scholarly journals DEVELOPMENT OF HPLC–UV TECHNIQUES FOR QUANTITATIVE ANALYSIS OF 4-HYDROXYBENZOIC ACID ESTERS (PARABENS) IN FOODSTUFFS, COSMETICS AND PHARMACEUTICAL PRODUCTS

2019 ◽  
Vol 63 (1) ◽  
pp. 11-17
Author(s):  
Anton S. Lebedev ◽  
Vladimir Yu. Orlov ◽  
Anton S. Petrov
Keyword(s):  
Pharmaceutical Formulations ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Pharmaceutical Products ◽  
Hydroxybenzoic Acid ◽  
Chromatography Method ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Propyl Esters ◽  
Gradient Elution Mode

Four methods have been proposed for the determination of methyl-, ethyl- and propyl- esters of 4-hydroxybenzoic acid (parabens) in foodstuff, cosmetic products and pharmaceutical formulations by RF-HPLC. Electronic spectra parameters of parabens have been determined. It was found that in neutral solutions the absorption maximums were 195 and 254 nm for all analytes. Signal ratios have been calculated (S254/S230). Signal ratios were used as an additional criterion for identification. The conditions of chromatographic separation were common for all types of samples. A precolumn and an Acclaim (Thermo) column with a C-18 sorbent without any additional modifications (both structural and dynamic), a gradient elution mode with water-acetonitrile mixtures and a spectrophotometric method of detection at two wavelengths were used. The total time of chromatographic analysis was 45 min, including the stage of conditioning the system with a starting eluent (15 min). The retention times of parabens in the reversed-phase variant of separation increased with the increase in alkyl groups in the structure of molecules. The effectiveness of the removal of surfactants from cosmetics by the column chromatography method with silica gel as a polar sorbent and using ethylacetate (an ethylacetate extract of the sample) as an eluent has been shown. The necessity of applying gradient elution mode for reducing analysis time and increasing the amplitude of analytes signals was established. The calculated validation parameters (detection limit, limit of quantitation, limit of repeatability, recovery) show the compliance of the methods with the current regulatory documents (SanPiN 2.3.2.1293-03, SanPiN 2.3.2.2364-08).

scholarly journals Simultaneous Determination of Bifonazole and Tinctures of Calendula Flower in Pharmaceutical Creams by Reversed-Phase Liquid Chromatography

2005 ◽  
Vol 88 (6) ◽  
pp. 1649-1654 ◽  
Author(s):  
Carola F Ferreyra ◽  
Cristina S Ortiz
Keyword(s):  
Liquid Chromatography ◽  
Pharmaceutical Formulations ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Pharmaceutical Products ◽  
Stability Studies ◽  
Reversed Phase Liquid Chromatography ◽  
Compound I ◽  
Phase Liquid

Abstract The aim of this research was to develop and validate a sensitive, rapid, easy, and precise reversed-phase liquid chromatography (LC) method for stability studies of bifonazole (I) formulated with tinctures of calendula flower (II). The method was especially developed for the analysis and quantitative determination of I and II in pure and combined forms in cream pharmaceutical formulations without using gradient elution and at room temperature. The influence on the stability of compound I of temperature, artificial radiation, and drug II used for the new pharmaceutical design was evaluated. The LC separation was carried out using a Supelcosil LC-18 column (25 cm × 4.6 mm id, 5 μm particle size); the mobile phase was composed of methanol–0.1 M ammonium acetate buffer (85 + 15, v/v) pumped isocratically at a flow rate of 1 mL/min; and ultraviolet detection was at 254 nm. The analysis time was less than 10 min. Calibration graphs were found to be linear in the 0.125–0.375 mg/mL (rI = 0.9991) and 0.639–1.916 mg/mL (rII = 0.9995) ranges for I and II, respectively. The linearity, precision, recovery, and limits of detection and quantification were satisfactory for I and II. The results obtained suggested that the developed LC method is selective and specific for the analysis of I and II in pharmaceutical products, and that it can be applied to stability studies.

scholarly journals Determination of Ten Corticosteroids in Illegal Cosmetic Products by a Simple, Rapid, and High-Performance LC-MS/MS Method

2017 ◽  
Vol 2017 ◽  
pp. 1-12 ◽  
Author(s):  
Vita Giaccone ◽  
Giuseppe Polizzotto ◽  
Andrea Macaluso ◽  
Gaetano Cammilleri ◽  
Vincenzo Ferrantelli
Keyword(s):  
High Performance ◽  
Skin Diseases ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Cosmetic Products ◽  
Chromatography Method ◽  
Esi Ms ◽  
Negative Ionization Mode ◽  
Negative Ionization

The aim of our present work was the development of a rapid high-performance liquid chromatography method with electrospray ionization and tandem mass spectrometry detection (LC-ESI-MS/MS) for the determination of several corticosteroids in cosmetic products. Corticosteroids are suspected to be illegally added in cosmetic preparations in order to enhance the curative effect against some skin diseases. Sample preparation step consists in a single extraction with acetonitrile followed by centrifugation and filtration. The compounds were separated by reversed-phase chromatography with water and acetonitrile (both with 0.1% formic acid) gradient elution and detected by ESI-MS positive and negative ionization mode. The method was validated at the validation level of 0.1 mg kg−1. Linearity was studied in the 5–250 μg L−1 range and linear coefficients (r2) were all over 0.99. The accuracy and precision of the method were satisfactory. The LOD ranged from 0.085 to 0.109 mg kg−1 and the LOQ from 0.102 to 0.121 mg kg−1. Mean recoveries for all the analytes were within the range 91.9–99.2%. The developed method is sensitive and useful for detection, quantification, and confirmation of these corticosteroids in cosmetic preparations and can be applied in the analysis of the suspected samples under investigation.

Rapid and Sensitive Liquid Chromatographic Method for Determination of Anastrozole in Different Polymer–Lipid Hybrid Nanoparticles

2021 ◽  
pp. 247263032098230
Author(s):  
Dilshad Ahmad ◽  
Faisal A. Al Meshaiti ◽  
Yazeed K. Al Anazi ◽  
Osama Al Owassil ◽  
Alaa Eldeen B. Yassin
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Hplc Method ◽  
Hybrid Nanoparticles ◽  
Array Detector ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Inhibitor Drug

Anastrozole, an aromatase inhibitor drug, is used for the treatment of breast cancer in pre- and postmenopausal women. Anastrozole’s incorporation into nanoparticulate carriers would enhance its therapeutic performance. To perceive the exact loaded amount of drug in nanocarriers, a valid analytical method is required. The reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated by using the C18 column, 150 × 4.6 mm, 5 µm particle size, in isocratic mobile phase composed of 50:50 V/V (volume/volume) acetonitrile–phosphate buffer (pH 3) flowing at a rate of 1.0 mL/min, and a diode array detector (DAD) set at λmax = 215 nm. The validation parameters such as linearity, accuracy, specificity, precision, and robustness have proven the accuracy of the method, with the relative standard deviation percentage (% RSD) values < 2. The limit of detection of the method was found equal to 0.0150 µg/mL, and the limit of quantitation was 0.0607 µg/mL. The percent recovery of sample was in the range of 98.04–99.25%. The method has the advantage of being rapid with a drug retention time of 2.767 min, specific in terms of resolution of peaks void of interference with any of the excipients, and high reproducibility. This makes it highly applicable for quality control purposes.

scholarly journals Validation of a Reversed-Phase High Performance Liquid Chromatography Method for the Simultaneous Analysis of Cysteine and Reduced Glutathione in Mouse Organs

2016 ◽  
Vol 2016 ◽  
pp. 1-7 ◽  
Author(s):  
Serena Brundu ◽  
Lucia Nencioni ◽  
Ignacio Celestino ◽  
Paolo Coluccio ◽  
Anna Teresa Palamara ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Reduced Glutathione ◽  
Reversed Phase ◽  
Mouse Strains ◽  
Precolumn Derivatization ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Validation Parameters

A depletion of reduced glutathione (GSH) has been observed in pathological conditions and in aging. Measuring GSH in tissues using mouse models is an excellent way to assess GSH depletion and the potential therapeutic efficacy of drugs used to maintain and/or restore cellular redox potential. A high performance liquid chromatography (HPLC) method for the simultaneous determination of GSH and cysteine (Cys) in mouse organs was validated according to USA and European standards. The method was based on separation coupled with ultraviolet detection and precolumn derivatization with 5,5′-dithiobis-(2-nitrobenzoic acid) (DTNB). The required validation parameters, that are, selectivity, linearity, lower limit of quantification, precision, accuracy, recovery, and stability, were studied for spleen, lymph nodes, pancreas, and brain. The results showed that the lower limits of quantification were 0.313 μM and 1.25 μM for Cys and GSH, respectively. Intraday and interday precisions were less than 11% and 14%, respectively, for both compounds. The mean extraction recoveries of Cys and GSH from all organs were more than 93% and 86%, respectively. Moreover, the stability of both analytes during sample preparation and storage was demonstrated. The method was accurate, reliable, consistent, and reproducible and it was useful to determine Cys and GSH in the organs of different mouse strains.

Development and Validation of a Liquid Chromatography Method for the Simultaneous Determination of Eight Water-Soluble Vitamins in Multivitamin Formulations and Human Urine

2013 ◽  
Vol 96 (6) ◽  
pp. 1273-1280 ◽  
Author(s):  
Suyog S Patil ◽  
Ashwini K Srivastava
Keyword(s):  
Simultaneous Determination ◽  
Human Urine ◽  
Pharmaceutical Formulations ◽  
Gradient Elution ◽  
Water Soluble ◽  
Thiamine Hydrochloride ◽  
Chromatography Method ◽  
B Complex Vitamins ◽  
Liquid Chromatography Method

Abstract A simple, precise, and rapid RPLC method has been developed without incorporation of any ion-pair reagent for the simultaneous determination of vitamin C (C) and seven B-complex vitamins, viz, thiamine hydrochloride (B1), pyridoxine hydrochloride (B6), nicotinamide (B3), cyanocobalamine (B12), folic acid, riboflavin (B2), and 4-aminobenzoic acid (Bx). Separations were achieved within 12.0 min at 30°C by gradient elution on an RP C18 column using a mobile phase consisting of a mixture of 15 mM ammonium formate buffer and 0.1% triethylamine adjusted to pH 4.0 with formic acid and acetonitrile. Simultaneous UV detection was performed at 275 and 360 nm. The method was validated for system suitability, LOD, LOQ, linearity, precision, accuracy, specificity, and robustness in accordance with International Conference on Harmonization guidelines. The developed method was implemented successfully for determination of the aforementioned vitamins in pharmaceutical formulations containing an individual vitamin, in their multivitamin combinations, and in human urine samples. The calibration curves for all analytes showed good linearity, with coefficients of correlation higher than 0.9998. Accuracy, intraday repeatability (n = 6), and interday repeatability (n = 7) were found to be satisfactory.

Simultaneous determination of ciprofloxacin hydrochloride and hydrocortisone in ear drops by high performance liquid chromatography

2014 ◽  
Vol 68 (7) ◽  
Author(s):  
Joanna Ronowicz ◽  
Bogumiła Kupcewicz ◽  
Łukasz Pałkowski ◽  
Piotr Bilski ◽  
Tomasz Siódmiak ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Array Detector ◽  
Chromatography Method ◽  
Ciprofloxacin Hydrochloride ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Ear Drops

AbstractThe aim of the study was to design and validate a reversed phase high performance liquid chromatography method for the separation and quantification of two active pharmaceutical ingredients (ciprofloxacin hydrochloride, hydrocortisone) and a preservative (benzyl alcohol) in ear drops. Effective separation of the examined compounds was achieved on a GraceSmart™ RP 18 column (150 mm × 4.6 mm, 5 μm) with gradient elution and a diode array detector. The total assay run time was 25 min. Analytical method validation assays were performed. Validation parameters used for the evaluation were: specificity, linearity, trueness, precision (repeatability and reproducibility), limit of detection and limit of quantitation. Results of the validation procedure (high recoveries, good standard deviations, no interfering peaks at the retention times corresponding to the analytes) confirm that the developed chromatographic method can be applied for routine analysis of ear drops.

scholarly journals Combined Determination of Succinic Acid and Cetylpyridinium Chloride in Medicinal Films by Gradient High Performance Liquid Chromatography

Medicina ◽  
2021 ◽  
Vol 9 (2) ◽  
pp. 75-88
Author(s):  
O. N. Dvorskaya ◽  
◽  
N. N. Nozhkina ◽  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Succinic Acid ◽  
High Performance ◽  
Cetylpyridinium Chloride ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Gradient Elution Mode

A technique has been developed based on reversed-phase high-performance liquid chromatography with diode-matrix detection for the joint determination of succinic acid and cetylpyridinium chloride in complex action medicinal films. Efficient chromatographic separation of active drug components was achieved in a gradient elution mode on a Luna C18 (2) 100A column (4.6 × 250 mm, 5 µm) using a mobile phase consisting of a 0.1% solution of phosphoric acid and acetonitrile. The detection wavelength was 210 nm for both compounds. The developed method is validated in terms of specificity, linearity, precision, accuracy and can be used to determine the authenticity and quantitative content of succinic acid and cetylpyridinium chloride in the joint presence in assessing the quality of medicinal films.

scholarly journals Analisis Glimepirida Dalam Plasma Tikus

2006 ◽  
Vol 3 (1) ◽  
Author(s):  
Yahdiana Harahap ◽  
Umar Mansur ◽  
Theresia Sinandang
Keyword(s):  
High Performance ◽  
Internal Standard ◽  
Reversed Phase ◽  
Array Detector ◽  
Diode Array Detector ◽  
Chromatography Method ◽  
Mobile Phase Flow Rate ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Method ◽  
The Given

The aim of this research is to find the method for analyze glimepiride and itÂ’s metabolite. Glimepiride is the second generation of antidiabetic oral from the sulphonyl urea that works by stimulating the insulin secretion from beta cells of pancreas. Glimepiride is isolated from plasma the using chloroform. Using the high performance liquid chromatography method which include C18 reversed phase column, using mixture of methanol:water (50:50, v/v) as a mobile phase, flow rate 1.0 ml/minutes, detection at wavelenght 228 nm with photo diode array detector gives retention times of glimepiride in 17 minutes without any interference from endogen component of plasma and from itÂ’s metabolite. Linearity with added internal standard gliclazide was established for the range concentration 100-1000 ng/ml with coefficient of correlation (r) is 0.9977 and give the limit of quantitation of glimepiride in 50 ng/ml. The results of validation method fulfilled for the given criterias.

scholarly journals Forced degradation studies and stability-indicating liquid chromatography method for determination of tirofiban hydrochloride and synthetic impurities

2020 ◽  
Vol 49 (2) ◽  
Author(s):  
Adriane Lettnin Roll Feijó ◽  
Fernanda Macke Hellwig ◽  
Clésio Soldateli Paim ◽  
Marcelo Donadel Malesuik
Keyword(s):  
Liquid Chromatography ◽  
Degradation Products ◽  
Gradient Elution ◽  
Pharmaceutical Products ◽  
Raw Material ◽  
Forced Degradation ◽  
Chromatography Method ◽  
Stability Indicating ◽  
Liquid Chromatography Method

This study aimed to develop and validate a stability-indicating liquid chromatography method for the determination of tirofiban hydrochloride and two synthetic impurities (impurity A and impurity C). The method utilizes a RP-18 column (250 mm × 4.6 mm; 5 μm) with the PDA detector for quantitation. A mixture of triethylamine 0.1% (acidified to pH 5.5 with phosphoric acid) and acetonitrile was used as the mobile phase at a flow rate of 1 mL min−1 with gradient elution. The method presented satisfactory linearity, precision, accuracy and robustness, as well as low limits of detection and quantification, which demonstrate sensitivity in the determination of tirofiban and impurities A and C. It was selective for the determination of the drug and impurities analysed, without interference of the degradation products generated under forced conditions, demonstrating the stability-indicating capacity of the proposed method. Tirofiban showed to be practically stable to oxidative (30% H2O2 for 24 h) and thermal (75 ºC for 24 h) conditions, but presented degradation to UVA light and acid hydrolysis, obeying the first order kinetics for both. In this way, it can be used as a stability-indicating method in the quality control of the raw material of tirofiban hydrochloride, as well as of the finished product. The obtained results demonstrate the importance of deepening the studies in this area, in order to guarantee the quality of commercialized pharmaceutical products.

scholarly journals Simultaneous Liquid Chromatographic Determination of Ezetimibe and Simvastatin in Pharmaceutical Products

2007 ◽  
Vol 90 (6) ◽  
pp. 1566-1572 ◽  
Author(s):  
Paulo Renato Oliveira ◽  
Thiago Barth ◽  
Vitor Todeschini ◽  
Sérgio luiz Dalmora
Keyword(s):  
Chromatographic Determination ◽  
Reversed Phase ◽  
Pharmaceutical Products ◽  
Array Detector ◽  
Control Analysis ◽  
Pharmaceutical Dosage Forms ◽  
Photodiode Array Detector ◽  
Validation Parameters ◽  
Liquid Chromatographic

Abstract A reversed-phase liquid chromatographic (LC) method was developed and validated for the simultaneous determination of ezetimibe and simvastatin in pharmaceutical dosage forms. The LC method was carried out on a Synergi fusion C18 column (150 mm 4.6 mm id) maintained at 45C. The mobile phase consisted of phosphate buffer 0.03 M, pH 4.5acetonitrile (35 + 65, v/v) run at a flow rate of 0.6 mL/min, and detection was made using a photodiode array detector at 234 nm. The chromatographic separation was obtained within 15.0 min, and calibration graphs were linear in the concentration range of 0.5200 g/mL. Validation parameters such as specificity, linearity, precision, accuracy, and robustness were evaluated, giving results within the acceptable range for both compounds. Moreover, the proposed method was successfully applied for the routine quality control analysis of pharmaceutical products.

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