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.

scholarly journals Determination of Patulin in Apple Juice by Liquid Chromatography

2006 ◽  
Vol 89 (1) ◽  
pp. 139-143 ◽  
Author(s):  
Maria Helena Iha ◽  
Myrna Sabino
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Mobile Phase ◽  
Apple Juice ◽  
Array Detector ◽  
Diode Array ◽  
Diode Array Detector ◽  
Relative Standard ◽  
Precision Study

Abstract A method was developed and validated in-house for the determination of patulin (PAT), a toxic mold metabolite, in apple juice. The sample was extracted with ethyl acetatehexane and analyzed by liquid chromatography equipped with a C18 column and diode array detector. The mobile phase used for the quantification was waterethanol, at a flow rate of 0.5 mL/min. The method showed a mean recovery of 84.8%, the relative standard deviation obtained in the precision study was &lt;7.7%, the quantification and detection limits were 7 and 3 μg/L, respectively, and the linear range for PAT in apple juice was 2.6650 μg/L. The ruggedness was evaluated by an intralaboratory experiment, in which 5 factors were studied, and only one was found to influence the observed results. The developed method is fast, practical, and simple; the solvents (except hexane) and reagents used were nontoxic. The results of the validation confirmed the efficiency of the method, which is sensitive enough to be used in studies required to quantify PAT in apple juice.

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.

scholarly journals SEPARATION AND ANALYSIS OF AMLODIPINE/BENAZEPRIL COMBINATION IN CAPSULES BY A NOVEL ION PAIR LIQUID CHROMATOGRAPHY

2019 ◽  
Vol 11 (1) ◽  
pp. 107 ◽  
Author(s):  
Saleh Trefi ◽  
Yaser Bitar
Keyword(s):  
Quality Control ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
Degradation Products ◽  
Correlation Coefficients ◽  
Ion Pair ◽  
Chromatography Method ◽  
Relative Standard ◽  
Liquid Chromatography Method

Objective: The objective of this study was to develop and validate a novel ion-pair liquid chromatography method, in order to separate and assay of amlodipine/benazepril combination in capsules. This method was a fast, practical and additional choice in quality control laboratories.Methods: The chromatographic conditions comprised of a classical C18-type stationary phase (250 × 4.6 mm, 5μ), with a mobile phase consisting of: 45% of 10-3 M of cetrimide and 55% acetonitrile. The flow rate was 1 ml/min; the detection wavelength was at 242 nm, under ambient temperature.Results: The method was validated for linearity with correlation coefficients very close to one, the accuracy with mean recovery values between 95.0-105.0%, precision with relative standard deviations of the calculated concentrations less than 5.0% and specificity in the presence of degradation products and excipients.Conclusion: The results presented in this paper showed that the developed method was fast and applicable, for the separation and determination of amlodipine/benazepril combination in capsules.

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.

Medium-pressure liquid chromatography of platinum metal ions on Spheron DEAE

1983 ◽  
Vol 48 (8) ◽  
pp. 2255-2262 ◽  
Author(s):  
František Vláčil ◽  
Ivan Vinš ◽  
Oldřich Malíček
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Metal Ions ◽  
Mobile Phase ◽  
Platinum Metal ◽  
Hydrochloric Acid Concentration ◽  
Chloride Medium ◽  
Relative Standard ◽  
Medium Pressure Liquid Chromatography

Spheron DEAE (modified macroreticular hydroxyethylmethacrylate-ethylenedimethacrylate copolymer) was used for chromatographic separation and determination of Rh(III), Pd(II), and Pt(IV) in chloride medium. The most suitable composition of the mobile phase was looked for by studying the influence of hydrochloric acid concentration on the capacity ratios of the metal ions mentioned and on their resolution, as well as the influence of different additions to the mobile phase on the decrease of the high Pt(IV) retention. Using the photometric (UV) detection, the linear dependence was found up to following concentrations: Rh 200 mg l-1, Pd 2 g l-1, Pt 500 mg l-1. The detection limit was 23 ng Rh, 62 ng Pd and 96 ng Pt in 7 μl sample injected.The reproducibility of the determination was (as relative standard deviation for n = 3) 1-4%, relative error 0.7-7%.

scholarly journals SIMULTANEOUS DETERMINATION OF PARACETAMOL AND IBUPROFENE MIXTURES BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

2010 ◽  
Vol 3 (1) ◽  
pp. 9-13 ◽  
Author(s):  
Sophi Damayanti ◽  
Slamet Ibrahim ◽  
Kurnia Firman ◽  
Daryono H Tjahjono
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
Retention Time ◽  
Analytical Method ◽  
Phosphate Buffer ◽  
Mobile Phase ◽  
High Performance ◽  
Relative Standard

Analytical method for the determination of paracetamol and ibuprofene mixtures has been developed by High Performance Liquid Chromatography using C-18 column and acetinitrile - phosphate buffer pH = 4.5 (75:25) containing 0.075% sodium hexanesulfunate as a mobile phase. The detector was set at 215 nm. Using such conditions, retention time for paracetamol and ibuprofen was 4.89 and 7.11 min, respectively. The recovery for paracetamol and ibuprofen was found to be 101.07± 0.73% and 102.02 ± 1.58%, respectively. The detector limits of the method was 1.30 and 1.60 μg/mL with the relative standard deviation (RSD) 0.74 and 1.52% for paracetamol and ibuprofen, respectively.   Keywords: paracetamol, ibuprofen, multi-component, validation, HPLC.

Rapid Determination of Deoxynivalenol (Vomitoxin) by Liquid Chromatography Using Modified Romer Column Cleanup

1984 ◽  
Vol 67 (1) ◽  
pp. 52-54 ◽  
Author(s):  
Henry L Chang ◽  
Jonathan W Devries ◽  
Paul A Larson ◽  
Hasmukh H Patel
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Mobile Phase ◽  
Rapid Determination ◽  
Alumina Column ◽  
Relative Standard ◽  
Alumina Column Chromatography ◽  
Wheat Products ◽  
Liquid Chromatographic

Abstract A modification of the Romer method for determining deoxynivalenol (DON) provides rapid sample cleanup and includes liquid chromatographic (LC) quantitation. The method was evaluated using wheat, wheat flour, and other wheat products. The sample is extracted with acetonitrile–water (84 + 16), and an aliquot of the extract is subjected to activated charcoal–alumina column chromatography. The extract is then evaporated and diluted to volume with mobile phase, and DON is quantitated using liquid chromatography. The relative standard deviation based on duplicate samples is 6.07%. The detection limit is 30 ppb based on 2 x signal/noise ratio. Results by this method compared with the results obtained by the Scott GC method showed a correlation coefficient of 0.992 with a mean vomitoxin content of 779 ppb by this method and 716 ppb by the Scott method for 14 samples.

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.

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.

Determination of Nitrate in Water by HPLC

2013 ◽  
Vol 448-453 ◽  
pp. 406-408
Author(s):  
Jing Liu ◽  
Xiao Na Ji ◽  
Qing Kai Ren ◽  
Sheng Shu Ai ◽  
Li Jun Wan ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Recovery Rate ◽  
High Performance ◽  
Separation Efficiency ◽  
Fast Analysis ◽  
Relative Standard

We established a method fordetermination of nitrate in water by High Performance Liquid Chromatography(HPLC). The sample was analysed by HPLC-ADA and was quantitated by externalstandard method after being simply processed. This methd has the advantages ofhigh separation efficiency and fast analysis. The experiment result showed thatthe linearly dependent coefficient was0.994, the recovery rate was between 98.7%～105.7%,the relative standard deviation（RSD）wasless than 2.1 %, and the lowest detectable limit is 0.01ng (S/N=1.6).

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