Simultaneous determination of vitamins A and E and carotenoids in plasma by reversed-phase HPLC in elderly and younger subjects

1993 ◽  
Vol 39 (11) ◽  
pp. 2229-2234 ◽  
Author(s):  
Z Zaman ◽  
P Fielden ◽  
P G Frost

Abstract A reversed-phase high-performance liquid-chromatographic method for the simultaneous determination of retinol, alpha-tocopherol, alpha-carotene, beta-carotene, cryptoxanthin, lutein/zeaxanthin, and lycopene is described. This method was applied to plasma measurements in healthy young and elderly subjects. The plasma, deproteinized with ethanol, is extracted twice with n-hexane. After evaporation, the residue is dissolved in 50 microL of tetrahydrofuran and made up to 200 microL with ethanol. Samples (50 microL) are injected onto a 250 x 4.6 mm column of 5-microns-particle Spherisorb ODS1 (Phase Separations) that had been equilibrated with solvent mixture A:B (90:10 by vol) [A = 100 mmol/L ammonium acetate in methanol: acetonitrile (80:20 by vol) and B = 100 mmol/L ammonium acetate in water] at 2 mL/min. The analytes are eluted by running a 12-min linear gradient to 100% A; solvent A is then maintained for 10 min. Intrabatch CVs were 2.3%, 3.3%, 2.8%, 3.6%, 3.6%, and 3.0% for retinol, alpha-tocopherol, lutein/zeaxanthin, cryptoxanthin, lycopene, and beta-carotene, respectively. The corresponding interbatch CVs were 4.9%, 5.8%, 12.3%, 6.5%, 8.0%, and 3.4%.

2009 ◽  
Vol 6 (2) ◽  
pp. 541-544 ◽  
Author(s):  
D. Anantha Kumar ◽  
D. P. Sujan ◽  
V. Vijayasree ◽  
J. V. L. N. Seshagiri Rao

A reverse phase high performance liquid chromatographic method was developed for the simultaneous determination of simvastatin and ezetimibe in tablet dosage forms. The separation was effected on a C18 Supelcosil column (250 mm x 4.6 mm; 5µ) using a mobile phase consisting of 0.01 M ammonium acetate buffer and acetonitrile (35:65v/v) at a flow rate of 1 mL/min. The detection was made at 240 nm. The retention times for ezetimibe and simvastatin were 5.9 and 8.5 min respectively. Calibration curves were linear over the ranges of 0.5-40 µg/mL for simvastatin and 2.5-50 µg/mL for ezetimibe. The proposed method was validated as per the ICH and USP guidelines. The method is accurate and precise and found to be suitable for the quantitative analysis of both the drugs individually and in combination in tablet dosage forms.


2012 ◽  
Vol 554-556 ◽  
pp. 2037-2040
Author(s):  
Yu Qin Li ◽  
Jing Zhao ◽  
Rui Duan ◽  
Bao Xiu Jia ◽  
Gui Rong You ◽  
...  

A reversed-phase high performance liquid chromatographic method was established for the simultaneous determination of tanshinones in three processing products of white flower Radix salvia miltiorrhiza. Cryptotanshinone, tanshinone IA and tanshinone IIA were successfully separated on a Yilite C18 column (250 mm x 4.6 mm, 5 µm). The mobile phase was a mixture of methanol, water, tetrahydrofuran and glacial acetic acid (70:24:5:1, v/v/v/v), employing isocratic elution at a flow rate of 1.0 mL/min. Detection was 254 nm. Regression equations revealed good linear relationship between the peak areas of the compounds and their concentrations (correlation coefficients: 0.9994 for cryptotanshinone, 0.9996 for tanshinone I A and 0.9996 for tanshinone IIA). The recoveries were between 98.03 % and 103.1 %. The method is simple, accurate and effective and can be used to determine the contents of tanshinones in processing products of Salvia miltiorrhiza bge. f. alba, and the contents of three tanshinones presented the stir-frying processing<the crude drugs<the wine prosessing.


1988 ◽  
Vol 34 (4) ◽  
pp. 724-729 ◽  
Author(s):  
M Hariharan ◽  
T VanNoord ◽  
J F Greden

Abstract We describe a rapid, sensitive method for the routine simultaneous determination of nicotine and cotinine in 1 mL of plasma. Extraction in 10-mL screw-capped Teflon tubes with methylene chloride after deproteinization with trichloroacetic acid eliminated emulsion formation. The extract, after evaporation and reconstitution in 30 microL of mobile phase, is injected into a reversed-phase C-18 ion-pair column of an isocratic high-performance liquid-chromatographic unit. Absorbance is monitored at 256 nm. The mobile phase is a citrate-phosphate (30 mmol each per liter) buffer mixture containing 50 mL of acetonitrile and 1 mmol of sodium heptanesulfonate per liter. 2-Phenylimidazole is the internal standard. The detection limit is 1 microgram/L for nicotine and 3 micrograms/L for cotinine. The standard curve is linear from 0 to 700 micrograms/L for both compounds. The average CV for nicotine in the concentration range 0-100 micrograms/L is 6.5%, and that for cotinine in the concentration range 50-700 micrograms/L is 4%.


2010 ◽  
Vol 7 (1) ◽  
pp. 198-202 ◽  
Author(s):  
R. Shinde Sachin ◽  
I. Bhoir Suvarna ◽  
S. Pawar Namdev ◽  
B.Yadav Suman ◽  
M. Bhagwat Ashok

A Simple, fast and precise reversed phase high performance liquid chromatographic method is developed for the simultaneous determination of satranidazole and ofloxacin. Chromatographic separation of these drugs were performed on Kromasil C18column (250 x 4.6 mm, 5 µ) as stationary phase with a mobile phase comprising of 20 mM potassium dihydrogen phosphate: acetonitrile in the ratio of 60:40 (v/v) containing 0.1% glacial acetic acid at a flow rate of 1 mL/min and UV detection at 318 nm. The linearity of satranidazole and ofloxacin were in the range of 1.5 to 3.6 µg/mL and 1.0 to 2.4 µg/mL respectively. The recovery was calculated by standard addition method. The average recovery was found to be 100.63% and 100.02% for satranidazole and ofloxacin respectively. The proposed method was found to be accurate, precise and rapid for simultaneous determination of satranidazole and ofloxacin


2009 ◽  
Vol 6 (1) ◽  
pp. 289-294 ◽  
Author(s):  
Uttam D. Pawar ◽  
Abhijit V. Naik ◽  
Aruna V. Sulebhavikar ◽  
Tirumal A. Datar ◽  
Kiran. V. Mangaonkar

A simple, fast and precise reversed phase high performance liquid chromatographic method is developed for the simultaneous determination of aceclofenac, paracetamol and chlorzoxazone. Chromatographic separation of the three drugs was performed on an Intersil C18column (250 mm × 4.6 mm, 5µm) as stationary phase with a mobile phase comprising of 10 mM potassium dihydrogen phosphate (pH adjusted to 5.55 with ammonia): acetonitrile in the ratio 60:40 (v/v) at a flow rate of 1.0 mL/min and UV detection at 205 nm. The linearity of aceclofenac, paracetamol and chlorzoxazone were in the range of 5.00-15.00 µg/µL, 25.00-75.00 µg/µL and 25.00-75.00 µg/µL respectively. The limit of detection for aceclofenac, paracetamol and chlorzoxazone was found to be 18.0 ng/mL, 22.0 ng/mL and 9.0 ng/mL respectively whereas, the limit of quantification was found to be 55 ng/mL, 65 ng/mL and 27.0 ng/mL respectively. The recovery was calculated by standard addition method. The average recovery was found to be 99.04%, 99.57% and 101.63% for aceclofenac, paracetamol and chlorzoxazone respectively. The proposed method was found to be accurate, precise and rapid for the simultaneous determination of aceclofenac, paracetamol and chlorzoxazone


2007 ◽  
Vol 90 (3) ◽  
pp. 693-699 ◽  
Author(s):  
Sonia Talaat Hassib ◽  
Mohammad Abdul-Azim Mohammad ◽  
Asmaa A El-Zaher ◽  
Ehab F El-Kady

Abstract New, simple, rapid, and precise reversed-phase high-performance liquid chromatographic (LC) methods were developed for the simultaneous determination of chlorzoxazone (CH) and ketoprofen (KT) in binary mixtures and in ternary mixtures containing the CH degradation product, 2-amino-4-chlorophenol (CD). The analytes were separated by LC on a Lichrosphere<sup/> 60 C18 column (250 4 mm, 5 m). The mobile phases, methanolwater (40:60, v/v) at 1 mL/min and methanol0.05% phosphoric acid (60:40, v/v, pH 2.81) at 1.5 mL/min, satisfactorily resolved the binary and ternary mixtures, respectively. The UV detector was operated at 280 nm for the determination of CH and at 254 nm for the determination of KT and CD. Linearity, accuracy, and precision were found to be acceptable over the concentration ranges of 20240 and 560 g/mL for CH and KT, respectively, in the binary mixtures and 50300, 1060, and 20160 g/mL for CH, KT, and CD, respectively, in the ternary mixtures. The optimized methods proved to be specific, robust, and accurate for the quality control of CH and KT in pharmaceutical preparations.


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