Application of the desulfurization of phenothiazines for a sensitive detection method by high-performance liquid chromatography

Shimada, Kenji; Mino, Tsukasa; Nakajima, Mitsutoshi; Wakabayashi, Hiroyuki; Yamato, Susumu

doi:10.1016/0378-4347(94)00329-7

Cited by 6 publications

(3 citation statements)

References 6 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…percritical fluid chromatography, 12 liquid chromatography, 13,14 and capillary electrophoresis 15 have been applied for the determination of phenothiazines. Recently, some liquid chromatography/mass spectrometry (LC/MS) methods have been developed for the determination of the phenothiazine derivatives with basic side chains.…”

mentioning

confidence: 99%

“…The large variety of analytical techniques used for this purpose confirms this statement. Titration, photometry, fluorometry, chemiluminescence, electroanalysis, enzyme inhibition assays, mass spectrometry (MS), gas chromatography, supercritical fluid chromatography, liquid chromatography, , and capillary electrophoresis have been applied for the determination of phenothiazines. Recently, some liquid chromatography/mass spectrometry (LC/MS) methods have been developed for the determination of the phenothiazine derivatives with basic side chains. , Protonation of the nitrogen atoms in the side chains provides for high ionization yields and therefore low limits of detection.…”

mentioning

confidence: 99%

See 1 more Smart Citation

Analysis of Phenothiazine and Its Derivatives Using LC/Electrochemistry/MS and LC/Electrochemistry/Fluorescence

Hayen

Kärst

2003

Anal. Chem.

View full text Add to dashboard Cite

The on-line electrochemical conversion of phenothiazine and its derivatives after liquid chromatographic separation has been studied by mass spectrometry and fluorescence spectroscopy. In an electrochemical cell consisting of porous glassy carbon, the phenothiazines are readily converted to oxidized products, which can be detected by on-line fluorescence spectroscopy and mass spectrometry. The method allows rapid investigations on the electrochemical oxidation pathways, as demonstrated for phenothiazine itself. The phenothiazine derivatives are transferred into their strongly fluorescent sulfoxides. Based on this reaction, an LC/electrochemistry/fluorescence method was developed that allows for limits of detection between 5 x 10(-9) and 4 x 10(-8) mol/L and limits of quantification between 2 x 10(-8) and 1 x 10(-7) mol/L for the individual phenothiazines. The linear ranges comprised three decades starting at the limit of quantification.

show abstract

mentioning

confidence: 99%

mentioning

confidence: 99%

Analysis of Phenothiazine and Its Derivatives Using LC/Electrochemistry/MS and LC/Electrochemistry/Fluorescence

Hayen

Kärst

2003

Anal. Chem.

View full text Add to dashboard Cite

show abstract

“…(316) Applications of photochemical reactors to a variety of pharmaceuticals, such as phenothiazines, have been summarized. (317,318) A precolumn derivatization method for phenothiazine involves desulfurization with Raney nickel to produce diphenylamine, which is electrochemically active. (319) A detection limit of 10 pg was found.…”

Section: Sulfur Compoundsmentioning

confidence: 99%

Chemical Reagents and Derivatization Procedures in Drug Analysis

Danielson

Gallagher

Bao

2008

Encyclopedia of Analytical Chemistry

View full text Add to dashboard Cite

This article describes both pre‐ and postcolumn derivatization chemistry used in conjunction with either chromatography or capillary electrophoresis (CE) to facilitate the determination of drugs. Generally, only prederivatization is used in gas chromatography (GC), principally to enhance the volatility, temperature stability, and/or detectability. The GC section considers derivatization of drugs by reagent class: alkylation, acylation, and silylation. The GC sample‐handling section describes an approach that combines the extraction and derivatization steps together. Both pre‐ and postcolumn derivatization are common approaches for high‐performance liquid chromatography (HPLC) and many of these methods have been adapted for CE. Derivatization for HPLC is often directed toward aliphatic amines, carboxylic acids, or alcohols that are difficult to detect at low levels by absorbance, luminescence, or electrochemical means. In addition, small hydrophilic molecules upon prederivatization are often converted into larger more hydrophobic compounds, making reversed‐phase HPLC easier or even feasible. The HPLC section considers derivatization of drugs based on the following types: alkaloids, amines, antibiotics, barbiturates, carbonyl compounds and carboxylic acids, catecholamines, hydroxy compounds, steroids, and sulfur compounds. For the GC and HPLC sections, tables are included, giving the structures of the more important derivatizing agents, the analytes, and the corresponding reaction products. A brief rationale for derivatization chemistry with CE concludes this article. For CE, derivatization is often done to improve detectability as the path length for absorbance detection is very short and fluorescence can be effective using laser‐based systems.

show abstract

High performance liquid chromatography/electrospray tandem mass spectrometry for phenothiazines with heavy side chains in whole blood

Seno

Hattori

Ishii

et al. 1999

Rapid Commun. Mass Spectrom.

View full text Add to dashboard Cite

Eleven phenothiazine derivatives with heavy side chains contained in human whole blood have been analyzed by high-performance liquid chromatography (HPLC)/electrospray (ES) tandem mass spectrometry (MS). All compounds gave the base peaks due to [M + 1](+) by HPLC/ES single MS. The product ions formed from each quasi-molecular ion by HPLC/ES tandem MS showed the base peaks due to side chains liberated. The mass chromatography of HPLC/ES tandem MS showed much higher sensitivity than that of HPLC/ES single MS for phenothiazines spiked to whole blood. Therefore, regression equations, detection limits, recovery rates and reproducibility were studied for thiethylperazine, clospirazine and flupentixol spiked to human whole blood by means of mass chromatography of HPLC/ES tandem MS. The three compounds showed good linearity in the range of 2-40 ng/mL with a detection limit of about 0.5 ng/mL. Recoveries of the three compounds spiked to whole blood (2 and 8 ng added to 1 mL whole blood) were 43.4-72.5 %; the coefficients of intraday and interday variations were 3.7-9.3 and 12.6-17.9 %, respectively. Thiethylperazine, clospirazine and flupentixol in whole blood could actually be determined with sufficient sensitivity 3 and 6 h after oral administration of 5-10 mg of each compound in a volunteer.

show abstract

Application of the desulfurization of phenothiazines for a sensitive detection method by high-performance liquid chromatography

Cited by 6 publications

References 6 publications

Analysis of Phenothiazine and Its Derivatives Using LC/Electrochemistry/MS and LC/Electrochemistry/Fluorescence

Analysis of Phenothiazine and Its Derivatives Using LC/Electrochemistry/MS and LC/Electrochemistry/Fluorescence

Chemical Reagents and Derivatization Procedures in Drug Analysis

High performance liquid chromatography/electrospray tandem mass spectrometry for phenothiazines with heavy side chains in whole blood

Contact Info

Product

Resources

About