Ultrasound-assisted cloud point microextraction of certain preservatives in real samples and determination by HPLC.

Ultrasound-assisted cloud point microextraction (UA-CPME) was performed for certain preservatives (p-hydroxy benzoic acid and its alkyl esters, methyl, ethyl, propyl and butyl parabens). Then, an HPLC method was developed for their simultaneous determination in pharmaceutical and cosmetic samples. The chromatograms of these substances were recorded on a C18 column using a gradient elution technique with various solvent systems at different flow rates and at 254 nm wavelength using a diode-array detector (DAD). The analysis conditions found by the classical method were optimized using the Box-Behnken design (BBD). In the design, the effect of each factor was examined with 3 and 4 factors for UA-CPME and HPLC analyses, respectively. The brij 58 concentration (BC), Na2SO4 amount (SA) and extraction time (ET) for UA-CPME, and the mobile phase 1 (MP1) ratio, mobile phase 2 (MP2) ratio, flow rate (FR) and column temperature parameters for HPLC analysis were obtained for the investigated levels. The factors affecting the resolution were determined by applying regression analysis to the experimental results. The analysis of variance (ANOVA) test was applied to ensure result reliability. The ANOVA test was used to determine the reliability of the results. A model was created with the obtained data. The developed method was validated by examining linearity, reproducibility, accuracy, limit of quantification and limit of the detection. Methyl paraben (with 0.148% RSD value and 0.060% relative error), and propyl paraben (with 0.149% RSD value and 0.120% relative error) were determined in the syrup sample by the developed method. Methyl paraben with recovery values of (98.32-99.42)% and ethyl paraben with recovery values of (99.17-99.41)%, were determined in a hand cream.

A validated capillary electrophoretic method for the determination of indacaterol and its application to a pharmaceutical preparation.

Indacaterol is a new inhaled ultra-long acting ß2-agonist. It has been recently approved in the European Union for the treatment of chronic obstructive pulmonary disease. This paper reports, for the first time, a method for the determination and validation of Indacaterol (IND) using an internal standard in capsules. Capillary electrophoretic separation was performed on an uncoated fused-silica capillary (50 cm effective length, 75 µm i.d.) and background electrolyte composed of 20 mmol L-1 of sodium tetraborate buffer, 15% (v/v) methanol (pH = 10.0) with the application of 20 kV of potential; 10 s at 5 × 103 N m-2 (50 mbar) of injection time; and wavelength of 200 nm and 25 °C of temperature. The linearity was evaluated in the range of 4.90 × 10-6 mol L-1 (2.50 µg mL-1) and 3.94 × 10-5 mol L-1 (20.00 µg mL-1), with R = 0.9993 for inter-day. LOD and LOQ values were 2.18 × 10-8 mol L-1 (0.011 µg mL-1) and 7.25 × 10-8 mol L-1 (0.037 µg mL-1) for inter-day, respectively. The precision values were 0.50-1.06% for intra-day and 2.12% for inter-day as RSD%. The accuracy was tested by the standard addition method with the recovery values being between 98.79 and 99.09 as percentages with RSD% interval of 0.01-0.80. The developed method was validated according to ICH guidelines. Indacaterol was successfully determined in Arcapta® capsule dosage form by the validated CE method with a relative error of 0.28%. The result was within the requirements of the USP 34-NF29. Therefore, the validated method may be used for the determination of Indacaterol in its capsules in quality control laboratories.

A Validated Capillary Electrophoretic Method for the Determination of Olopatadine and Its Application to a Pharmaceutical Preparation of Eye Drops.

A validated rapid and sensitive capillary zone electrophoretic method for the determination of olopatadine hydrochloride (OLO) is described. Optimum conditions were found: 20 mmol/L sodium tetraborate buffer, acetonitrile 15% (v/v), 10 mmol/L NaCl at pH 9.5, with 25 kV of applied potential, injection time of 10 s at 5 × 103 N/m2, at a wavelength of 205 nm, and fixed temperature of 30°C. The calibration curve was linear in the range of 1.13 × 10-5 mol/L (4.22 µg/mL) to 5.65 × 10-5 mol/L (21.12 µg/mL), with R = 0.9995 for interday precision. LOD and LOQ values were 1.58 × 10-6 (0.58 µg/mL) and 4.78 × 10-6 mol/L (1.75 µg/mL), respectively. Precision values were 1.10-1.97% for intraday and 1.41% for interday RSDs. Accuracy was tested by preparing a synthetic mixture whose composition was similar to the pharmaceutical preparation for Patanol. The RSDs of the recovery values (98.2%) were between 0.42 and 0.65% and the amount of OLO found was 1.09 mg/mL. The result was within the requirements of USP 31-NF 26. Therefore, this validated method is suggested for routine analysis for the determination of OLO in laboratories.

A rapid determination of patulin using capillary zone electrophoresis and its application to analysis of apple juices.

This study describes a capillary zone electrophoretic method for the determination of patulin. An optimum run buffer was found to be 25 mM of sodium tetraborate and 10% acetonitrile (v/v) at pH 10. Optimum conditions were determined to be: an applied voltage of 25 kV (normal polarity), temperature of 25°C and injection time of 10 s at 50 mbar; the signals of patulin and phenobarbital as internal standard were detected at 276 nm. The method was highly reproducible, with relative standard deviations of 0.02-0.85 for intra-day and 0.04-0.42 for inter-day for standard patulin. Acceptable linearity [y = 0.0020C (µg/L) - 0.0680 (r = 0.9999)] was obtained over a concentration range of 0.25 to 4.99 µg/mL of patulin. The limits of detection and quantification were calculated to be 5.9 × 10(-3) and 1.79 × 10(-2) µg/mL, respectively. Recovery was 68.0%. The proposed method was applied to 21 apple juice samples purchased from different Turkish markets, and two were found to contain higher than the limits of the European Union Directive for patulin.

Separation of catechins and methylxanthines in tea samples by capillary electrochromatography.

In this paper, the simultaneous separation of several polyphenols such as (+)-catechin, (-)-epicatechin, (-)-epigallocatechin, theophylline, caffeine in green and black teas by capillary electrochromatography (CEC) was developed. Several experimental parameters such as stationary phase type, mobile phase composition, buffer and pH, inner diameter of the columns, sample injection, were evaluated to obtain the complete separation of the analysed compounds. Baseline resolution of the studied polyphenols was achieved within 30 min by using a capillary column (id 100 microm) packed with bidentate C(18) particles for 24.5 cm and a mobile phase composed of 5 mM ammonium acetate buffer pH 4 with H(2)O/ACN (80:20, v/v). The applied voltage and the temperature were set at 30 kV and 20 degrees C. Precision, detection and quantification limits, linearity, and accuracy were investigated. A good linearity (R(2) > 0.9992) was achieved over a concentration working range of 2-100 microg/mL for all the analytes. LOD and LOQ were 1 and 2 microg/mL, respectively, for all studied compounds. The CEC method was applied to the analysis of those polyphenols in green and black tea samples after an extraction procedure. Good recovery data from accuracy studies ranged between 90% and 112% for all analytes.

Time and temperature dependent microbiological and mycotoxin (ochratoxin-A) levels in boza.

This study describes the examination of microbiological tests and the determination of OTA in boza temperature and time dependently. Prior to the analysis, physicochemical properties of the boza samples such as moisture, total acidity as lactic acid, pH, protein amount and viscosity were investigated. The incidence of total aerobic bacteria (TAB), lactic acid bacteria (LAB), coliforms, E.coli, Salmonella, S. aureus, B. cereus, yeast and moulds were examined. E.coli, Salmonella, S. aureus and B. cereus were not found in all boza samples. Initially, Aspergillus fumigatus; Acremonium sp.; Geotrichum candidum and Geotrichum capitatum were identified in the samples. Certain extraction techniques such as direct injection, liquid-liquid and solid phase (SP) were tried for the OTA analysis. The most available way was found to be direct injection among them and the recovery was 70.56%+/-9.80 (13.89 RSD). OTA amounts were determined in all boza samples utilizing an isocratic HPLC analysis with an ODS column. OTA was detected in only one sample as 3.58 microg/kg and this amount is above the limits of European Commission Regulations. Time and temperature-dependent changes were investigated and insignificant variation was observed.