Fluorogenic reactions for biomedical chromatography

Ohkura, Yosuke; Kai, Masahiro; Nohta, Hitoshi

doi:10.1016/0378-4347(94)00125-1

Cited by 79 publications

(46 citation statements)

References 173 publications

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“…Derivatization of analyte molecules with chemical reagents, prior to LC/fluorescence (Ohkura et al, 1994), GC/MS (Segura et al, 1998) or LC/ESI/MS (Barry et al, 2003) analysis has been well documented in the literature. Quirke et al (1994) first reported the use of dansyl chloride to derivatize phenols in order to improve the electrospray sensitivity, although they did not give specific applications.…”

Section: Lc/ms/msmentioning

confidence: 99%

Development and validation of a high‐sensitivity liquid chromatography/tandem mass spectrometry (LC/MS/MS) method with chemical derivatization for the determination of ethinyl estradiol in human plasma

Shou

Jiang

Weng

2004

Biomedical Chromatography

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An ultra-sensitive liquid chromatography/tandem mass spectrometry (LC/MS/MS) method for the analysis of oral contraceptive ethinyl estradiol (EE) was developed and validated over the curve range of 2.5-500 pg/mL using 1 mL of human plasma sample. Ethinyl estradiol and the internal standard, ethinyl estradiol tetra-deuterated (EE-d4), were extracted from the plasma matrix with methyl t-butyl ether, derivatized with dansyl chloride and then back-extracted into hexane. The hexane phase was evaporated to dryness, reconstituted and injected onto the LC/MS/MS system. The chromatographic separation was achieved on a Luna C(18) column (50 x 2 mm, 5 micro m) with an isocratic mobile phase of 20:80 (v/v) water:acetonitrile with 1% formic acid. The offline derivatization procedure introduced the easily ionizable tertiary amine function group to EE. This greatly improved analyte sensitivity in electrospray ionization and enabled us to achieve the desired lower limit of quantitation at 2.5 pg/mL. This high sensitivity method can be used for therapeutic drug monitoring or supporting bio-equivalence and drug-drug interaction studies in human subjects.

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Section: Lc/ms/msmentioning

confidence: 99%

Development and validation of a high‐sensitivity liquid chromatography/tandem mass spectrometry (LC/MS/MS) method with chemical derivatization for the determination of ethinyl estradiol in human plasma

Shou

Jiang

Weng

2004

Biomedical Chromatography

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“…There are numerous fluorescent derivatization reagents for carboxylic acids for high-performance liquid chromatography (HPLC) and CE (Waterval et al, 2000;Mukherjee and Karnes, 1996;Ohkura et al, 1994;Toyo'oka, 1995). The reagents bearing positive or negative charge seem to be suitable for CE.…”

Section: Introductionmentioning

confidence: 99%

Design and synthesis of a hydrophilic fluorescent derivatization reagent for carboxylic acids, 4‐N‐(4‐N‐aminoethyl)piperazino‐7‐nitro‐2,1,3‐benzoxadiazole (NBD‐PZ‐NH₂), and its application to capillary electrophoresis with laser‐induced fluorescence detection

Santa

Matsumura

Huang

et al. 2002

Biomedical Chromatography

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A hydrophilic fluorescent derivatization reagent for fatty acids, 4-N-(4-N-aminoethyl)piperazino-7-nitro-2,1,3-benzoxadiazole (NBD-PZ-NH 2 ), was designed and synthesized. NBD-PZ-NH 2 possesses not only a fluorophore and a reacting group but also a positive charge group and, thus, was hydrophilic and suitable for application to capillary electrophoresis. NBD-PZ-NH 2 reacted with fatty acids in the presence of triphenylphosphine (TPP) and 2,2'-dipyridyl disulfide (DPDS) at room temperature within 10 min. The derivatives were strongly fluoresced and were positively charged at pH below 3. The derivatives of C4-C20 fatty acids were separated within 10 min in 50% acetonitrile in water containing 30 mM ammonium acetate and 1.0 M acetic acid by capillary electrophoresis with laser-induced fluorescence (CE-LIF) detection. The detection limits attained were 6.5 nM (signal-to-noise ratio of 3). It is proposed that NBD-PZ-NH 2 is a prominent derivatization reagent for fatty acids which is suitable for CE-LIF application.

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“…18 During the early stage of the method development, attempts were made to use OPA as the derivatizing reagent, but the OPA derivates are very unstable and degrade within 30 min. The Dansyl-Cl derivates are more stable than OPA derivates.…”

Section: Methods Selectionmentioning

confidence: 99%

Quantification of fudosteine in human plasma by high‐performance liquid chromatography‐electrospray ionization mass spectrometry employing precolumn derivatization with 9‐fluorenylmethyl chloroformate

Zhang

Jiao

et al. 2006

J. Mass Spectrom.

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This paper describes a novel method for the sensitive and selective determination of fudosteine in human plasma. The method involves a derivatization step with 9-fluorenylmethyl chloroformate (FMOC-Cl) in borate buffer and detection based on high-performance liquid chromatography-electrospray ionization mass spectrometry (LC/ESI/MS). After acetonitrile-induced protein precipitation of plasma samples, fudosteine was derivatized with FMOC-Cl, then extracted by ethyl acetate, evaporated, reconstituted and injected using an LC/ESI/MS instrument. Separation was achieved using an ODS column and isocratic elution. Excellent linearity was obtained for the entire calibration range from 0.05 to 20 microg/ml. Validation assays of the lower limit of quantification (LLOQ) as well as for the intra- and inter-batch precision and accuracy met the international acceptance criteria for bioanalytical method validation. Using the developed analytical method, fudosteine could be detected for the first time in human plasma with a low limit of detection (LLOD) of 0.03 microg/ml. The proposed method has been successfully applied to study the pharmacokinetics of fudosteine in healthy Chinese volunteers after single and multiple oral administration.

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Fluorogenic reactions for biomedical chromatography

Cited by 79 publications

References 173 publications

Development and validation of a high‐sensitivity liquid chromatography/tandem mass spectrometry (LC/MS/MS) method with chemical derivatization for the determination of ethinyl estradiol in human plasma

Development and validation of a high‐sensitivity liquid chromatography/tandem mass spectrometry (LC/MS/MS) method with chemical derivatization for the determination of ethinyl estradiol in human plasma

Design and synthesis of a hydrophilic fluorescent derivatization reagent for carboxylic acids, 4‐N‐(4‐N‐aminoethyl)piperazino‐7‐nitro‐2,1,3‐benzoxadiazole (NBD‐PZ‐NH₂), and its application to capillary electrophoresis with laser‐induced fluorescence detection

Quantification of fudosteine in human plasma by high‐performance liquid chromatography‐electrospray ionization mass spectrometry employing precolumn derivatization with 9‐fluorenylmethyl chloroformate

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Fluorogenic reactions for biomedical chromatography

Cited by 79 publications

References 173 publications

Development and validation of a high‐sensitivity liquid chromatography/tandem mass spectrometry (LC/MS/MS) method with chemical derivatization for the determination of ethinyl estradiol in human plasma

Development and validation of a high‐sensitivity liquid chromatography/tandem mass spectrometry (LC/MS/MS) method with chemical derivatization for the determination of ethinyl estradiol in human plasma

Design and synthesis of a hydrophilic fluorescent derivatization reagent for carboxylic acids, 4‐N‐(4‐N‐aminoethyl)piperazino‐7‐nitro‐2,1,3‐benzoxadiazole (NBD‐PZ‐NH2), and its application to capillary electrophoresis with laser‐induced fluorescence detection

Quantification of fudosteine in human plasma by high‐performance liquid chromatography‐electrospray ionization mass spectrometry employing precolumn derivatization with 9‐fluorenylmethyl chloroformate

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Design and synthesis of a hydrophilic fluorescent derivatization reagent for carboxylic acids, 4‐N‐(4‐N‐aminoethyl)piperazino‐7‐nitro‐2,1,3‐benzoxadiazole (NBD‐PZ‐NH₂), and its application to capillary electrophoresis with laser‐induced fluorescence detection