A novel on-line two-step stacking preconcentration method by sweeping plus micelle to solvent stacking in capillary zone electrophoresis was developed for the simultaneous determination of three organic anions (vanillic acid, ferulic acid and cinnamic acid) in . Hexadimethrine bromide was used for electroosmotic flow reversal. The main experimental parameters that affected the separation and sensitivity were investigated and optimized. The best separation was achieved in 50 mM ammonium acetate (pH 12.0) containing 50% methanol (v/v) under a negative voltage of 20 kV. The micellar solution was a mixed solution comprised of 12 mM cetyltrimethyl ammonium bromide and 20 mM ammonium acetate. After injecting a short plug (0.5 psi, 30 s) of micellar solution, the sample was introduced into the capillary at 0.5 psi for 45 s. Under the optimal conditions, the sensitivity enhancement factors obtained by the developed method were between 42 and 77. The intra-day ( = 6) and inter-day ( = 5) precisions of the method expressed as their relative standard deviations were found to be less than 7.2%. The sample was pulverized and then refluxed in 95% ethanol and filtered. After an aliquot of the extractant was dried, it was reconstituted in 20 mM ammonium acetate for capillary electrophoresis analysis. The recoveries of the analytes by this method for the analysis of were in the range of 94.4% to 108.4%.
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http://dx.doi.org/10.1039/c7ra11553a | DOI Listing |
J Sep Sci
January 2025
Department of Analytical, Bioanalytical Sciences and Miniaturization (LSABM) Chemistry, Biology and Innovation (CBI), UMR CNRS-ESPCI Paris 8231, ESPCI Paris, PSL University, CNRS, Paris, France.
Adduction on protein nucleophile sites by mustard agents can be monitored to assess detection of retrospective exposure to these agents. Cysteine 34 (Cys34) on human serum albumin was selected as the target of choice. This work targets di- and tripeptides adducted on Cys34 by sulfur mustard, sesquimustard, and nitrogen mustards separated in hydrophilic liquid chromatography (HILIC) and Reversed-Phase (RP) mode.
View Article and Find Full Text PDFJ Chromatogr Sci
December 2024
Analytical Research Laboratory, Cadila Pharmaceuticals Ltd., Dholka, Ahmedabad 382225, India.
N-nitrosamine impurities have been detected in a vast variety of drug substances and drug products, showing concern for regulatory aspects. To meet the regulatory requirement for the concerned impurity, a sensitive analytical method capable of quantifying these impurities at a lower level with accuracy and precision is required. This article focuses on the development and validation of an analytical method for the simultaneous detection of nine nitrosamine impurities in a single method for nebivolol drug product using liquid chromatography-mass spectrometry/mass spectrometry-atmospheric pressure chemical ionization (LC-MS/MS-APCI).
View Article and Find Full Text PDFJ Sep Sci
December 2024
Natural and Medical Sciences Research Center, University of Nizwa, Nizwa City, Oman.
Micellar liquid chromatography (MLC) has proven beneficial efficiency and ecological impact for routine quality control activities. In the proposed study, cyrene was investigated for the first time, together with other green additives, as a novel safe organic solvent in reversed-phase MLC. Quality-by-design (QbD) approach screened their effect on the separation performance.
View Article and Find Full Text PDFElectrophoresis
December 2024
Chinese Academy of Inspection and Quarantine, Beijing, China.
An analytical method for identifying the chemical constituents in the Chinese herbal combination Jiuwei decoction was established using capillary electrophoresis coupled with quadrupole time-of-flight mass spectrometry. Nine herbs were extracted with a 60:40 (v/v) ethanol/water solution to prepare the Jiuwei decoction. Electrophoretic separation was carried out using a 50 µm i.
View Article and Find Full Text PDFMass Spectrom (Tokyo)
December 2024
Department of Applied Chemistry for Environment, School of Science and Technology, Kwansei Gakuin University, Gakuen-Uegahara-1, Sanda, Hyogo 669-1330, Japan.
A simple and rapid analytical method was developed for the simultaneous determination of two chromium species, Cr(III) and Cr(VI), in the environmental waters by high-performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS). This study incorporated a chelating pretreatment with 2,6-pyridinedicarboxylic acid (PDCA) to convert Cr(III) species into a stable Cr(III)-PDCA anion complex, which was then separated from Cr(VI) oxyanion using an anion exchange column. Building on the fundamental analytical approach proposed by Shigeta .
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