Application of atmospheric pressure chemical ionisation mass spectrometry in the analysis of barbiturates by high‐speed analytical countercurrent chromatography

Abstract

Four barbiturates (barbital, allobarbital, phenobarbital and butalbital) were analysed using high-speed analytical countercurrent chromatography (HSACCC) and high-performance liquid chromatography (HPLC) interfaced with mass spectrometry, using negative mode atmospheric pressure chemical ionisation (APCI). The polar biphasic solvent system of butyronitrile/acetonitrile/water (1:1:1) was used, in the upper-stationary, lower-mobile mode of operation, at a flow rate of 1 mL/min and a rotational speed of 1200 rpm, equating to an applied "g"-field of 177 g. The fractional stationary phase retention (S(F)) was 0.58. Representative mass spectral data are presented from the HPLC and the HSACCC analyses. Structural information was obtained using source-induced fragmentation at increased source block voltages. The effect of increasing g-field on chromatographic resolution is illustrated using the binary base system of butyronitrile/water (1:1), under electrospray ionisation.

Preparation of Magnetic Molecularly Imprinted Polymer for Cyclobarbital and Its Application to the Assay of Phenobarbital in Human Serum

“…A lot of analytical methods have been developed for the determination of one or more barbiturates in biological samples such as serum or urine and environmental samples. Those include GC [4,5], GC-MS [6,7], LC-MS [3,8,9] and LC-MS/MS [10,11]. Recently, LC-MS and LC-MS/MS have been mainly used since they require no sample derivatization for vaporization, but are sensitive with high reproducibility.…”

Complete Biotransformation of Protopanaxadiol-Type Ginsenosides into 20-O-β-Glucopyranosyl-20(S)-protopanaxadiol by Permeabilized Recombinant Escherichia coli Cells Coexpressing β-Glucosidase and Chaperone Genes

“…Ginsenosides, the primary active ingredients of ginseng ( Panax ginseng C. A. Meyer), have traditionally been used to strengthen immunity, provide nutrition, and reduce fatigue in Asia. − Dammarane-type ginsenosides are classified into two groupsprotopanaxadiol (PPD) types and protopanaxatriol (PPT) typesbased on their chemical structures. The PPD-type ginsenosides exhibit different sugars at the hydroxyl groups of C3 and C20 of the aglycone PPD skeleton, whereas the PPT-type ginsenosides show different sugars at the hydroxyl groups of C6 and C20 of the aglycone PPT skeleton. − …”

Competitive immunoassay of phenobarbital by microchip electrophoresis with laser induced fluorescence detection

“…These methods include mainly high-performance liquid chromatography [4][5][6][7][8][9][10][11], gas chromatography [12][13][14] and capillary electrophoresis [15][16][17]. However, as a result of the increase in the number of determinations done for antiepileptic drugs, immunoassay has become the most common method for routine therapeutic drug monitoring because of its simplicity, reliability and speed.…”