succinate standard solution to different forced degradation conditions using neutral (water), basic (0.1 M NaOH), acidic (0.1 M HCl), oxidative (10% H(2)O(2)) and photolytic (exposure to UV light at 254 nm for 2 h). It is concluded that the stability-indicating method for sumatriptan succinate can be used for the analysis of the drug in various samples.
A micellar electrokinetic chromatography (MEKC) method for the simultaneous determination of the antiviral drugs acyclovir and valacyclovir and their major impurity, guanine, was developed. The influences of several factors (surfactant and buffer concentration, pH, applied voltage, capillary temperature and injection time) were studied. Using tyramine hydrochloride as internal standard, the analytes were all separated in about 4 min. The separation was carried out in reversed polarity mode at 28 degrees C, 25 kV and using hydrodynamic injection (15 s). The separation was effected in a fused-silica capillary 100 microm x 56 cm and a background electrolyte of 20 mM citric acid-1 M Tris solution (pH 2.75), containing 125 mM sodium dodecyl sulphate and detection at 254 nm. The method was validated with respect to linearity, limit of detection and quantification, accuracy, precision and selectivity. Calibration curves were linear over the range 0.1-1 microg/mL (guanine) and from 0.1 to 120 microg/mL for both valacyclovir and acyclovir. The relative standard deviations of intra- and inter-day migration times and corrected peak areas were less than 5.0%. The proposed method was successfully applied to the determination of the analytes in tablets and creams. From the previous study it is concluded that the stability-indicating method developed for acyclovir and valacyclovir can be used for analysis of the drug in various stability samples.
The current work reports an extended theoretical study from our previous experimental work for the enantioselective extraction of amlodipine enantiomers in a biphasic recognition chiral extraction system (BRCES) consisting of hydrophobic D-diisopropyl tartrate dissolved in organic phase (n-decanol) and hydrophilic hydroxypropyl-β-cyclodextrin (HP-β-CD) in aqueous phase (acetate buffer) which preferentially recognize the R-enantiomer and S-enantiomer, respectively. The calculations were simulated using a semi-empirical PM3 method as a part of the Gaussian09 software package and were used to optimize the structures of the hosts, guests, and host-guest complexes in the gas phase without any restrictions. It was found that HP-β-CD has the strongest recognition ability among the three β-CD derivatives studied, namely HP-β-CD, hydroxyethyl-β-cyclodextrin (HE-β-CD), and methylated-β-cyclodextrin (Me-β-CD), due to the large interaction energies (Ecomp = -14.3025 kcal/ mol), while D-diisopropyl tartrate has the strongest ability among the four tartaric acid derivatives studied namely; L-diisopropyl tartrate, D-diisopropyl tartrate, L-diethyl tartrate, and D-diethyl tartrate (Ecomp = -5.9964 kcal/ mol). The computational calculations for the enantioselective partitioning of amlodipine enantiomers rationalized the reasons for the different behaviors for this extraction. The present theoretical results may be informative to scientists who are devoting themselves to developing models for their experimental parts or for enhancing the hydrophobic drug solubility in drug delivery systems.
Blend copolymers (PVA/S) were grafted with polyethylene glycol methyl methacrylate (PEGMA) with different ratios. Potassium persulfate was used as an initiator. The blend copolymer (PVA/S) was created by combining poly(vinyl alcohol) (PVA) with starch (S) in various ratios. The main idea was to study the effect of different ratios of the used raw materials on the biodegradability of plastic films. The resulting polymers (PVA/S/PEGMA) were analyzed using FTIR spectroscopy to investigate the hydrogen bond interaction between PVA, S, and PEGMA in the mixtures. TGA and SEM analyses were used to characterize the polymers (PVA/S/AA). The biodegradability and mechanical properties of the PVA/S/PEGMA blend films were evaluated. The findings revealed that the mechanical properties of the blend films are highly influenced by PEGMA. The time of degradation of the films immersed in soil and Coca-Cola increases as the contents of PVA and S and the molecular weight (MW) of PEGMA increase in the terpolymer. The M8 sample (PVA/S/PEGMA in the ratio of 3:1:2, respectively) with a MW of 950 g/mol produced the lowest elongation at break (67.5%), whereas M1 (PVA/S/PEGMA in the ratio of 1:1:1, respectively) with a MW of 300 g/mol produced the most (150%). The film's tensile strength and elongation at break were improved by grafting PEGMA onto the blending polymer (PAV-b-S). Tg and Tm increased when the PEGMA MW increased from 300 to 950. Tg (48.4 °C) and Tm (190.9 °C) were the lowest in M1 (300), while Tg (84.8 °C) and Tm (190.9 °C) were greatest in M1 (950) at 209.3 °C. The increased chain and molecular weight of PEGMA account for the increase in Tg and Tm of the copolymers.