A high pressure liquid chromatographic (HPLC) procedure for the analysis of methyl paraben (MP) and propyl paraben (PP) in pharmaceutical preparations containing a halogenated hydroxyquinoline (HHQ) is described. phenolic constituents, MP, PP and HHQ with a Bio-Rad AG 1-X8 anion exchange resin, elution of the phenols with methanol after acidification and a reverse phase HPLC separation of the parabens using methanol -pH 6.5 buffer (60140) mobile phase, a 30 cm x 3.9 mm (i.d.) column packed with Waters WBondapak c18 packing and a guard column packed with Waters Bondapak C18/Corasil packing. Recovery, precision, specificity and interference data along with the application of the proposed method for some commercial formulations both with and without a hydroxyquinoline are described.
Fast HPLC offers a definite time advantage for analyses such as content uniformity which requires, in general, a routine analysis of as many as 30 samples and for the analysis of dosage forms of developmental drugs. The columns for Fast HPLC can be used with a minimal amount of modification to conventional HPLC hardware. The resolution obtainable with a Fast HPLC column is poorer than that of a conventional column.(All references to conventional columns in the article imply, unless otherwise indicated, those columns 15-30 cm in length and 3.9-4.6 mm i.d.) improve the resolution of a closely eluting peak resulted in retention times not too different from typical conventional columns. tion and a savings in both solvent and sample consumption, the utility of these columns is limited by the need for specialized hardware. Since the sample volume is not a limiting factor in a typical pharmaceutical analysis and overall cost savings from lesser solvent consumption are not significant in a majority of Attempts to modify a mobile phase to Although microbore columns offered improved resolu-3393 Copyright 0 1987 by Marcel Dekker, Inc. Downloaded by [Duke University Libraries] at 15:44 03 January 2015 3394 PADMANABHAN ET AL.cases as solvent can be recycled, it is concluded that the Fast HPLC columns can play a more important role than the currently available microbore columns in laboratories engaged in pharmaceutical analysis, particularly at the product development stage.Fast high pressure liquid chromatography (1, 2) (Fast HPLC) is a technique in high pressure liquid chromatographic (HPLC) analysis in which the components of analytical interest are eluted in the order of 30 to 100 seconds, which is about 5 to 10 times faster than conventional HPLC.should not be confused with Technicon "Fast-LC"B, which is a sample pretreatment system ( 3 ) . ] Fast HPLC and the columns employed with it have been referred to in the literature by terminologies such as "Fast Analysis by HPLC" ( 4 ) , "Fast LC Separations" (5), "High Speed Chromatography" ( 6 ) , "High Speed, Low Dispersion LC" (7), "Very High Speed Liquid Chromatography" (8, 9, lo), "High Speed LC Using Short Columns" ( 7 ) , "Short High Efficiency HPLC Column" ( 1 1 ) , "Very Short LC Column" ( 1 2 ) , and "Little Champ@" ( 1 3 ) . These columns are typically short [This technique and packed with smaller particles with the following column parameters: size -3 or 5 microns. ferred mainly for the following reasons (14): the gain in chromatographic run time was not significant in terms of total analysis time, which includes sample clean-up and post HPLC length -3 to 5 cm; diameter -4 . 6 mm and particle In the past, Fast HPLC was not predata processing times; columns with 3 micron packings were not available commercially and the 5 micron or larger column Downloaded by [Duke University Libraries] at 15:44 03 January 2015 FAST HPLC IN PHARMACEUTICAL ANALYSIS 3395 packings available at that time had, in general, poor reso tion characteristics; and the hardware available were not s...
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