High Performance Liquid Chromatographic Determination of Primidone in Tablets

1982 ◽  
Vol 65 (5) ◽  
pp. 1063-1065
Author(s):  
Stanley E Roberts

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%.

1988 ◽  
Vol 34 (9) ◽  
pp. 1897-1899 ◽  
Author(s):  
M H Cheng ◽  
W Y Huang ◽  
A I Lipsey

Abstract This high-performance liquid-chromatographic (HPLC) method for simultaneous determination of prednisone and its metabolite, prednisolone, in plasma is a modification of the method of Frey et al. (Clin Chem 1979;25:1944-7). Heparinized plasma (1.0 mL) with 0.1 mL of internal standard solution (11-deoxy-17-hydroxycorticosterone, 2 mg/L) is extracted with 7.0 mL of dichloromethane, then washed sequentially with 0.1 mol/L HCl, 0.1 mol/L NaOH, and deionized water, 2.0 mL each. The extract is evaporated and the residue reconstituted with 75 microL of mobile phase, methanol/H2O (40/60 by vol). Thirty microliters of this is injected onto a reversed-phase C6 column, which is eluted at 1.4 mL/min. Analytical recoveries of prednisone and prednisolone were 94-98% and 102-106%, respectively. Day-to-day precision (CV) was 3.8% for prednisone, 6.1% for prednisolone. We encountered no interference from the 21 other steroids and 25 drugs tested. This method is simple, accurate, and precise.


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.


1981 ◽  
Vol 64 (5) ◽  
pp. 1083-1087 ◽  
Author(s):  
Mary W Trucksess ◽  
Leonard Stoloff

Abstract Samples of milk were extracted with chloroform, the extract was transferred to methanol, and residual interferences were removed by liquid-liquid partition against hexane and by silica gel column chromatography. Aflatoxicol (AFL) in the purified extract was resolved on a μBondapak C18 column, using water - methanol - acetonitrile - tetrahydrofuran (70 + 15 + 20 + 3) as the mobile phase, and measured with a fluorescence detector (excitation 325-385 nm, emission >408 nm). Recoveries of AFL added to samples of whole pasteurized milk at levels ranging from 0.025 to 0.10 ng/mL averaged 92% (range 78- 100%). The method for AFL has also been applied to the analysis of raw milk, whole beef blood, and beef liver, with recoveries of 70-88%.


1983 ◽  
Vol 66 (3) ◽  
pp. 606-609 ◽  
Author(s):  
Samy H Ashoor ◽  
George J Seperich ◽  
Woodrow C Monte ◽  
Jim Welty

Abstract A method was developed for determining caffeine in decaffeinated coffee, tea, and beverage products by high performance liquid chromatography (HPLC). The HPLC system consisted of a Bio-Sil ODS-5S C18 column, methanol-water (25 + 75) mobile phase at 1 mL/min, and a UV detector. The method is simple and specific. Caffeine recoveries were 93.8-98.3% and coefficients of variation were 0.90-2.25%.


2010 ◽  
Vol 93 (4) ◽  
pp. 1121-1128 ◽  
Author(s):  
Jelena Letica ◽  
Slavko Marković ◽  
Jelena Zirojević ◽  
Katarina Nikolić ◽  
Danica Agbaba

Abstract An RP-HPLC method for simultaneous separation and quantification of pantoprazole and its five main impurities in pharmaceutical formulations was developed and validated. The separation was accomplished on a Zorbax Eclipse XDB C18 column (5 m particle size, 150 4.6 mm id) using a gradient with mobile phase A [bufferacetonitrile (70 + 30, v/v)], and mobile phase B [bufferacetonitrile (30 + 70, v/v)]. The buffer was 0.01 M ammonium acetate solution with addition of 1 mL triethylamine/L of the solution, adjusted to pH 4.5 with orthophosphoric acid. The eluent flow rate was 1 mL/min, the temperature of the column was 30C, and the eluate was monitored at 290 nm. Linearity (r = 0.999), recovery (97.6105.8), RSD (0.551.90), and LOQ (0.0991.48 g/mL) were evaluated and found to be satisfactory. The proposed method can be used for simultaneous identification and quantification of the analyzed compounds in pharmaceutical formulations.


1980 ◽  
Vol 63 (3) ◽  
pp. 595-599
Author(s):  
W Jeffrey Hurst ◽  
Robert A Martin ◽  
◽  
M Bueno ◽  
H Clemente ◽  
...  

Abstract A collaborative study determining sucrose, glucose, fructose, maltose, and lactose in chocolate products was conducted using a previously published high performance liquid chromatographic (HPLC) method. Five samples (2 milk chocolates, 1 dark chocolate, 1 powdered mix, and 1 sirup) were analyzed in duplicate by 7 collaborators. The results indicate adequate method precision. In addition, the HPLC method allows for the simultaneous determination of 5 saccharides in chocolate products in 15 min. The method has been adopted as official first action.


1983 ◽  
Vol 66 (2) ◽  
pp. 304-308
Author(s):  
Teruhisa Hirayama ◽  
Naohide Yamada ◽  
Motoshi Nohara ◽  
Shozo Fukui

Abstract A simple high performance liquid chromatographic (HPLC) method has been developed for determining malondialdehyde (MDA) in vegetable oils. MDA was reacted with dansyl hydrazine in an acidic medium, and the product, 1-dansyl-pyrazole, was determined by HPLC, using a Zorbax sil column with mixed mobile phase of n-hexane-methylene chloride. MDA can be determined as 1-dansyl-pyrazole by f luorometric detection at a level of 0.01 ppm in vegetable oils.


2007 ◽  
Vol 90 (6) ◽  
pp. 1532-1538 ◽  
Author(s):  
Bharathi Avula ◽  
Vaishali C Joshi ◽  
Yan-Hong Wang ◽  
Ikhlas A Khan

Abstract A high-performance liquid chromatographic (HPLC) method with ultraviolet absorption detection was developed to determine the presence of anthraquinones, polydatin, and resveratrol in Polygonum multiflorum Thunb. as well as other medicinal Polygonum species, viz., P. cuspidatum, P. oriental, P. aviculare, and P. vulgare, as well as commercial products that claim to contain P. multiflorum. The best results were obtained with a Phenomenex Gemini C18 column using gradient mobile phase composed of water (0.1 acetic acid) and acetonitrile (0.1 acetic acid). Elution was at a flow rate of 1.0 mL/min. The detection wavelength was 280 nm for anthraquinones and 320 nm for polydatin and resveratrol. The main anthraquinones identified were emodin and physcion. The HPLC pattern of P. multiflorum was also compared with 5 other species of Polygonum. The method was validated for precision, repeatability, and accuracy. The relative standard deviation was between 0.9 and 1.6. The method was sensitive, quick, and accurate for determination of anthraquinones, polydatin, and resveratrol in 6 different species of Polygonum and can be used for quality control of P. multiflorum. The commercial samples and the 6 Polygonum species were compared microscopically, and a detailed description is provided for P. multiflorum.


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