A Rapid High-Performance Liquid-Chromatographic Method for Simultaneously Determining the Concentrations of TFM and Bayer 73 in Water During Lampricide Treatments

1982 ◽  
Vol 39 (5) ◽  
pp. 778-782 ◽  
Author(s):  
V. K. Dawson

The high-performance liquid-chromatography (HPLC) procedure requires only minutes per sample, is specific, and is relatively sensitive (limit of detection < 0.005 mg/L for both chemicals). A combined buffer (pH 4) and internal standard (3-chlorodiphenylamine) reagent is added to the water sample, which is injected through a Sep Pak C18 disposable cartridge. The cartridge adsorbs and retains both the lampricides and the internal standard. The quantitative elution of the three chemicals from the cartridge with a small volume of methanol effectively concentrates the sample and provides sample cleanup. The methanol extract is then analyzed directly by HPLC on an MCH 10 reverse phase column by using a methanol:0.01 mol/L acetate buffer (87:13, v:v) as the mobile phase at 2 mL/min and detected by ultraviolet spectrophotometry at 330 (or 254) nm. A microprocessor data system further facilitates the procedure by quantifying off-scale peaks and yielding results directly in units of concentration (mg/L).Key words: sea lamprey, lampricides, methodology, chromatographic techniques, 3-trifluoromethyl-4-nitrophenol, 2′,5-dichloro-4′-nitrosalicylanilide, streams

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.


INDIAN DRUGS ◽  
2012 ◽  
Vol 49 (09) ◽  
pp. 27-32
Author(s):  
V. S Reddy ◽  
◽  
T. E. G. K. Murthy ◽  
N Usha Rani ◽  
R. S Rao ◽  
...  

A simple, precise, accurate, reproducible, robust reverse phase high-performance liquid chromatographic method was developed for the simultaneous estimation of frovatriptan, almotriptan and zolmitriptan in bulk and pharmaceutical dosage forms. The method was validated as per ICH and FDA guidelines. Analysis of the drugs was performed on Phenomenex Chromosil C-18 (250 x 4.6 mm, 5 mc) column, in an isocratic mode employing methanol, acetonitrile and THF in the ratio of 46:50:04 (v/v/v) as mobile phase. UV-visible detector at 269 nm was found to be suitable for detection. Linearity was observed in the range of 40-100 ppm.The % recovery was found to be 99.51, 99.69 and 99.34 for frovatriptan, almotriptan and zolmitriptan respectively. The % RSD values for method precision was found to be 0.86, 0.65 and 1.28 for frovatriptan, almotriptan and zolmitriptan respectively. Limit of quantification (LOQ) and limit of detection (LOD) values were found to be 0.15, 0.08 and 0.09 ppm. and 0.05, 0.02, 0.03 for frovatriptan, almotriptan and zolmitriptan respectively.


1982 ◽  
Vol 28 (7) ◽  
pp. 1478-1481 ◽  
Author(s):  
H Kelly ◽  
A Huggett ◽  
S Dawling

Abstract In this simple and rapid "high-performance" liquid-chromatographic method for determining nitrazepam in plasma, serum, or whole blood, the sample at pH 7.4 is extracted into diethyl ether with an internal standard (prazepam), chromatographed, and detected at 280 nm with a fixed-wavelength ultraviolet detector. A specimen, together with standards and a quality control, can be analyzed in duplicate within 90 min. The limit of sensitivity is 5 micrograms/L (nitrazepam and 7-acetamidonitrazepam) and 50 micrograms/L (7-aminonitrazepam), and no interferents have been found. This method has the advantages of a small sample requirement and complete resolution of nitrazepam and the above-mentioned major metabolites. We have used this method for analysis of therapeutic and overdose concentrations of nitrazepam, and to investigate the stability of the drug in blood.


1982 ◽  
Vol 65 (3) ◽  
pp. 753-756
Author(s):  
Walter F Schmidt

Abstract A high performance liquid chromatographic procedure has been developed for the assay of phenprocoumon in tablets. In comparison to the present official USP assay procedure, it is equivalent in precision and accuracy and is faster and more specific. A mobile phase consisting of a 1% solution of acetic acid in acetonitrile-water (4 + 3) separates phenprocoumon from warfarin internal standard on a 6 μm octadecylsilane (ODS) column with UV detection at 311 nm. The method enables the concurrent determination of phenprocoumon and possible contaminants such as salicylic acid.


1979 ◽  
Vol 25 (3) ◽  
pp. 401-404 ◽  
Author(s):  
S J Soldin ◽  
Y P Chan ◽  
B M Hill ◽  
J M Swanson

Abstract We describe a "high performance" liquid chromatographic method for quantitating methylphenidate in serum. The internal standard, 4,5-diphenylimidazole, and serum or plasma sample are extracted in chloroform, evaporated, and redissolved in 20 mmol/L potassium phosphate (pH 3.5)/high-purity acetonitrile, 80/20 by vol. A centrifuged aliquot is chromatographed on mu-Bondapak C-18 with the phosphate/acetonitrile solvent as mobile phase, a flow rate of 1.6 mL/min, and a column temperature of 40 degrees C. Absorbances are read at 192 nm. This method reliably measures concentrations greater than 20 micrograms/L and has analytical recoveries of 74%.


1982 ◽  
Vol 28 (10) ◽  
pp. 2143-2148 ◽  
Author(s):  
P M Edelbroek ◽  
E J de Haas ◽  
F A de Wolff

Abstract To study correlations between the concentrations, in serum, of amitriptyline and its most important metabolites with clinical response in patients, we developed a "high-performance" liquid-chromatographic method for routine determination of amitriptyline, nortriptyline, total 10-hydroxy-amitriptyline, desmethylnortriptyline, and E(trans)- and Z(cis)-10-hydroxynortriptyline. These compounds are extracted from 1 mL of alkalinized serum into hexane/isoamyl alcohol (99/1 by vol). Perazine is the internal standard. To minimize irreversible adsorption of the drugs onto the glassware, 5 micrograms of maprotiline is added to the organic phase just before evaporation. After a 10-min resolution on a silica column eluted with acetonitrile/methanol/NH4OH (1 mol/L), absorbance is measured at 240 nm. Only chlorimipramine, doxepin, procainamide, and N-acetylprocainamide may interfere with assay of the compounds that probably are therapeutically relevant: amitriptyline, nortriptyline, and E-10-hydroxynortriptyline. Uremia, lipemia, and icterus also do not affect the analysis.


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.


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