scholarly journals Determination of Parthenolide in Selected Feverfew Products by Liquid Chromatography

2000 ◽  
Vol 83 (4) ◽  
pp. 789-792 ◽  
Author(s):  
Ehab A Abourashed ◽  
Ikhlas A Khan
Keyword(s):  
United States ◽  
Quality Control ◽  
Mobile Phase ◽  
Chromatographic Method ◽  
The United States ◽  
Linear Gradient ◽  
Tanacetum Parthenium ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Abstract The migraine prophylactic herb feverfew (Tanacetum parthenium L.) is marketed in the United States in a variety of forms and compositions. Although its therapeutic efficacy is still uncertain, the sesquiterpene lactone parthenolide is the constituent recommended to be measured for quality control of feverfew preparations. A validated liquid chromatographic method was developed and used to estimate parthenolide in a number of U.S. feverfew market products formulated as capsules, tablets, or crude powder. The method uses a Lichrosphere 5 C18 column, a mobile phase consisting of 50mM NaH2PO4 in H2O (solvent A), and CH3CN–MeOH (90 + 10, v/v; solvent B). Elution was run at a flow rate of 1.0 mL/min with a linear gradient of 50–15% A in B over 20 min and UV detection at 210 nm. The correlation coefficient for the calibration curve was 0.9999 over the range of 0.00–0.400 mg/mL. Overall recovery of parthenolide was 103.1%.

A Versatile Stability-indicating Liquid Chromatographic Method for the Simultaneous Determination of Atenolol, Hydrochlorothiazide and Chlorthalidone

2020 ◽  
Vol 16 (8) ◽  
pp. 1037-1051
Author(s):  
Ehab Farouk Elkady ◽  
Marwa Ahmed Fouad ◽  
Abdulgabar A. Ezzy Faquih
Keyword(s):  
Quality Control ◽  
Chromatographic Method ◽  
Degradation Products ◽  
Pharmaceutical Dosage Forms ◽  
Potassium Dihydrogen ◽  
Ich Guidelines ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic ◽  
Potassium Dihydrogen Orthophosphate

Background: Atenolol is a selective beta 1 blocker that can be used alone or in combination with hydrochlorothiazide or with chlorthalidone for the treatment of hypertension and prevention from a heart attack. Objective: The main target of this work was to improve modern, easy, accurate and selective liquid chromatographic method (RP-HPLC) for the determination of these drugs in the presence of their degradation products. These methods can be used as analytical gadgets in quality control laboratories for a routine examination. Methods: In this method, the separation was accomplished through an Inertsil® ODS-3V C18 column (250 mm x 4.6 mm, 5 μm), the mobile phase used was 25 mM aqueous potassium dihydrogen orthophosphate solution adjusted to pH 6.8 by using 0.1M sodium hydroxide and acetonitrile (77 : 23, v/v), the flow rate used was 1 ml/min and detection was achieved at 235 nm using UV. Results: All peaks were sharp and well separated, the retention times were atenolol degradation (ATN Deg.) 2.311 min, atenolol (ATN) 2.580 min, hydrochlorothiazide degradation (HCT Deg.) 5.890 min, hydrochlorothiazide (HCT) 7.016 min, chlorthalidone degradation CTD Deg 8.018 min and chlorthalidone (CTD) 14.972 min. Linearity was obtained and the range of concentrations was 20- 160 μg/ml for atenolol, 10-80 μg/ml for hydrochlorothiazide and 10-80 μg/ml for chlorthalidone. According to ICH guidelines, method validation was accomplished, these methods include linearity, accuracy, selectivity, precision and robustness. Conclusion: The optimized method demonstrated to be specific, robust and accurate for the quality control of the cited drugs in pharmaceutical dosage forms.

A Green Liquid Chromatographic Method For The Simultaneous Determination of Chlorpheniramine Maleate, Pseudoephedrine Hydrochloride and Propyphenazone

2019 ◽  
Vol 15 (6) ◽  
pp. 635-641
Author(s):  
Nadia M. Mostafa ◽  
Ghada M. Elsayed ◽  
Nagiba Y. Hassan ◽  
Dina A. El Mously
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Dosage Form ◽  
Chromatographic Method ◽  
Green Analytical Chemistry ◽  
Chlorpheniramine Maleate ◽  
Accuracy And Precision ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Background:The concept of green analytical chemistry prevails due to the growing environmental pollution.Objective:Our attempts are to develop simple and eco-friendly method which is non-harmful to the environment by producing minimal waste. In this context, a green liquid chromatographic method was applied for the simultaneous determination of chlorpheniramine maleate, pseudoephedrine hydrochloride and propyphenazone in their combined dosage form.Methods:Separation was carried out using X select HSS RP C18 analytical column (250 × 4.6 mm, 5μm) using methanol - 0.02 M phosphate buffer pH 3 - triethylamine (60:40: 0.1, by volume) as a mobile phase. The separated peaks were detected at 215 nm at a flow rate 1.0 mL/min.Results:Quantification was done over the concentration ranges of 1-25 µg/mL for chlorpheniramine maleate, 5-35 µg/mL for pseudoephedrine hydrochloride and 10-120 µg/mL for propyphenazone. The suggested method was validated with regard to linearity, accuracy and precision according to the International Conference on Harmonization guidelines with good results.Conclusion:It could be used as a safer alternative for routine analysis of the mentioned drugs in quality control laboratories.

Validation of Liquid Chromatographic Method for Assay of Calcitriol and Alfacalcidol in Capsule Formulations

1986 ◽  
Vol 69 (6) ◽  
pp. 1026-1030
Author(s):  
Bruce C Flann ◽  
Bruce A Lodge
Keyword(s):  
Standard Deviation ◽  
Calibration Curve ◽  
Mobile Phase ◽  
Chromatographic Method ◽  
Liquid Chromatographic Method ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic ◽  
Better Than

Abstract The validation of a liquid chromatographic procedure suitable for the determination of calcitriol and alfacalcidol in their respective formulations labeled to contain at least 0.25 μ.g drug per unit is described. The capsule content is diluted and chromatographed in 15-20 min on silica columns (5 μm) with a mobile phase of hexane-tetrahydrofuranmethylene dichloride-isopropanol (72 + 12 + 12 + 4, v/v) with detection at 254 nm. The calibration curve is linear. Recoveries of “spikes” averaged 101% with a standard deviation of 2%. Precision was better than 1.5%.

scholarly journals Development and Validation of a Liquid Chromatographic Method for the Simultaneous Determination of Estradiol, Estriol, Estrone, and Progesterone in Pharmaceutical Preparations

2009 ◽  
Vol 92 (3) ◽  
pp. 846-854 ◽  
Author(s):  
Phyllis Wilson
Keyword(s):  
Mobile Phase ◽  
Chromatographic Method ◽  
Pharmaceutical Preparations ◽  
Men And Women ◽  
Naturally Occurring ◽  
Vital Functions ◽  
Liquid Chromatographic Method ◽  
Development And Validation ◽  
Liquid Chromatographic

Abstract Progesterone and estrogens are hormones produced in the human body that are essential for regulating many vital functions. The three major estrogens produced by women are estriol, estradiol, and estrone. Progesterone is a naturally occurring hormone in both men and women. Pharmaceuticals containing estrogens alone or estrogens in combination with progesterone are commonly used in therapy. Patients requiring unique combinations of the drugs rely on pharmacies to compound the ingredients. In order to assess the potency of drugs containing combinations of estrogens and progesterone, a method was developed to determine all four ingredients simultaneously. The liquid chromatographic method utilized a Bondapak C18 column with an isocratic mobile phase of acetonitrilewater (50 + 50, v/v) at a flow rate of 1.0 mL/min and temperature of 30C. Under these conditions, the order of elution was estriol, estradiol, and estrone, followed by progesterone. UV detection was at 205 nm to monitor elution of the estrogens, then switched to 270 nm to monitor progesterone. The method was applied to the analysis of pharmacy-compounded drugs containing combinations of the hormones. Validation studies demonstrated that the method is accurate and precise.

Determination of Cymiazole Residues in Honey by Liquid Chromatography

1993 ◽  
Vol 76 (1) ◽  
pp. 92-94 ◽  
Author(s):  
Paolo Cabras ◽  
Marinella Melis ◽  
Lorenzo Spanedda
Keyword(s):  
Liquid Chromatography ◽  
Chromatographic Analysis ◽  
Mobile Phase ◽  
Chromatographic Method ◽  
Reversed Phase ◽  
Limit Of Determination ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic ◽  
Control Samples

Abstract A liquid chromatographic method is described for the determination of cymiazole residues in honey. This acaricide is determined on a reversed-phase (C18) column, with a CH3CN-O.OOIN HCI-NaCI mixture (950 mL + 50 mL + 0.3 g/L) as the mobile phase, and UV detection at 265 nm. Cymiazole is extracted with n-hexane from aqueous alkalinized (pH 9) honey solutions. No further cleanup of the honey extract was required before chromatographic analysis. Recoveries on control samples fortified with 0.01,0.10, and 1.00 ppm cymiazole ranged from 92 to 102%. The limit of determination was 0.01 ppm.

scholarly journals New High-Performance Liquid Chromatographic Method for Determination of Clopidogrel in Coated Tablets

2008 ◽  
Vol 91 (1) ◽  
pp. 67-72 ◽  
Author(s):  
Juliana Sippel ◽  
Letcia L Sfair ◽  
Elfrides E S Schapoval ◽  
Martin Steppe
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Chromatographic Method ◽  
High Performance Liquid Chromatographic ◽  
Array Detector ◽  
Aqueous Sample ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract A new high-performance liquid chromatographic method was developed and validated for clopidogrel determination in pharmaceutical formulations. The system consisted of an ACE 5 octadecylsilane (C18; 150 4.6 mm id), 5.0 m particle size column; methanol0.1 triethylamine (75 + 25, v/v), pH 5.3, mobile phase at a flow rate of 1.2 mL/min; and a diode array detector set at 220 nm. Specificity, linearity, precision, accuracy, and robustness were the parameters evaluated. The retention time for clopidogrel was 6.8 min. To estimate specificity, an aqueous sample solution was subjected to degradation by ultraviolet light and by acid, alkaline, and oxidation media. The peaks of degradation products did not interfere with the compound signal, and there was no interference when a placebo solution was analyzed. Linearity over a concentration range of 10.0 to 90.0 g/mL was shown (correlation coefficient = 0.9998). Low values of relative standard deviation indicated the adequate intraday and interday precision. The average recovery was found as 99.16. In the robustness test, small modifications to the mobile phase composition did not affect the determination of clopidogrel. The proposed method proved to be simple, fast, and cost efficient for the intended use.

scholarly journals Taxane Contents of Taxus Cultivars Grown in American Nurseries

1997 ◽  
Vol 15 (4) ◽  
pp. 200-205 ◽  
Author(s):  
Hala N. ElSohly ◽  
Edward M. Croom ◽  
Wlodzimierz J. Kopycki ◽  
Alpana S. Joshi ◽  
Mahmoud A. ElSohly ◽  
...  
Keyword(s):  
United States ◽  
High Performance ◽  
Chromatographic Method ◽  
The United States ◽  
High Performance Liquid Chromatographic ◽  
Baccatin Iii ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Abstract The taxane content of the needles, stems and clippings of 92 cultivars obtained from ten nurseries in the United States is presented. The analysis of 10-desacetyl baccatin III (1), baccatin III (2), 10-desacetyl taxol (3) cephalomannie (4), 10-desacetyl-7-epi-taxol (5) and taxol (6) was carried out using a high performance liquid chromatographic method developed in our laboratory. The total ‘useful’ taxane content of the leaves, stems, and clippings in the studied cultivars ranged from 0.0135–0.1471%, 0.0055–0.0462% and 0.0121–0.1183%, respectively, with 1 and 6 being the most abundant. The survey identified 18 cultivars with a content of 1 ranging from 0.015% to 0.0622% and 24 cultivars with a content of 6 ranging from 0.012% to 0.062%; compound 2 was either undetectable or found in negligible amounts in all the cultivars studied. The contents of 3 varied between 0.0019–0.0264% and that of 4 between 0.0017–0.0386%, while that of 5 between 0–0.0107%.

REVERSE PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD FOR DETERMINATION OF BEXAROTENE IN CAPSULE DOSAGE FORM

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (05) ◽  
pp. 67-71
Author(s):  
N Dhanvijay ◽  
◽  
Vijaya Kumar Munipalli ◽  
M. Patel ◽  
S. Ghani ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Chromatographic Method ◽  
High Performance Liquid Chromatographic ◽  
Control Analysis ◽  
Capsule Formulation ◽  
Reverse Phase ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

A simple precise and rapid Reverse Phase High Performance Liquid Chromatographic method has been developed for quantitative determination of antineoplastic drug bexarotene and its capsule formulation. In this method Synchronis (C18, 25cm×4.6mm id , 5μ) column with mobile phase consisting of buffer (25mM ammonium acetate w/v solution adjusted to pH 4.0 with diluted acetic acid) and acetonitrile in the ratio of (20: 80 v/v) in an isocratic mode was used. The detection was carried out at 262 nm and 20.0 μL injection volume was selected, with the flow rate of 1.0 mL/min being used. The linearity range of bexarotene shows concentration between 5-200 μg/mL. Retention time of bexarotene was found to be 12.58 minutes. Mobile phase itself was used as a diluent. The method was validated as per ICH guidelines and is simple, fast, accurate, precise and can be applied for routine quality control analysis of bexarotene in its formulation.

Liquid Chromatographic Method for Determination of Aflatoxins B1, B2, G1, and G2 in Corn and Peanut Products: Collaborative Study

1990 ◽  
Vol 73 (2) ◽  
pp. 260-266 ◽  
Author(s):  
Douglas L Park ◽  
Stanley Nesheim ◽  
Mary W Trucksess ◽  
Michael E Stack ◽  
Richard F Newell
Keyword(s):  
Chromatographic Method ◽  
Peanut Butter ◽  
Collaborative Study ◽  
The United States ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Standard Deviations ◽  
Contamination Levels ◽  
Liquid Chromatographic

Abstract A collaborative study of a liquid chromatographic method for the determination of aflatoxins B1, B2, G1, and G2 was conducted in laboratories located in the United States, Canada, South Africa, and Switzerland. Twenty-one artificially contaminated raw peanuts, peanut butter, and corn samples containing varying amounts of aflatoxins B1, B2, G1, and G2 were distributed to participating laboratories. The test portion was extracted with methanol-0.1N HCl ( 4 + 1 ) , filtered, defatted with hexane, and then partitioned with methylene chloride. The concentrated extract was passed through a silica gel column. Aflatoxins B1 and G1 were derivatized with trifluoroacetic acid, and the individual aflatoxins were determined by reverse-phase liquid chromatography with fluorescence detection. Statistical analysis of the data was performed to determine or confirm outliers, and to compute repeatability and reproducibility of the method. For corn, relative standard deviations for repeatability (RSDr) for anatoxin B1 ranged from 27.2 to 8.3% for contamination levels from 5 through 50 ng/g. For raw peanuts and peanut butter, RSDr values for aflatoxin Bi were 35.0 to 41.2% and 11.2 to 19.1 %, respectively, for contamination levels from 5 through 25 ng/g. RSDr values for aflatoxins B2, G1, and G2 were similar. Relative standard deviations for reproducibility (RSDR) for aflatoxin B1 ranged from 15.8 to 38.4%, 24.4 to 33.4%, and 43.9 to 54.0% for corn, peanut butter, and raw peanuts, respectively. The method has been adopted official first action for the determination of aflatoxins B1, B2, G1, and G2 in peanut butter and corn at concentrations ≥13 ng total aflatoxlns/g.

scholarly journals Development and Validation of Liquid Chromatographic Method for Estimation of Ibuprofen and Famotidine in Combined Dosage Form

2012 ◽  
Vol 2012 ◽  
pp. 1-5 ◽  
Author(s):  
Dimal A. Shah ◽  
Dixita J. Suthar ◽  
Sunil L. Baldania ◽  
Usman K. Chhalotiya ◽  
Kashyap K. Bhatt
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Chromatographic Method ◽  
Reversed Phase ◽  
Assay Method ◽  
Liquid Chromatographic Method ◽  
Phase Liquid ◽  
Development And Validation ◽  
Liquid Chromatographic

An isocratic, reversed phase-liquid-chromatographic assay method was developed for the quantitative determination of ibuprofen and famotidine in combined-dosage form. A Brownlee C18, 5 μm column with mobile phase containing water : methanol : acetonitrile (30 : 60 : 10, v/v/v) was used. The flow rate was 1.0 mL/min, and effluents were monitored at 264 nm. The retention times of ibuprofen and famotidine were 4.9 min and 6.8 min, respectively. The linearity for ibuprofen and famotidine was in the range of 2–20 μg/mL and 0.1–10 μg/mL, respectively. The proposed method was validated with respect to linearity, accuracy, precision, specificity, and robustness. The method was successfully applied to the estimation of ibuprofen and famotidine in combined dosage form.

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