Determination of Selected Phthalates in Some Commercial Cosmetic Products by HPLC-UV

2020 ◽  
Vol 23 (10) ◽  
pp. 1010-1022
Author(s):  
Emrah Dural
Keyword(s):  
High Performance ◽  
Phthalate Esters ◽  
High Sensitivity ◽  
Hplc Method ◽  
Cosmetic Products ◽  
Limit Of Quantification ◽  
Nail Polish ◽  
Accuracy And Precision ◽  
Butyl Phthalate

Aim and scope: Due to the serious toxicological risks and their widespread use, quantitative determination of phthalates in cosmetic products have importance for public health. The aim of this study was to develop a validated simple, rapid and reliable high-performance liquid chromatography (HPLC) method for the determination of phthalates which are; dimethyl phthalate (DMP), diethyl phthalate (DEP), benzyl butyl phthalate (BBP), di-n-butyl phthalate (DBP), di(2- ethylhexyl) phthalate (DEHP), in cosmetic products and to investigate these phthalate (PHT) levels in 48 cosmetic products marketing in Sivas, Turkey. Materials and Methods: Separation was achieved by a reverse-phase ACE-5 C18 column (4.6 x 250 mm, 5.0 μm). As the mobile phase, 5 mM KH2PO4 and acetonitrile were used gradiently at 1.5 ml min-1. All PHT esters were detected at 230 nm and the run time was taking 21 minutes. Results: This method showed the high sensitivity value the limit of quantification (LOQ) values for which are below 0.64 μg mL-1 of all phthalates. Method linearity was ≥0.999 (r2). Accuracy and precision values of all phthalates were calculated between (-6.5) and 6.6 (RE%) and ≤6.2 (RSD%), respectively. Average recovery was between 94.8% and 99.6%. Forty-eight samples used for both babies and adults were successfully analyzed by the developed method. Results have shown that, DMP (340.7 μg mL-1 ±323.7), DEP (1852.1 μg mL-1 ± 2192.0), and DBP (691.3 μg mL-1 ± 1378.5) were used highly in nail polish, fragrance and cream products, respectively. Conclusion: Phthalate esters, which are mostly detected in the content of fragrance, cream and nail polish products and our research in general, are DEP (1852.1 μg mL-1 ± 2192.0), DBP (691.3 μg mL-1 ± 1378.5) and DMP (340.7 μg mL-1 ±323.7), respectively. Phthalates were found in the content of all 48 cosmetic products examined, and the most detected phthalates in general average were DEP (581.7 μg mL-1 + 1405.2) with a rate of 79.2%. The unexpectedly high phthalate content in the examined cosmetic products revealed a great risk of these products on human health. The developed method is a simple, sensitive, reliable and economical alternative for the determination of phthalates in the content of cosmetic products, it can be used to identify phthalate esters in different products after some modifications.

scholarly journals Development and Validation of a Rapid RP-HPLC Method for the Estimation of Esmolol Hydrochloride in Bulk and Pharmaceutical Dosage Forms

2010 ◽  
Vol 7 (3) ◽  
pp. 807-812 ◽  
Author(s):  
Vanita Somasekhar ◽  
D. Gowri Sankar
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Detector Response ◽  
Reverse Phase Hplc ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Development And Validation

A reverse phase HPLC method is described for the determination of esmolol hydrochloride in bulk and injections. Chromatography was carried on a C18column using a mixture of acetonitrile, 0.05 M sodium acetate buffer and glacial acetic acid (35:65:3 v/v/v) as the mobile phase at a flow rate of 1 mL/min with detection at 275 nm. The retention time of the drug was 4.76 min. The detector response was linear in the concentration of 1-50 μg/mL. The limit of detection and limit of quantification was 0.614 and 1.86 μg/mL respectively. The method was validated by determining its sensitivity, linearity, accuracy and precision. The proposed method is simple, economical, fast, accurate and precise and hence can be applied for routine quality control of esmolol hydrochloride in bulk and injections.

scholarly journals ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF ATOMOXETINE HYDROCHLORIDE USING RAPID HIGH-PERFORMANCE LIQUID CHROMATOGRAPHIC TECHNIQUE

2018 ◽  
Vol 11 (11) ◽  
pp. 118
Author(s):  
Zubaidur Rahman ◽  
Vijey Aanandhi M ◽  
Sumithra M
Keyword(s):  
High Performance ◽  
Method Development ◽  
High Sensitivity ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Chromatographic Technique ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Liquid Chromatographic

Objective: A simple, novel, sensitive, rapid high-performance liquid chromatographic (RP-HPLC) method has been developed and validated for quantitative determination of atomoxetine HCl (ATH) in bulk and formulations.Methods: The chromatographic development was carried out on RP-HPLC. The column used as Xterra RP 18 (250 mm × 4.6 mm, 5 μ particle size), with mobile phase consisting of methanol: water 80:20 V/V. The flow rate was 1.0 mL/min and the effluents were monitored at 270 nm.Results: The retention time was found to be 5.350 min. The method was validated as per International Conference on Harmonization Guideline with respect to linearity, accuracy, precision, and robustness. The calibration curve was found to be linear over a range of 2–10 μg/mL with a regression coefficient of 0.9999. The method has proved high sensitivity and specificity.Conclusion: The results of the study showed that the proposed RP-HPLC method was simple, rapid, precise and accurate which is useful for the routine determination of ATH in bulk drug and in its pharmaceutical dosage form.

Simultaneous Determination of Cholecalciferol and 25- Hydroxycholecalceferol in Lipid-based Self-nanoemulsifying formulations and Marketed Product Vi-de 3® by UHPLC-UV

2019 ◽  
Vol 16 (1) ◽  
pp. 100-109
Author(s):  
Ibrahim Aljuffali ◽  
Fahad Almarri ◽  
A. F. M. Motiur Rahman ◽  
Fars Kaed Alanazi ◽  
Musaed Alkholief ◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Column Temperature ◽  
Related Substances ◽  
Accuracy And Precision ◽  
Regulatory Guidelines ◽  
25 Hydroxycholecalciferol

Background: The purpose of the current study was to develop a selective, precise, fast economical and advanced reverse phase ultra-high-performance liquid chromatography (UHPLC UV) method and validate it for the simultaneous estimation of cholecalciferol and its analogue 25- hydroxycholecalciferol in lipid-based self-nano emulsifying formulation (SNEDDS). Methods: The chromatographic separation was simply performed on a Dionex® UHPLC systems (Ultimate 3000, Thermo scientific) by using HSS C18 (2.1x50 mm, 1.8 µm) analytical column. The elution was carried out isocratically with the mobile phase consisting of acetonitrile and methanol in the ratio of 50:50 %v/v with a flow rate of 0.4 ml/min, followed by the UV detection at 265 nm. The injection volume was 1µl and the column temperature was maintained at 45°C. FDA regulatory guidelines were used to develop and validate the method. Results: The current developed UHPLC-UV method was found to be rapid (run time 2 min), and selective with the high resolution of cholecalciferol and 25-hydroxycholecalciferol (RT=0.530 min & 1.360 min) from different lipid matrices. The method was highly sensitive (Limit of Detection and Lower Limit of Quantification were 0.13 ppm & 0.51ppm, and 0.15 ppm & 0.54 ppm, respectively). The linearity, accuracy and precision were determined as suitable over the concentration range of 0.5-50.0 ppm for both the analytes. Conclusion: The proposed UHPLC-UV method can be used for the determination of cholecalciferol and 25-hydroxycholecalciferol in SNEDDS and marketed Vi-De 3® as pure forms (intact) with no interference of excipients or drug-related substances.

scholarly journals Simultaneous Determination of Eight Synthetic Permitted and Five Commonly Encountered Nonpermitted Food Colors in Various Food Matrixes by High-Performance Liquid Chromatography

2010 ◽  
Vol 93 (5) ◽  
pp. 1503-1514 ◽  
Author(s):  
Sumita Dixit ◽  
Subhash K Khanna ◽  
Mukul Das
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
High Sensitivity ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Hplc Method ◽  
Food Category ◽  
Food Commodities ◽  
Food Colors

Abstract A simple and sensitive HPLC method has been developed for the simultaneous determination of eight permitted food colors and five commonly encountered nonpermitted colors in various food commodities, including sugar-, fat-, and starch-based food matrixes. The method uses a specific food category-based cleanup/treatment procedure before color extraction to avoid the interference of food matrixes, and to obtain the optimal color extraction. Analysis was performed on a reversed-phase C18 -Bondapak column with ammonium acetate and acetonitrile gradient elution as the mobile phase; a programmable max-specific visible detection was used to monitor colors to obtain the higher sensitivity and expanded scope needed for multicolor blends having diverse absorption maxima. All colors showed good linearity, with regression coefficients of 0.99740.9999. The LOD and LOQ values ranged from 0.01 to 0.12 mg/L, and from 0.04 to 0.83 mg/L or mg/kg, respectively. The intraday and interday precision tests produced good RSD values, and the recoveries from different food matrixes ranged from 82 to 104%. The method offers high sensitivity for analysis of a wide variety of food matrixes containing a broad scope of multicolor blends. Two nonpermitted colors, orange II and metanil yellow, were found. Also, a number of samples contained permitted colors at levels two-to seven-fold higher than those prescribed.

Serotonin and its N-Acetylated and Acidic Derivatives in Insect Brain as Determined by High-Performance Liquid Chromatography with Electrochemical Detection

1993 ◽  
Vol 28 (1) ◽  
pp. 16-24 ◽  
Author(s):  
R. Vieira ◽  
M. Aldegunde
Keyword(s):  
Analytical Method ◽  
High Performance ◽  
Amperometric Detection ◽  
High Sensitivity ◽  
Hplc Method ◽  
Insect Brain ◽  
Oxidative Deamination ◽  
Wide Range ◽  
Hydrodynamic Voltammetry

The determination of serotonin (5-HT), N-acetylserotonin (NAS) and 5-hydroxy-3-indoleacetic acid (5-HIAA) in single brains of two acridids (Paracinema tricolor and Oedipoda caerulescens) was accomplished using a HPLC method combined with amperometric detection. A hydrodynamic voltammetry approach was used to assess the identity of each peak by comparing the voltammograms of standards and those of samples. The analytical method gave satisfactory reproducibility and sensitivity, and detected levels of 5-HT, NAS and 5-HIAA as low as 29, 55 and 10 fmol, respectively. This high sensitivity together with the simplicity of sample processing make the present analytical method suitable for a wide range of studies concerning indoleamine analyses in the insect nervous system. In both acridids, 5-HT showed the largest quantities, while its derivatives occurred in extremely low amounts. The results suggest that N-acetylation of 5-HT is quantitatively preferred to oxidative deamination in both species (NAS levels were 4-fold those of 5-HIAA). The relative importance of each catabolic pathway is discussed as related to physiological and genetic aspects.

scholarly journals HPLC method validation and application for organic acid analysis in wine after solid-phase extraction

2016 ◽  
Vol 35 (2) ◽  
pp. 225 ◽  
Author(s):  
Violeta Ivanova-Petropulos ◽  
Krste Tašev ◽  
Marina Stefova
Keyword(s):  
Solid Phase Extraction ◽  
Organic Acids ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Hplc Method ◽  
Phase Extraction ◽  
Hplc Separation ◽  
Limit Of Quantification

<p>A solid-phase extraction method followed by reverse phase high-performance liquid chromatography (RP-HPLC) was optimized and validated for the quantitative determination of tartaric, malic, shikimic, lactic, citric and succinic acids in wine. Solid-phase extraction was carried out with C18 cartridges and extraction recoveries for all acids ranging from 98.3 to 103% were obtained. HPLC separation was performed with isocratic elution on a LiChrosorb RP-18 column (250 × 4.6 mm I.D., 5 µm) protected with the appropriate guard column. The mobile phase was a 5 mM solution of H<sub>3</sub>PO<sub>4</sub> with pH 2.1 at a flow rate of 1 ml/min. Detection of the organic acids was performed at 210 nm. The developed method was validated by checking its linearity, limit of detection (LOD), limit of quantification (LOQ), precision and recovery. The method was applied to the analysis of organic acids in Macedonian red and white wines.</p>

scholarly journals Validation method for determining sodium benzoate in fruit juice drinks in Malang

2019 ◽  
Vol 4 (1) ◽  
pp. 19
Author(s):  
Engrid Juni Astuti ◽  
Roha Fakhri Naufal Ilham ◽  
Januar Rahman
Keyword(s):  
Sodium Benzoate ◽  
Mobile Phase ◽  
High Performance ◽  
Glacial Acetic Acid ◽  
Fruit Juice ◽  
Hplc Method ◽  
Mobile Phase Composition ◽  
Validation Method ◽  
Accuracy And Precision

Sodium benzoate is a preservative that is permitted to be used in food and beverages. The maximum limit for using sodium benzoate in food is 600 mg/L of ingredients calculated as benzoic acid. In this study, High-Performance Liquid Chromatography (HPLC) method using a PDA detector was used for sodium benzoate levels analysis in fruit juice drink circulating in Malang. The mobile phase composition used in this study was methanol pro-HPLC:aqua pro injection (70:30) and added glacial acetic acid to reach pH 3. The analysis was conducted at a wavelength of 245 nm, and the flow rate was set at 1.00 mL/minute. This method was validated against the parameters of selectivity, linearity, accuracy, and precision, and the results obtained to meet the validation requirements. The application of the HPLC method after being validated in the determination of sodium benzoate levels in fruit juice drink circulating in Malang resulted in selectivity Rs ≥ 1.5, linearity obtained in the range 0.1-5 μg/mL with a correlation coefficient (r) = 0,9999, recovery at a concentration of 80%, 100%, and 120% was 105.31%, and precision with an RSD value of 1.40%. Based on the results, it can be concluded that the validation method of analysis shows that the method can be used to determine sodium benzoate level using HPLC with PDA detectors for routine use in fruit juice drink samples.

RAPID HIGH PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE DETERMINATION OF RALTEGRAVIR IN HUMAN SALIVA

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (09) ◽  
pp. 68-73
Author(s):  
K Vijaya Sri ◽  
M. Shiva Kumar ◽  
M. A. Madhuri ◽  
Suresha K. ◽  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Human Saliva ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Liquid Chromatography Method ◽  
Liquid Chromatographic

In this study, a high-performance liquid chromatographic method (HPLC) was developed, validated and applied for the determination of raltegravir in biological sample like saliva. Liquid- liquid extraction was performed for isolation of the drug and elimination of saliva interferences. Samples of saliva was extracted with 50µL of ortho phosphoric acid and 3ml of methanol was added and spiked with raltegravir. The chromatographic separation was performed on Agilent Eclipse C18 (100 mm × 4.6 mm, 3.5µm) column, by using 80:20 v/v acetonitrile: water as a mobile phase under isocratic conditions at a flow rate of 1.0 mL/min for UV detection at 240 nm. Retention time of raltegravir was found to be 1.030 min. Linearity was found to be in the range of 25-1000 ng/mL with regression equation y = 13864x + 40495 and correlation coefficient 0.999. The low % RSD value indicates the method is accurate and precise. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.76 and 2.28 ng/mL, respectively. It can be concluded that this validated HPLC method is easy, precise, accurate, sensitive and selective for determination of raltegravir in saliva.

scholarly journals Stability-Indicating Assay for the Determination of Pentobarbital Sodium in Liquid Formulations

2015 ◽  
Vol 2015 ◽  
pp. 1-6 ◽  
Author(s):  
Myriam Ajemni ◽  
Issa-Bella Balde ◽  
Sofiane Kabiche ◽  
Sandra Carret ◽  
Jean-Eudes Fontan ◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Drug Stability ◽  
Reversed Phase ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Reliable Determination ◽  
Pentobarbital Sodium ◽  
Stability Indicating

A stability-indicating assay by reversed-phase high performance liquid chromatography (RP-HPLC) method was developed for the determination of pentobarbital sodium in oral formulations: a drug used for infant sedation in computed tomography (CT) or magnetic resonance imaging (MRI) scan. The chromatographic separation was achieved on a reversed-phase C18 column, using isocratic elution and a detector set at 214 nm. The optimized mobile phase consisted of a 0.01 M potassium buffer pH 3 and methanol (40 : 60, v/v). The flow rate was 1.0 mL/min and the run time of analysis was 5 min. The linearity of the method was demonstrated in the range of 5 to 250 μg/mL pentobarbital sodium solution (r2= 0.999). The limit of detection and limit of quantification were 2.10 and 3.97 μg/mL, respectively. The intraday and interday precisions were less than 2.1%. Accuracy of the method ranged from 99.2 to 101.3%. Stability studies indicate that the drug is stable to sunlight and in aqueous solution. Accelerated pentobarbital sodium breakdown by strong alkaline, acidic, or oxidative stress produced noninterfering peaks. This method allows accurate and reliable determination of pentobarbital sodium for drug stability assay in pharmaceutical studies.

scholarly journals Chromatographic Methods for the Determination of Aminexil, Pyridoxine, and Niacinamide in a Novel Cosmetic Hair Preparation

2020 ◽  
Vol 103 (4) ◽  
pp. 1167-1172
Author(s):  
Mamdouh R Rezk ◽  
Hebatallah M Essam ◽  
Enas A Amer ◽  
Dina M S Youssif
Keyword(s):  
High Performance ◽  
High Sensitivity ◽  
Ammonia Solution ◽  
Hplc Method ◽  
The Novel ◽  
Chromatographic Methods ◽  
Ich Guidelines ◽  
Sensitivity And Selectivity ◽  
Keratin Fibers

Abstract Background Aminexil, a new compound patented by L’Oreal, has a stimulating effect on human keratin fibers. Pyridoxine HCl and niacinamide are added to boost the hair tonic effect of aminexil. Objective Two novel chromatographic methods were developed for the determination of aminexil (AX), niacinamide (NA) and pyridoxine HCl (PD) in the novel hair tonic preparation. Methods The developed methods were high-performance liquid chromatography (HPLC) and thin layer chromatography (TLC) with densitometric determination. Different experimental parameters were investigated and optimized to achieve complete baseline separation and well resolved peaks. The RP-HPLC separation was achieved using a Thermoscientific BDS hypersil C18 (250 × 4.6 mm, 5 µm) column using 0.005 M hexane sulfonic acid: methanol (80: 20, v/v) as a mobile phase. For the TLC method, the three analytes were partitioned between propanol: toluene: ammonia solution (40:60:2, v/v/v) and fluorescent silica plates. The two methods were validated in compliance with International Conference on Harmonization (ICH) guidelines. The obtained data were statistically analyzed to confirm the existing results. The developed methods were successfully applied for determination of the studied drugs in pure forms and in the cosmetic preparation. Results For the HPLC method, the RSDs of AX, NA and PD were 0.70, 0.88 and 1.17 respectively. For the TLC method, the RSDs of AX, NA and PD were 1.06, 1.37 and 0.73 respectively. Conclusions The proposed chromatographic methods showed high sensitivity and selectivity for the three compounds under analysis in the laboratory prepared mixture and in the hair tonic preparation. Highlights Aminexil, Pyridoxine, Niacinamide, HPLC. The present work offers two reproducible, accurate, validated, time and cost saving alternatives for the quantitative and qualitative determination of medicated hair preparation.

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