Determination of glycolic acid in cosmetics by online liquid chromatography-Fourier transform infrared spectrometry.
ABSTRACT An isocratic online liquid chromatography Fourier transform infrared procedure has been developed for the determination of glycolic acid in cosmetics. The method involves the ultrasound-assisted extraction of glycolic acid from the samples with an acetonitrile:phosphate buffer (25 mM, pH 2.7) (3:97 v/v). The extracts were centrifuged and filtered before their injection into the chromatography system, which was equipped with a C18 column and used a flow rate of 150 microL min(-1). FTIR spectra were acquired using a time-resolved rapid scan mode. To calculate the chromatograms, the spectral area was integrated between 1288 and 1215 cm(-1), with baseline correction established between 1319 and 1150 cm(-1), after correcting for the eluent spectral background. Peak area values of the extracted sample chromatograms were interpolated from an external calibration curve. The method provided a limit of detection of 0.034 mg mL(-1) and a relative standard deviation of 6% for five measurements at the 0.174 mg mL(-1) concentration level. Recovery values obtained by spiking 400 mg of three commercially available samples with amounts of glycolic acid from 3.7 to 9.8 mg ranged between 99.6 and 101%. The results obtained for the commercial samples agree well with their declared concentrations. An attempt to directly determine glycolic acid by attenuated total reflectance measurements using partial least squares calibration showed that results were strongly influenced by compounds coextracted from the matrix.
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ABSTRACT: In the present study the simultaneous use of two quantum cascade lasers (QC-lasers) was investigated for the on-line detection in high performance liquid chromatography (HPLC). An optical set-up based on three gold mirrors and a ZnSe beam splitter was used to direct the emitted laser light trough a liquid flow cell with an optical path length of 52μm onto a mercury-cadmium-telluride (MCT) detector. Using the separation of eight components of wine and grape juice as an example, on-line dual QC-laser detection in HPLC could be shown successfully for the first time.Applied Physics B 06/2010; 99(4):833-840. DOI:10.1007/s00340-010-4013-y · 1.63 Impact Factor
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ABSTRACT: A capillary liquid chromatographic system has been successfully interfaced with a mid-IR Fourier transform infrared (FT-IR) spectrometer. Spectra were recorded on-line using a micromachined transmission CaF(2) cell (internal volume of 7.5 nL) that was placed on a dedicated beam condenser attached to the spectrometer. Linear gradients were run from (50:50) to (35:65) water (0.05% TFA)/acetonitrile in 15 min for the separation of standard solutions of four nitrophenols (4-nitrophenol, 3-methyl-4-nitrophenol, 2,4-dinitrophenol, and 2-nitrophenol) in a reversed phase system, providing limits of detection between 35 and 94 ng on-column. The changing background absorption due to gradient elution was successfully corrected by using a dedicated algorithm implemented in Matlab. When this chemometric data treatment was used, highly characteristic analyte spectra could be recorded as indicated by correlation coefficients between 89 and 95.8%, obtained when comparing mid-IR spectra of standard solutions and the spectra extracted from the chromatogram.Analytical Chemistry 05/2009; 81(10):3746-53. DOI:10.1021/ac8025459 · 5.83 Impact Factor
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ABSTRACT: A new background correction method for the on-line coupling of gradient liquid chromatography and Fourier transform infrared spectrometry has been developed. It is based on the use of a point-to-point matching algorithm that compares the absorption spectra of the sample data set with those of a previously recorded reference data set in order to select an appropriate reference spectrum. The spectral range used for the point-to-point comparison is selected with minimal user-interaction, thus facilitating considerably the application of the whole method. The background correction method has been successfully tested on a chromatographic separation of four nitrophenols running acetonitrile (0.08%, v/v TFA):water (0.08%, v/v TFA) gradients with compositions ranging from 35 to 85% (v/v) acetonitrile, giving accurate results for both, baseline resolved and overlapped peaks.Talanta 03/2010; 80(5):1771-6. DOI:10.1016/j.talanta.2009.10.021 · 3.51 Impact Factor