scholarly journals Determination of Frequently Used Parabens in Shampoo and Conditioners using Validated HPLC Assay Method

2021 ◽  
Vol 33 (7) ◽  
pp. 1651-1655
Author(s):  
S. Lavakumar ◽  
P.A. Vivekanand ◽  
A.A.M. Prince

Parabens are esters of p-hydroxy benzoic acid and widely used as preservatives with a broad spectrum of antimicrobial activity in cosmetic, foods and pharmaceutical products. Methyl, ethyl, propyl and butyl paraben are commonly used in many cosmetic products. The concentration level of these parabens was restricted to maximum 1%. Recently, many cosmetic products such as shampoo and hair conditioners are available in the Indian market with label claims "no-parabens in the products". A HPLC method is developed for determining four frequently used parabens namely, methyl, ethyl, propyl and butyl paraben in shampoo and hair conditioners. The chromatographic separation was carried out on Phenomenex Kromasil C18 column (150 mm × 4.6mm i.d, 5 μm particle size) with water: methanol (60:40 v/v) as mobile phase and UV detection was performed at 254 nm. The method was validated with respect to specificity, linearity, accuracy, precision and robustness. The calibration curve was achieved to be linear and regression coefficient obtained was > 0.9999 for all the parabens. Accuracy of chromatographic method was evaluated by standard addition method; paraben content was estimated in eleven commercial shampoos and four hair conditioners available in Indian market which were claimed as no parabens were evaluated to assess the quality of claims of these samples. The results indicated that all the tested shampoos and hair conditioners met the requirements of the standards.

2020 ◽  
Vol 23 (10) ◽  
pp. 1010-1022
Author(s):  
Emrah Dural

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.


Author(s):  
V.L.N. Balaji Gupta Tiruveedhi ◽  
Venkateswara Rao Battula ◽  
Kishore Babu Bonige ◽  
Tejeswarudu B.

This research work was designed to establish and validate a novel stability indicating RP-HPLC method for the combined determination of Benidipine hydrochloride (BHE) and Nebivolol hydrochloride (NHE) in bulk and tablets, dependent on ICH guidelines.The assay method to analyse BHE and NHE was optimized with isocratic elution using acetonitrile: 0.1M acetate buffer (45:55, pH 5.1), Lichrospher ODS RP-18 column and flow pace of 1 ml/min. Total time for single run was 14 min. The injection quantity was 20μl, and was detected at 249nm. The method was verified on a concentration series of 1.25-10μg/ml (NHE) and 1.0-10μg/ml (BHE) for precision, accuracy and linearity. The LOD values were 0.059µg/ml and 0.028µg/ml for NHE and BHE, respectively. The LOQ values were 0.196µg/ml for NHE and 0.094µg/ml for BHE. The recovery percentages were 98.60-100.11% (BHE) and 98.94-101.50% (NHE) with relative standard deviation 0.250-0.694% (BHE) and 0.183-0.400% (NHE). The method was also observed to be efficient, and was sufficiently specific to measure BHE and NHE in the presence of stress-produced degradation products.


1995 ◽  
Vol 41 (6) ◽  
pp. 897-903 ◽  
Author(s):  
A J Ji ◽  
S R Savon ◽  
D W Jacobsen

Abstract An estimated 500,000 individuals in the US, mostly steroid-dependent asthmatics, suffer severe adverse reactions to sulfites in foods, beverages, and pharmaceutical products. In an attempt to understand the pathogenesis of sulfite hypersensitivity, we have developed an assay for the determination of total serum sulfite by utilizing: (a) reductive release of serum protein-bound sulfite; (b) derivatization of free sulfite with monobromobimane; (c) separation of sulfite-bimane from thiol-bimanes by reversed-phase HPLC; and (d) quantitation of sulfite-bimane by fluorescence detection. The detection limit of this assay was 0.44 mumol/L serum sulfite. The intra- and interassay CVs for total serum sulfite at 5.4 mumol/L were 8.1% and 22.0%, respectively. The standard addition method was used to determine total serum sulfite in normal subjects. More than 70 samples were prepared in 2-3 h, followed by automated overnight analysis. The mean concentrations (+/- SD) of total serum sulfite in female (n = 41) and male (n = 35) donors were 4.63 +/- 2.33 and 5.16 +/- 2.68 mumol/L, respectively (not statistically significant: P = 0.368). The combined mean concentration of total sulfite in both sexes was 4.87 +/- 2.49 mumol/L. There was no correlation between total serum sulfite and total serum cysteine, cysteinylglycine, homocysteine, subject age, serum cobalamin, or serum folic acid. The reference range (mean +/- 2 SD) for total serum sulfite in normal subjects is 0-9.85 mumol/L.


2012 ◽  
Vol 9 (3) ◽  
pp. 1165-1174 ◽  
Author(s):  
L. Maheshwara Reddy ◽  
K. Janardhan Reddy ◽  
L. Bhaskar Reddy ◽  
P. Raveendra Reddy

A chromatographic method was established for the determination of lenalidomide and related substances in 10 mg and 5 mg capsules using Sunfire C-18(250×4.6 mm ID, 5 μm) HPCL column with 85:15 v/v ratio of mobile phases A (mixture of phosphoric acid buffer and 1-octane sulphonic acid sodium salt) and B(55: 45 v/v ratio of methanol and acetonitrile) at 40°C and 210 nm wave length. The degradation studies were performed using 0.1N HCl, 0.1 N NaOH, 1% v/v hydrogen peroxide, humidity, UV at 254 nm, Sun light, and heat to 60°C. No significant degradation of lenalidomide was observed. However, the slight degradation was observed in presence of NaOH. The developed HPLC method gave the peaks purity angle was less their threshold angle, indicating it to be suitable for stability studies. It was validated with respect to linearity, accuracy, precision, ruggedness, and robustness.


1974 ◽  
Vol 57 (4) ◽  
pp. 982-986
Author(s):  
John T Goras ◽  
Donald A Gonci ◽  
Kotaro Murai ◽  
James E Curley ◽  
Philip N Gordon

Abstract The assay method is applicable to samples containing 0.00110-0.0606% carbadox (methyl 3-(2-quinoxalinylmethylene)carbazate - N1, N4-dioxide) (10–550 g/ton). Carbadox is leached from the sample with chloroform-methanol (3+1), followed by a series of solvent-solvent extractions, column chromatography, and finally the spectrophotometric measurement of the carbadox content of the final solution at 420 nm. This treatment of the feed or feed supplement sample serves to isolate the carbadox from materials that might interfere in the spectrophotometric measurement. The method of standard addition compensates for a feed or feed supplement matrix effect in the assay. A water pretreatment step improves recovery of drug from pelleted feeds. Assay results for feeds and feed supplements that were prepared under carefully controlled conditions showed good agreement between the amounts of carbadox added and found. Multiple assay values for feeds containing 0.00551% carbadox exhibited a coefficient of variation of about 5%. Assay results for commercial feed and feed supplement samples indicated that the assay method is applicable to a wide variety of feeds and feed supplements.


Chemosensors ◽  
2020 ◽  
Vol 8 (4) ◽  
pp. 113
Author(s):  
Ancuta Dinu ◽  
Constantin Apetrei

This paper describes the sensitive properties of screen-printed carbon electrodes (SPCE) modified by using three different electroactive chemical compounds: Meldola’s Blue, Cobalt Phthalocyanine and Prussian Blue, respectively. It was demonstrated that the Prussian Blue (PB) modified SPCE presented electrochemical signals with the highest performances in terms of electrochemical process kinetics and sensitivity in all the solutions analyzed. PB-SPCE was demonstrated to detect Phe through the influence it exerts on the redox processes of PB. The PB-SPCE calibration have shown a linearity range of 0.33–14.5 µM, a detection limit (LOD) of 1.23 × 10−8 M and the standard deviation relative to 3%. The PB-SPCE sensor was used to determine Phe by means of calibration and standard addition techniques on pure samples, on simple pharmaceutical samples or on multicomponent pharmaceutical samples. Direct determination of the concentration of 4 × 10−6–5 × 10−5 M Phe in KCl solution showed that the analytical recovery falls in the range of 99.75–100.28%, and relative standard deviations in the range of 2.28–3.02%. The sensors were successfully applied to determine the Phe in pharmaceuticals. The validation of the method was performed by using the FTIR, and by comparing the results obtained by PB-SPCE in the analysis of three pharmaceutical products of different concentrations with those indicated by the producer.


Author(s):  
Ngoc Mai Pham Thi ◽  
Binh Le Thai ◽  
Dong Pham Huy ◽  
Tuyet Nhung Nguyen Thi ◽  
Duc Pham Tien ◽  
...  

Tea and tea products have been known and used for long and became a tradional culture in many countries in the world, including Vietnam. The quality of tea depends on the concentrations of typical active substances such as polyphenol groups and their active substances (EGCG, ECG, catechin,…). Therefore, study of analytical methods to determine these active substances is necessary to evaluate the quality of tea and tea products. In this study, UV-Vis method was selected to determine total polyphenol and HPLC method was selected to determine the main active ingredient of polyphenol group EGCG. The limit of detections are 0.12 mg/g and 0.064 mg/g for total polyphenol and EGCG, respectively. These methods were applied to determine the concentrations of total phenol and EGCG in 10 samples of tea and tea products. Results show that the concentrations of total phenol and EGCG vary significantly among samples, but there is a certain relationship between the concentration of total phenol and EGCG in each sample.


2009 ◽  
Vol 15 (2) ◽  
pp. 77-81 ◽  
Author(s):  
Kanakapura Basavaiah ◽  
Nagaraju Rajendraprasad ◽  
Basavaiah Vinay

Two simple, rapid, reliable and cost-effective methods based on titrimetry in non-aqueous medium are described for the determination of olanzapine in pharmaceuticals. In these methods, the drug dissolved in the glacial acetic acid was titrated with the acetous perchloric acid with visual and potentiometric end point detection, crystal violet being used as the indicator for visual titration. The methods are applicable over 1-15 mg range of olanzapine. The procedures were applied to determine olanzapine in pharmaceutical products and the results were found to be in a good agreement with those obtained by the reference method. Associated pharmaceutical materials did not interfere. The precision results, expressed by inter-day and intra-day relative standard deviation values, were satisfactory, higher than 2%. The accuracy was satisfactory as well. The methods proved to be suitable for the analysis of olanzapine in bulk drug and in tablets. The accuracy and reliability of the methods were further ascertained by recovery studies via a standard addition technique with percent recoveries in the range 97.51-103.7% with a standard deviation of less than 2%.


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