scholarly journals Determination of methylparaben from cosmetic products by ultra performance liquid chromatography

2009 ◽  
Vol 74 (6) ◽  
pp. 669-676 ◽  
Author(s):  
Manuela Mincea ◽  
Ioana Lupşa ◽  
Dan Cinghiţă ◽  
Ciprian Radovan ◽  
Ioan Talpos
Keyword(s):  
Liquid Chromatography ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Pharmaceutical Products ◽  
Cosmetic Products ◽  
Minimal Sample ◽  
Relative Standard ◽  
Good Determination ◽  
Optimized Conditions

A new method for the determination of methylparaben by ultra-performance liquid chromatography (UPLC) was developed. Methylparaben is often used as preservative, alone or in combination with other parabens, being added to cosmetic products, pharmaceutical products and foods to avoid microbial contamination. Due to its widespread use and potential risk to human health, assessing human exposure to this compound is of interest. A good determination and quantification of methylparaben was developed with a gradient elution using a mixture of methanol and water (60:40, v/v) within 1.455 min. Under optimized conditions, the linear working range extends over two orders of magnitude with relative standard deviations of intra- and inter-day precision below 2.3 %, and a detection limit of 0.02 ng ?L-1 for methylparaben. The proposed method was successfully applied to the assay of methylparaben in cosmetic products with minimal sample preparation.

scholarly journals Simultaneous Determination of Rutin, Luteolin, Quercetin, and Betulinic Acid in the Extract ofDisporopsis pernyi(Hua) Diels by UPLC

2015 ◽  
Vol 2015 ◽  
pp. 1-5 ◽  
Author(s):  
Yanqi Wang ◽  
Shuyi Li ◽  
Dandan Han ◽  
Kehan Meng ◽  
Miao Wang ◽  
...  
Keyword(s):  
Quality Control ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
Betulinic Acid ◽  
Mobile Phase ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Relative Standard ◽  
Quantitative Basis

Disporopsis pernyi(Hua) Diels, which belongs to genusDisporopsis, has been widely used for the treatment of abnormal sweating, chronic cough, and so forth. An ultra-performance liquid chromatography (UPLC) analysis was developed for the determination of rutin, luteolin, quercetin, and betulinic acid inDisporopsis pernyi(Hua) Diels roots. UPLC analysis was conducted by using a Shim-pack XR-ODS column with gradient elution with the mobile phase of acetonitrile and water containing 0.1% formic acid and with a flow rate of 0.2 mL/min, detected at 210, 254, and 280 nm. The method was precise, with relative standard deviation < 2.0%. The recoveries for the four components inDisporopsis pernyi(Hua) Diels were between 98.5 and 100.9%. The average contents of rutin, luteolin, quercetin, and betulinic acid in roots were 5.63, 2.51, 3.87, and 2.41 μg/g, respectively. The method was accurate and reproducible and it can provide a quantitative basis for quality control ofDisporopsis pernyi(Hua) Diels.

Simultaneous Determination of Methocarbamol and Paracetamol in the Presence of Three Related Substances by Ultra Performance Liquid Chromatography

2019 ◽  
Vol 15 (5) ◽  
pp. 505-510
Author(s):  
Yanjuan Zheng ◽  
Qiushi Peng ◽  
Rui Dong ◽  
Tingyu Chen ◽  
Yi Bao ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Pharmaceutical Preparations ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Related Substances ◽  
Bulk Powder ◽  
Highly Sensitive ◽  
Optimal Protocol ◽  
Acquity Uplc

Introduction: A rapid, and accurate Ultra Performance Liquid Chromatography (UPLC) method was developed to simultaneously analyze Methocarbamol, Paracetamol and the related substances Materials and Methods: Waters ACQUITY UPLC® BEH Phenyl C18 column was used in conjunction with UV detection at 225nm. Gradient elution with 0.05M, pH 6 phosphate buffer and acetonitrile flow at 0.3mL /min rate were used to separate the substances. The retention times for 4-Aminopheno, Paracetamol, Guaifenesin, Methocarbamol, and 4-Chloroacetanilide were 1.319 minute, 2.224 minute, 4.467 minute, 4.769 minute and 5.433 minute respectively. The concentration was linear in the range of 2-100 µg/ml for Methocarbamol, and 1-100 µg/mL for Paracetamol. The percentage recoveries were between 99.28±1.23% to 100.57±0.99% for Methocarbamol, and between 99.08±1.23% to 101.23±1.39% for Paracetamol. Results and Discussion: The validated optimal protocol is robust and accurate for simultaneous analysis of Methocarbamol, Paracetamol and the related substances, applicable for bulk powder as well as pharmaceutical formulation. Conclusion: In this paper, a highly sensitive, accurate, and precise UPLC method with UV-Vis detection was developed and validated for quality control of MET and PAR in bulk as well as in pharmaceutical preparations.

Validation of HPLC Method for Determination of Histamine in Human Immunoglobulin Formulations

2020 ◽  
Vol 103 (5) ◽  
pp. 1223-1229
Author(s):  
Michikazu Tanio ◽  
Toru Nakamura ◽  
Hideki Kusunoki ◽  
Kyohei Ideguchi ◽  
Kazuyuki Nakashima ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
High Performance ◽  
Gradient Elution ◽  
Hplc Method ◽  
Human Immunoglobulin ◽  
Histamine Dihydrochloride ◽  
Relative Standard

Abstract Background Histamine fixed-immunoglobulin formulations, which consisted of 0.15 µg of histamine dihydrochloride and 12 mg of human immunoglobulin in a vial, are used for anti-allergic treatments, and controlling the amounts of histamine in the formulations is essential to avoid histamine intoxication. Objective A high-performance liquid chromatography (HPLC) method for determination of histamine contents of the formulations was established and validated. Methods Histamine extracted from the formulation was labeled with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate and was analyzed by gradient elution HPLC with UV detection at 260 nm. Results The method showed linearity in the range 0.8–2.4 µM (R &gt; 0.999), accuracy (100.1–105.8% recovery), and precision (relative standard deviation ≤ 1.93%). The validated method was applied for five lots of the pharmaceutical, and their histamine contents were determined to be 0.149–0.155 µg/vial. Conclusions These results indicated that the validated method is useful to control amounts of histamine in biopharmaceutical products. Highlights The HPLC method was developed for quantitative determination of histamine content of the histamine fixed-immunoglobulin formulations.

Determination of Total Taurine in Pet Foods by Liquid Chromatography of the Dansyl Derivative: Collaborative Study

2000 ◽  
Vol 83 (4) ◽  
pp. 784-788 ◽  
Author(s):  
Kieran McCarthy ◽  
Claudia Hischenhuber ◽  
Neil Joyce ◽  
G Cherix ◽  
C Hischenhuber ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
Collaborative Study ◽  
Gradient Elution ◽  
Taurine Concentration ◽  
Dansyl Derivative ◽  
Relative Standard ◽  
Standard Deviations ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method for the determination of total taurine in pet foods was evaluated in a collaborative study. Ten laboratories assayed 6 blind duplicate pairs of wet and dry pet foods. The taurine in the 6 sample pairs ranged from low (170 mg/kg) to high (2250 mg/kg) concentrations as is. Collaborators also assayed a sample of known taurine concentration for familiarization purposes. Samples were hydrolyzed to release bound taurine, which was subsequently converted to the dansyl derivative and quantitated by gradient-elution LC with fluorescence detection. Repeatability relative standard deviations, RSDr, ranged from 3.2 to 10.0%; reproducibility relative standard deviations, RSDR, ranged from 6.1 to 16.1%. The method has been adopted Official First Action status by AOAC INTERNATIONAL.

scholarly journals Determination of sibutramine and phenolphthalein in weight­loss tea, coffee, and milk by ultra-­performance liquid chromatography mass spectrometry UPLC­-MS/MS

2019 ◽  
Vol 2 (4) ◽  
pp. 42-48
Author(s):  
Than Truong Van ◽  
Duy Nguyen Thanh ◽  
Kiet Ly Tuan ◽  
Vinh Hoang Ngoc ◽  
Hai Chu Van ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Formic Acid ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Distilled Water ◽  
Liquid Chromatography Mass Spectrometry ◽  
Ms Detection ◽  
Chromatography Mass Spectrometry

A rapid, simply and effective method using ultra&shy;performance liquid chromatography coupled to mass spectrometry (MS) detection was developed in order to determine sibutramine and phenolphthalein in weight&shy;loss tea, coffee, and milk. QuEChERS technique was used for cleaning&shy;up sample matrices. The extracts were separated on C18 LC columns using the gradient elution of 0.1% formic acid in distilled water and acetonitrile. The recoveries at the concentration of 50 &micro;g/kg were from 90.1 to 105.8% (with RSDR of 4.04 &shy; 4.24%), from 91.9 to 100.2% (with RSDR of 3.20 &shy; 4.71%), and from 86.5 to 100.5% (with RSDR of 5.17 &shy; 5.49%) for weight&shy;loss tea, coffee, and milk, respectively. Method quantitation limits were of 30 &micro;g/kg.

Identification, Isolation and Determination of Biomarkers for Quality Control of Bush Tea (Athrixia phyllicoides)

Planta Medica ◽  
2018 ◽  
Vol 84 (12/13) ◽  
pp. 902-912 ◽  
Author(s):  
Lefa Lerotholi ◽  
Sushil Chaudhary ◽  
Weiyang Chen ◽  
Clinton Veale ◽  
Sandra Combrinck ◽  
...  
Keyword(s):  
South Africa ◽  
Quality Control ◽  
Liquid Chromatography ◽  
Ultra Performance Liquid Chromatography ◽  
Mass Spectrometry Data ◽  
Resonance Spectroscopy ◽  
Analysis Model ◽  
Relative Standard ◽  
Marker Compounds

Abstract Athrixia phylicoides, known as “bush tea”, grows abundantly in South Africa. An infusion of the leaves is used as a beverage and to treat a multitude of health conditions. The aim of this study was to investigate the chemical variation within A. phylicoides and to identify characteristic compounds for quality control. Samples from 12 locations in South Africa were analysed using ultra-performance liquid chromatography. Hierarchical cluster analysis of the aligned ultra-performance liquid chromatography-time-of-flight mass spectrometry data indicated two groups on the resulting dendrogram, representing 48 samples. Five marker compounds, identified through visual inspection and the construction of a discriminant analysis model, were evident on the ultra-performance liquid chromatography-MS profiles. Four of these compounds were isolated and identified, three as hydroxy methoxyflavones and the fourth as a coumarate, using nuclear magnetic resonance spectroscopy. An ultra-performance liquid chromatography-photodiode array method was developed and validated for the determination of the marker compounds using the isolates as standards. The limits of detection for the four compounds ranged from 0.92 – 2.50 µg/mL. Their recoveries at three concentration levels (1.00, 10.0, and 100 µg/mL) were between 97.0 and 101%, while acceptable intra- and inter-day precision was obtained as reflected by percentage relative standard deviation values below 2.24%. The concentrations of all the marker compounds were found to be higher in samples corresponding to Group 1 of the dendrogram than in those from Group 2. This may be attributable to differences in altitude, climate, and some edaphic factors. Identification of these marker compounds will make a valuable contribution towards the quality control and sustainable commercialisation of bush tea.

Simultaneous determination of 8 fluoroquinolone antibiotics in sewage treatment plants by solid-phase extraction and liquid chromatography with fluorescence detection

2009 ◽  
Vol 59 (4) ◽  
pp. 805-813 ◽  
Author(s):  
L. Shi ◽  
X. F. Zhou ◽  
Y. L. Zhang ◽  
G. W. Gu
Keyword(s):  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
Fluorescence Detection ◽  
Solid Phase ◽  
Sewage Treatment ◽  
Gradient Elution ◽  
Ammonium Bromide ◽  
Sewage Treatment Plants ◽  
Relative Standard

Fluoroquinolones (FQs) are among the most important antibiotics used in human and veterinary medicines. A simple and effective analytical method based on reversed-phased liquid chromatography with fluorescence was developed and validated for the simultaneous determination of eight FQs in wastewater at trace level. Aqueous samples were extracted using AnpelTM MEP cartridges where they were subsequently eluted by formic acid in methanol. The aqueous extracts were analyzed by gradient elution Liquid Chromatography with Fluorescence Detection (LC–FLD), whose mobile phase was composed of acetonitrile and 10 mM tetrabutyl ammonium bromide (TBAB). The limits of detection (LOD) and the relative standard deviation (RSD) were as low as 0.11–1.06 μg/L and 2–5%, respectively. The presented method was successfully applied to quantify FQs in the influent and effluent of several typical Sewage Treatment Plants (STPs) in Shanghai. For the extraction of 100 mL influent and 500 mL effluent sewage water samples, recoveries obtained were between 79–109% and 80%–105%, respectively. 7 FQs were occurred and identified in the STPs with the concentrations varying from 7 ng/L to 1 μg/L. Norfloxacin, ciprofloxacin and lomefloxacin were the most frequently detected antibiotics occurring in the wastewaters. The analytical procedure developed may be used for more in-depth studies on the occurrences and the fate of these commonly used pharmaceuticals in the sewage treatment plants and in the aquatic environment.

Qualitative and Quantitative Analysis of Flavonoids in Humulus scandens (Lour.)Merr. by UPLC-TQD and HPLC

2013 ◽  
Vol 295-298 ◽  
pp. 354-359 ◽  
Author(s):  
Xiao Wei Wang ◽  
Zhen Hua Liu ◽  
Rui Xiang Yu ◽  
De Hua Guo ◽  
Si Ming Zhu ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
High Performance ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Hplc Method ◽  
Qualitative And Quantitative Analysis ◽  
Ultraviolet Detector ◽  
Relative Standard ◽  
Four Levels ◽  
Humulus Scandens

To qualify and quantify the flavonoids existing in Humulus scandens (Lour.)Merr., a Ultra performance liquid chromatography triple-quadrupole tandem mass spectrometer (UPLC-TQD) method was applied to preliminarily analyze the flavonoids exiting in Humulus. And a High performance liquid chromatography (HPLC) method was used to analyze the flavonoids existing in Humulus. Flavonoids in methanol extracts of Humulus were cleaned up by a C18 cartridge, separated by a PLASMA ODS column(5μm,250×4.6mm), with a gradient elution of methanol and 0.1% formic acid at a flow rate of 1 mL•min-1 . Analytes were detected with ultraviolet detector (UV) at 280nm. Flavonoids, including Epicatechin, Luteolin-7-O-Glucoside, Vitexin or Apigenin-7-glucoside, Morin hydrate or Quercetin dehydrate and Luteolin were found in Humulus according to the UPLC-TQD. Results of HPLC analysis showed the linear ranges of 11 flavonoids were 0.1mg•L-1-20mg•L-1 with the correlation coefficient (r) all above 0.9909. Limits of detection (signal/ noise=3) was 100Superscript text μg•L-1. The average recoveries of all the compounds spiked at four levels of 200μg•L-1, 500μg•L-1, 1 mg•L-1 and 1.5 mg•L-1 were in the ranges of 70.8%-112.1%, 74.6%-116.6%, 73.1%-110.6%, 73.7%-99.9%, with the corresponding relative standard deviation (RSD, n=6) of 2.5%-5.8%, 0.8%-4.3%, 0.8%-3.7%, 1.7%-3.8%, respectively. This method ,which was proved to be precise, sensitive and reliable, could be applied to analyze flavonoids in leaves.

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 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.

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