Improved direct determination of alpha- and gamma-tocopherols in plasma and platelets by liquid chromatography, with fluorescence detection.

1982 ◽  
Vol 28 (8) ◽  
pp. 1784-1787 ◽  
Author(s):  
J Lehmann ◽  
H L Martin

Abstract Tocopherols extracted from plasma with methanol or from platelets with chloroform/methanol were injected in methanol on a reversed-phase (C18) "high-performance" liquid-chromatographic column and eluted with water/methanol (2/98, by vol) at a flow rate of 1.4 mL/min. A "high-performance" spectrophotofluorometer was used for detection. Analytical recoveries ranged from 89 to 106%. The response was linear to at least 0.3 micrograms of either tocopherol (alpha- or gamma-) applied to the column, and the limit of detection was 0.1 ng. The method was used to measure tocopherols in plasma and platelets from human subjects, and some values are presented.

1977 ◽  
Vol 23 (11) ◽  
pp. 1984-1988 ◽  
Author(s):  
A M Krstulovic ◽  
P R Brown ◽  
D M Rosie ◽  
P B Champlin

Abstract Concentrations of total tryptophan were determined rapidly and sensitively in 50 microliter of serum by a reversed-phase partition version of high-performance liquid chromatography. For determination of total tryptophan, sample preparation requires only precipitation of the serum protein with trichloroacetic acid and removing excess trichloroacetic acid with a 1,1,2-trichlorotrifluoroethane(Freon)/tri-N-octylamine solution. Tryptophan in serum samples was detected by ultraviolet and fluorescence spectrometry. No interferences from the naturally occurring constituents of serum were observed. Elution time for tryptophan is 15 min, the limit of detection is 1 pmol.


2013 ◽  
Vol 10 (3) ◽  
pp. 1014-1022
Author(s):  
Baghdad Science Journal

A simple, precise, rapid, and accurate reversed – phase high performance liquid chromatographic method has been developed for the determination of guaifenesin in pure from pharmaceutical formulations.andindustrial effluent. Chromatography was carried out on supelco L7 reversed- phase column (25cm × 4.6mm), 5 microns, using a mixture of methanol –acetonitrile-water: (80: 10 :10 v/v/v) as a mobile phase at a flow rate of 1.0 ml.min-1. Detection was performed at 254nm at ambient temperature. The retention time for guaifenesin was found 2.4 minutes. The calibration curve was linear (r= 0.9998) over a concentration range from 0.08 to 0.8mg/ml. Limit of detection (LOD) and limit of quantification ( LOQ) were found 6µg/ml and 18µg/ml respectively. The method was validated for its linearity, precision and accuracy .The proposed method was successfully applied for the determination of guaifenesin in syrups and industrial effluent samples.


1983 ◽  
Vol 29 (10) ◽  
pp. 1840-1842 ◽  
Author(s):  
J Lehmann ◽  
H L Martin

Abstract We have adapted to erythrocytes a method for the determination of alpha- and gamma-tocopherols in plasma and platelets. Erythrocytes (50 microL) were extracted with methanol containing tocol (internal standard) and pyrogallol. Tocopherols were partitioned into chloroform, washed, and injected in methanol onto a reversed-phase (C18) "high-performance" liquid-chromatographic column. The mobile phase was methanol/water (99/1 by vol) at a flow rate of 2 mL/min and detection was with a "high-performance" spectrophotofluorometer. The limit of detection for either tocopherol is 0.10 microgram/mL of packed cells. Analytical recoveries ranged from 93 to 104%. Some values for tocopherols in human erythrocytes are presented.


2019 ◽  
Vol 31 (5) ◽  
pp. 1002-1008
Author(s):  
Somana Siva Prasad ◽  
G.V. Krishna Mohan ◽  
A. Naga Babu

A novel reversed-phase high performance liquid chromatographic (HPLC) technique for the determination of everolimus (Isomer-B) and its impurities in the tablet dosage form has been optimized using analytical quality by design (QbD) approach. All the compounds are monitored with the photodiode array (PDA) detector at 280 nm and the parameters namely; precision, accuracy, specificity, stability, linearity, limit of quantitation (LOQ) and limit of detection (LOD) are evaluated. The quantitation limits of IMP-A, IMP-B, IMP-C, IMP-D, IMP-E, Sirolimus and TGR are found to be 0.08, 0.08, 0.10, 0.10, 0.10, 0.08 and 0.08, respectively. Recovery studies from 0.9 mg/L to 9.0 mg/L are performed for all impurities and the values were obtained between 85-110 %. Injection volume and test concentrations have been optimized to achieve LOQ values under the reporting threshold. The whole technique is developed and validated as per International Council for Harmonization (ICH) guidelines. The proposed method is robust, sensitive, rapid and successful and helpful in the regions where regulatory agencies recommend HPLC analytical method.


2021 ◽  
Vol 9 (2) ◽  
Author(s):  
Darinka Brodnjak Vončina ◽  
Maša Islamčivic Razboršek ◽  
Marjana Simonič

The aim of this study was to develop a method for identification and quantification of phenolic acids in different wine samples. The simple reversed-phase HPLC-UV method for simultaneous determination of p-coumaric and ferulic acid was developed. The method was validated and working range, linearity, repeatability, accuracy, limit of quantitation LOQ and limit of detection LOD were determined. The linearity of the method was tested in concentration ranges 0.1-1 mg L-1 and 1-10 mg L-1. The correlation coefficients (r2) were greater than 0.996 and quality coefficients (QC) ≤ 5%. Detection limit for both compounds was 0.01 mg L-1. The method is precise (RSD


2007 ◽  
Vol 4 (1) ◽  
pp. 109-116 ◽  
Author(s):  
K. Basavaiah ◽  
B. C. Somashekar

A rapid, highly sensitive high performance liquid chromatographic method has been developed for the determination of finasteride(FNS) in bulk drug and in tablets. FNS was eluted from a ODS C18reversed phase column at laboratory temperature (30 ± 2°C) with a mobile phase consisting of methanol and water (80+20) at a flow rate of 1 mL min-1with UV detection at 225 nm. The retention time was ∼ 6.1 min and each analysis took not more than 10 min. Quantitation was achieved by measurement of peak area without using any internal standard. Calibration graph was linear from 2.0 to 30 μg mL-1with limits of detection (LOD) and quantification (LOQ) being 0.2 and 0.6 μg mL-1, respectively. The method was validated according to the current ICH guidelines. Within-day co efficients of variation (CV) ranged from 0.31 to 0.69% and between-day CV were in the range 1.2-3.2%. Recovery of FNS from the pharmaceutical dosage forms ranged from 97.89 – 102.9 with CV of 1.41-4.13%. The developed method was compared with the official method for FNS determination in its tablet forms.


INDIAN DRUGS ◽  
2013 ◽  
Vol 50 (05) ◽  
pp. 48-52
Author(s):  
A Lodhi ◽  
◽  
A Jain ◽  
B. Biswal

A validated high performance liquid chromatographic method was developed for the determination of chromium picolinate in pharmaceutical dosage forms. The analysis was performed at room temperature using a reversed-phase ODS, 5µm (250×4.6) mm column. The mobile phase consisted of acetonitrile: buffer (60:40 V/V) at a flow rate of 0.5 mL/min. The PDA-detector was set at 264 nm. The developed method showed a good linear relationship in the concentration range from 1.5 – 12.5 µg/mL with a correlation coefficient from 0.999. The limit of detection and limit of quantification were 0.0540513 and 0.1637919 µg/mL respectively.


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