Determination of phenolic preservatives in gelatin and vacant capsules for medicine use by ion-suppression reversed-phase high performance liquid chromatography.
ABSTRACT A reliable method for the simultaneous determination of phenolic preservatives parahydroxybenzoic acid, methyl, ethyl, propyl, butyl and pentyl parahydroxybenzoates in gelatin and vacant capsules for medical use has been developed by ion-suppression reversed-phase high performance liquid chromatography. Separation was carried out on a Kromasil C(18) column by isocratic elution using methanol-perchloric acid (pH 2.0; 10 mM) (60:40, v/v) at a flow-rate of 1.0 ml min(-1), and detection by UV absorbance at a wavelength of 254 nm. This method has been successfully applied to the routine analyses of these preservatives in the real samples.
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ABSTRACT: The application of high performance liquid chromatography time-of-flight mass spectrometry (HPLC/TOF-MS) for the qualitation and quantitation of 11 synthetic antioxidants and preservatives in edible vegetable oil samples is reported here. The qualitation by HPLC/TOF-MS is accomplished with the accurate mass of the deprotonated molecules [M−H]−, along with the accurate mass of their main fragment ion. In order to obtain sufficient sensitivity for quantitation purposes (using deprotonated molecule), segment programme of fragmentor voltage is designed in negative ion mode. The mass accuracy typically obtained is routinely better than 5 ppm. The 11 compounds behave linearly in the 0.05–5.0 mg/kg concentration range, with correlation coefficient >0.997. The recoveries at the tested concentrations of 0.1–2.0 mg/kg are 65.8–106.9%, with coefficients of variation <8.1%. The method illustrated is suitable for routine qualitative and quantitative analyses of synthetic antioxidants and preservatives in edible vegetable oils.Food Chemistry. 01/2009;
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ABSTRACT: Optimized conditions for the determination of 14 food preservatives were selected by using interpretative optimization strategy and Derringer’s desirability function for combining three main chromatographic goals: resolution, separation time and ruggedness. The best mobile phase for separation by micellar liquid chromatography contains 0.045M SDS and 1.0% (v/v) 1-pentanol at pH 2.5 adjusted with trichloroacetic acid. The accuracy of the method was confirmed by analysis of spiked samples and is useful for routine analysis of food preservatives in drinks due to simple sample preparation, safety and low cost of micellar mobile phases.Chromatographia 03/2008; 67(7):615-620. · 1.44 Impact Factor
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ABSTRACT: A novel and quick ultra performance liquid chromatography-photo diode array detector method has been developed and validated for the simultaneous determination of ten synthetic preservatives in foodstuff. An Acquity BEH C18 column (50×2.1mm i.d., 1.7μm particle size) was used. The mobile phase consisted of a mixture of acetonitrile and 20mM potassium dihydrogen phosphate/phosphoric acid (pH 4.29) buffer at the gradient elution program. The ten compounds behaved linearly in the 0.100–20.0μgmL−1 concentration range, with correlation coefficient >0.999. The precision inter- and intra-day of the ten synthetic preservatives at three concentration levels were 0.11–5.75% (RSD). The recoveries at three different concentrations were 88.7–99.0%, with coefficients of variation <6.3%. The method was applied to the determination of preservatives in cola beverages, fruit-flavoured carbonate beverages and fruit juice beverages, and proved its suitability for quick and reliable quality control.Chromatographia 06/2008; 68(1):57-63. · 1.44 Impact Factor