899 resultados para High-performance Liquid Chromatography-mass Spectrometry (hplc-ms)


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A high performance liquid chromatographic method for the simultaneous determination of five organochlorine pesticides (aldrin, p,p’-DDT, dieldrin, endrin, and heptachlor) was developed. The method was used to determine the levels of these pesticides in medicinal plant samples. Analysis was carried out using a Merck LiChrospher 100 RP C18 (5 μm) column with a gradient solvent system of acetonitrile-water and PDA UV detection (224 nm). Quantification was carried out by the external standard method. The limit of detection for the utilized method was below the local legal limits (ANZFA) for similar plant materials for all 5 pesticides excepting endrin. Medicinal plant extracts were further analyzed by conventional GC-ECD and GC-NPD means using SPE and GPC cleanup as required.

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Extracts of Echinacea spp. are widely used as therapeutic immunostimulants with such activity being attributed in part to the alkamide fractions of these plants. Using high performance liquid chromatography, the levels of 8 alkamides, including 2 tetraene alkamides (dodeca-2E, 4E, 8Z, 10E/Z-tetraenoic acid isobutylamide), were quantitatively determined in 2 Australian-grown Echinacea spp. Overall, the levels of alkamides in Australian-grown E. angustifolia were found to be comparable with levels obtained in this study and other studies for USA and European Echinacea spp. However, results obtained for one sample of E. angustifolia suggested that it may have been mislabelled and that it was most likely a sample of E. pallida. Levels of tetraene alkamides in Australian-grown E. purpurea were also similar to, if not higher, than levels which have been reported for the same species grown in Germany and the USA. Preliminary studies on the stability of alkamide compounds in E. angustifolia indicated that they are susceptible to degradation, with a 13% loss of alkamide level over 2 months. Overall, results indicate that there is considerable potential to develop Echinacea as a viable crop in Australia.

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Flos Chrysanthemum is a generic name for a particular group of edible plants, which also have medicinal properties. There are, in fact, twenty to thirty different cultivars, which are commonly used in beverages and for medicinal purposes. In this work, four Flos Chrysanthemum cultivars, Hangju, Taiju, Gongju, and Boju, were collected and chromatographic fingerprints were used to distinguish and assess these cultivars for quality control purposes. Chromatography fingerprints contain chemical information but also often have baseline drifts and peak shifts, which complicate data processing, and adaptive iteratively reweighted, penalized least squares, and correlation optimized warping were applied to correct the fingerprint peaks. The adjusted data were submitted to unsupervised and supervised pattern recognition methods. Principal component analysis was used to qualitatively differentiate the Flos Chrysanthemum cultivars. Partial least squares, continuum power regression, and K-nearest neighbors were used to predict the unknown samples. Finally, the elliptic joint confidence region method was used to evaluate the prediction ability of these models. The partial least squares and continuum power regression methods were shown to best represent the experimental results.

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A method was presented for the determination of testosterone, methyltestosterone and progesterone in liquid cosmetics by coupling polymer monolith microextraction (PMME) to high performance liquid chromatography with UV detection. A poly (methacrylic acid-ethylene glycol dimethacrylate) monolithic capillary column was selected as the extraction medium, which showed high extraction capacity towards these compounds. To achieve optimum extraction performance, several parameters relating to PMME were investigated, including extraction flow rate and pH value, inorganic salt and organic phase concentration of the sample matrix. By simple dilution with phosphate solution and filtering, the sample solution then could be directly injected into the device for extraction. The limits of detection of testosterone, methyltestosterone and progesterone were calculated to be 2, 3, 2, 8 and 4.6 mu g/L. Good linearity was achieved in the range of 10 to 1000 mu g/L with a linear coefficient. r value above 0. 996. Excellent method reproducibility was found by intra- and inter-day precisions, yielding the relative standard deviations of < 7. 7 % and < 7. 5 %, respectively. Recovery for them in the real samples was between 83% and 119%.

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This paper presents a method for trace level analysis of microcystins in water using solid-phase extraction and high performance liquid chromatography. The optimized condition enabled the determination of common microcystins at levels as low as 0.02 similar to 0.05 mug/L, and the liner range is from 0.1 mug/L to 50 mug/L. The method has been applied to the analysis of field sample from Dianchi lake.

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A simple, sensitive, and mild method for the determination of amino compounds based on a condensation reaction with fluorescence detection has been developed. 9-(2-Hydroxyethyl)acridone reacts with coupling agent N,N-carbonyldiimidazole at ambient temperature to form activated amide intermediate 9-(2-acridone)oxyethylcarbonylimidazole (AOCD). The amide intermediate (AOCD) preferably reacts with amino compounds under mild reactions in the presence of 4-(dimethylamino)pyridine (base catalyst) in acetonitrile to give the corresponding sensitively fluorescent derivatives with an excitation maximum lambda(ex) 404 mn and an emission maximum at lambda(em) 440 nm. The labeled derivatives exhibit high stability under reversed-phase conditions. The fluorescence intensities of derivatives in various solvents or at different temperatures were investigated. The method, in conjunction with a gradient elution, offers a baseline resolution of the common amine derivatives on a reversed-phase C-18 column. The LC separation for the derivatized amines shows good reproducibility with acetonitrile-water including 2.5% DMF as mobile phase. The relative standard deviations (n = 6) for each amine derivative are <4.5%. The detection limits (at a signal-to-noise ratio of 3) per injection were 0.16-12.8 ng/mL. Further research for the field of application, based on the AOCD amide intermediate as derivatization reagent, for the determination of free amines in real water samples is achieved.

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2-(9-Carbazole)-ethyl-chloroformate (CEOC), a novel pre-column fluorescence derivatization reagent, has been developed for the analysis of aromatic amines. Taking five monocyclic aromatic amines (o-toluidine, aniline, 3,4-dimethylaniline, N-ethyl-p-toluidine, and p-phenylenediamine) as testing compounds, derivatization conditions such as pH of borate buffer, reaction time and fluorescent tagging reagent concentration have been investigated. By a one-step procedure, CEOC reacts readily with the aromatic amines to form stable derivatives with excitation and emission wavelengths, respectively, at 293 and 360 nm. This derivatization reaction could be finished within 20 min even at room temperature. The peak shapes of the derivatized aromatic amines can be improved greatly without any addition of competition amines into the mobile phase. Furthermore, this method can offer excellent quantitative precision with high tolerance of the matrix of samples. (C) 2003 Elsevier B.V. All rights reserved.