HPLC method for the determination of the S- and R-diastereomers of telaprevir for treatment of patients with hepatitis C

2015 ◽  
Vol 39 (3) ◽  
Author(s):  
Werner J. Heinz ◽  
Dieter Kuschak ◽  
Diana Schirmer ◽  
Anna Grau ◽  
Daniela Keller ◽  
...  
Keyword(s):  
Hepatitis C ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Clinical Samples ◽  
Coefficients Of Variation ◽  
Significant Difference ◽  
High Degree ◽  
Liquid Chromatographic

AbstractTelaprevir (TVR) was approved by the FDA in May 2011 for the treatment of hepatitis C. This protease inhibitor converts into two diastereomers with significant difference in antiviral activity. Clinical efficacy has been correlated with serum concentrations. Therefore, a sensitive and selective high-performance liquid chromatographic method for the simultaneous determination of both clinically relevant diastereomers of TVR was developed. Linearity ranged from 20 to 10,000 ng/mL. The coefficients of variation were <7.3%, and accuracy was between −4.0 and 5.4%. In 105 clinical samples, both diastereomers of TVR had a high degree of correlation to each other, but concentrations showed a broad range and an increase during therapy.

High Performance Liquid Chromatography of Aflatoxins in Cottonseed Products

1977 ◽  
Vol 60 (1) ◽  
pp. 89-95 ◽  
Author(s):  
Walter A Pons ◽  
Anthony O Franz
Keyword(s):  
Silica Gel ◽  
High Performance ◽  
Methylene Chloride ◽  
High Performance Liquid Chromatographic ◽  
Peak Height ◽  
Hplc Method ◽  
Coefficients Of Variation ◽  
Water Saturated ◽  
High Degree ◽  
Liquid Chromatographic

Abstract A precise and sensitive high performance liquid chromatographic (HPLC) method is proposed for determining aflatoxins in cottonseed products in 1.0—1.5 hr. After aqueous acetone extraction, lead acetate treatment, and partition of aflatoxins into methylene chloride, sample extracts are purified on a small silica gel column requiring only 125 ml solvent/sample. Aflatoxins B1 and B2 in the purified extract are resolved on a micro particulate (10 μm) silica gel column in ca 8 min, using a water-saturated chloroform - cyclohexane - acetonitrile solvent, with detection by ultraviolet absorbance at 365 nm. The resolution was highly reproducible, giving coefficients of variation of 0.2—1.0% for retention and 1.0—2.3% for quantitation. Recovery of added aflatoxins B1 and B2 was 90— 95% at levels of 5—100 μg/kg. The within-laboratory coefficients of variation of the entire method, based on repetitive assays of a cottonseed meal (34 μg B1/kg, 6 μg B2/kg), were 7.3% (B1) and 7.4% (B3). A high degree of correlation was obtained for HPLC estimation by 2 different commercial columns; for quantitation by peak height vs. electronic integration; and for quantitation by HPLC or thin layer chromatography.

High Performance Liquid Chromatographic Method for Determination of Temephos in Technical and Formulated Products: Collaborative Study

1982 ◽  
Vol 65 (3) ◽  
pp. 580-583
Author(s):  
James W Miles ◽  
Dwight L Mount
Keyword(s):  
Ethyl Acetate ◽  
High Performance ◽  
Collaborative Study ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Water Dispersible ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic

Abstract An HPLC method for the determination of temephos in temephos technical and formulated products has been subjected to an international collaborative study with 14 laboratories participating. Samples were extracted with ethyl acetate and eluted on a silica gel column with ethyl acetate-hexane (1 + 9); p-nitrophenyl p-nitrobenzoate served as the internal standard. Collaborators were furnished samples of technical, 20 and 50% emulsifiable concentrates, 50% water-dispersible powder, and 1% sand granules. The coefficients of variation of the values obtained on the 5 samples were 1.21,2.02,1.26,1.89, and 9.90%, respectively. The method has been adopted official first action.

scholarly journals A Reliable Semiautomated Method for the Determination of Total Thiamine in Whole Blood by the Thiochrome Method with High-Performance Liquid Chromatography

1982 ◽  
Vol 19 (1) ◽  
pp. 52-56 ◽  
Author(s):  
Jaap Schrijver ◽  
Andries J Speek ◽  
Jan A Klosse ◽  
Herman J M Van Rijn ◽  
Wil H P Schreurs
Keyword(s):  
Whole Blood ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Coefficients Of Variation ◽  
Analytical Recovery ◽  
On Line ◽  
Liquid Chromatographic ◽  
Hydrolysis Of

A sensitive and reliable method for the determination of total thiamine (vitamin B1) in whole blood has been developed which is suited for routine analysis. After extraction, and enzymatic hydrolysis of thiamine phosphate esters, thiamine is separated from interfering compounds by a fully automated high-performance liquid chromatographic (HPLC) system. Thiamine is detected fluorometrically as thiochrome. By calculating the concentration of thiamine on-line with the aid of a computer, it is possible to complete one analysis within four hours. Routine thiamine determinations can be carried out in a series of 120 samples within 48 hours. The within-assay and between-assay coefficients of variation of the analysis of total thiamine in whole blood were 4·2 and 4·4%, respectively. The between-assay analytical recovery of thiamine diphosphate added to blood samples was 99·9 ± 11·7% (mean ± SD). The HPLC method described has been applied also to the analysis of thiamine in plasma and erythrocytes. In agreement with other reports, it was found that about 80% of total thiamine of whole blood is present in the erythrocytes. Reference values of thiamine in whole blood of the human were found in the range 95–155 nmol/l.

scholarly journals Determination of Dyclonine Hydrochloride by a HPLC Method and Camphor and Menthol by a GC Method in Compound Lotion

2013 ◽  
Vol 2013 ◽  
pp. 1-4
Author(s):  
Suying Ma ◽  
Haixia Lv ◽  
Xiaojun Shang
Keyword(s):  
Retention Time ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Ionization Detector ◽  
Uv Detector ◽  
Flame Ionization ◽  
Liquid Chromatographic

A high performance liquid chromatographic (HPLC) method with UV detector for the determination of dyclonine hydrochloride and a gas chromatography (GC) method with flame ionization detector (FID) for the determination of camphor and menthol in lotion were developed. The developed HPLC method involved using a SinoChoom ODS-BP C18reversed-phase column (5 μm, 4.6 mm × 200 mm) and mobile phase consisting of acetonitrile : water : triethylamine in a ratio of 45 : 55 : 1.0; pH was adjusted to 3.5 with glacial acetic acid. The developed GC method for determination of camphor and menthol involved using an Agilent 19091J-413 capillary chromatographic column (30 m × 320 μm × 0.25 μm). The two methods were validated according to official compendia guidelines. The calibration of dyclonine hydrochloride for HPLC method was linear over the range of 20–200 μg/mL. The retention time was found at 6.0 min for dyclonine hydrochloride. The calibration of camphor and menthol of GC method was linear over the range of 10–2000 μg/mL. The retention time was found at 2.9 min for camphor and 3.05 min for menthol. The proposed HPLC and GC methods were proved to be suitable for the determination of dyclonine hydrochloride, camphor, and menthol in lotion.

REVERSE PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD FOR DETERMINATION OF REGORAFENIB IN TABLET DOSAGE FORM

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (06) ◽  
pp. 63-68
Author(s):  
R. Raut ◽  
◽  
A. Patil ◽  
V. K Munipalli ◽  
M. Patel ◽  
...  
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Control Analysis ◽  
Reverse Phase ◽  
Ich Guidelines ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A simple precise and rapid Reverse Phase High Performance Liquid Chromatographic (RP-HPLC) method has been developed for quantitative determination of Regorafenib in tablet dosage form. In this method Hypersil Gold (C18, 150mm× 4.6mm id, 3μ) column with mobile phase consisting of Trifluoroacetic acid (0.2% v/v) and Acetonitrile in the ratio of (50: 50 v/v) at 400C in an isocratic mode was used. The detection was carried out at 260 nm and 20μL injection volume was selected with the flow rate 1mL/min. The linearity range of Regorafenib shows concentration between 5-200 μg/mL. The regression coefficient obtained was 0.999. Retention time of Regorafenib was found to be 6.49 minutes. Acetonitrile and Water in the ratio of (3:1) 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 Regorafenib in tablet dosage form.

DEVELOPMENT AND VALIDATION OF A NEW RP HPLC METHOD FOR ROUTINE DETERMINATION OF TEA TREE OIL IN BULK AND COSMECEUTICAL FORMULATIONS

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (07) ◽  
pp. 43-49
Author(s):  
B.P. Manjula ◽  
V. G Joshi ◽  
Siddamsetty Ramachandra Setty ◽  
M Geetha ◽  
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Tea Tree Oil ◽  
Tea Tree ◽  
Liquid Chromatographic Method ◽  
Development And Validation ◽  
Liquid Chromatographic

Tea tree oil, an active ingredient of skin, hair and nail care cosmeceuticals, has claims for topical antimicrobial, analgesic and anti-inflammatory activity. Its complex composition is governed by ISO 4730:2017. Terpinene-4-ol is the principal constituent of the oil (35% - 48%) followed by γ-terpinene (14% -28%), α-terpinene (6%-12%) and 1,8-cineole (≤15%). A reversed-phase, isocratic high performance liquid chromatographic method has been developed and validated for routine determination of tea tree oil based on1,8-cineole content in bulk and commercially available cosmeceuticals using C18 column, methanol-water (70:30 v/v) as mobile phase and flow rate of 1mL/min. UV detection was done at 200 nm. Linearity of the method was established for 20-100μL/mL (R2 = 0.9992) with LOD, LOQ values of 0.5594 μL/mL and 5.5941μL/mL respectively. The % RSD values for robustness and precision were <1% and recovery ranged between 99.09-102.96%. The method was successfully applied for determination of 1,8-cineole content in cosmeceuticals.

scholarly journals Development of a New High-Performance Liquid Chromatographic Method for the Determination of Ceftazidime

2008 ◽  
Vol 91 (4) ◽  
pp. 739-743 ◽  
Author(s):  
Andréia de Haro Moreno ◽  
Hérida Regina Nunes Salgado
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Calibration Graph ◽  
Raw Material ◽  
Relative Standard ◽  
Validation Parameters ◽  
Liquid Chromatographic

Abstract A rapid, accurate, and sensitive high-performance liquid chromatographic (HPLC) method was developed and validated for the determination of ceftazidime in pharmaceuticals. The method validation parameters yielded good results and included range, linearity, precision, accuracy, specificity, and recovery. The excipients in the commercial powder for injection did not interfere with the assay. Reversed-phase chromatography was used for the HPLC separation on a Waters C18 (WAT 054275; Milford, MA) column with methanolwater (70 + 30, v/v) as the mobile phase pumped isocratically at a flow rate of 1.0 mL/min. The effluent was monitored at 245 nm. The calibration graph for ceftazidime was linear from 50.0 to 300.0 g/mL. The values for interday and intraday precision (relative standard deviation) were &lt;1. The results obtained by the HPLC method were calculated statistically by analysis of variance. We concluded that the HPLC method is satisfactory for the determination of ceftazidime in the raw material and pharmaceuticals.

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.

High Performance Liquid Chromatographic Determination of Methapyrilene Hydrochloride in Feed and Sleep Aid Tablets

1981 ◽  
Vol 64 (4) ◽  
pp. 889-892
Author(s):  
Badaruddin Shaikh ◽  
Margarette R Hallmark
Keyword(s):  
High Performance ◽  
Ammonium Carbonate ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Reverse Phase ◽  
Phase Partition ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Methapyrilene hydrochloride (MP·HCl) was extracted from feed with methanol and determined by reverse phase partition chromatography in less than 15 min, using isocratic elution with acetonitrile-1.1% ammonium carbonate (1 + 1) as the mobile phase. This procedure was tested on feed treated with MP·HCl at levels of 125,500, and 2000 ppm. Recoveries were 104,95, and 96% with coefficients of variation of 2.4,1.6, and 0.6%, respectively. MP·HCl in feed was stable for 14 days. This method was also successfully used to determine MP·HCl in 3 sleep aid tablets.

High Performance Liquid Chromatographic Determination of Primidone in Tablets

1982 ◽  
Vol 65 (5) ◽  
pp. 1063-1065
Author(s):  
Stanley E Roberts
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Average Recovery ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A high performance liquid chromatographic (HPLC) method is described for the quantitative determination of primidone in tablets. A ground tablet sample is diluted directly in the mobile phase, at a concentration of about 1 mg/mL of primidone, mixed and deaerated, and filtered. The resulting solution is then quantitated by HPLC. The average spike recoveries for the 50 mg and 250 mg tablets were 101.2% and 99.0%, respectively. The average recovery for an authentic mixture formulated at the 250 mg level was 100.1% with a relative standard deviation of 0.45%.

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