Solid-phase derivatization reactions for biomedical liquid chromatography

Krull, Ira S.; Szulc, Michael; Bourque, André J.; Zhou, Feng-Xiang; Yu, J.; Strong, Richard A.

doi:10.1016/0378-4347(93)e0437-u

Cited by 26 publications

(6 citation statements)

References 65 publications

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“…One of the most elegant proposals for the on-line determination of amphetamines in biological fluids is the employment of solid-phase extraction reagents, which was introduced by Krull and co-workers. 3,4 This approach is based on coupling a resinbased derivatization reagent to the analytical column. Controlled pore resins allow the direct injection of the samples and the exclusion of macromolecular matrix components.…”

Section: Introductionmentioning

confidence: 99%

“…Successful results have been reported for different tags such as 9-fluoreneacetyl, 3,5-dinitrobenzoyl, p-nitrobenzoyl and 9-fluorenylmethyl chloroformate (FMOC), among others. 3,4 However, this methodology has not gained wide acceptance, probably because of the difficulties in synthesizing the reagents, and also because of their limited stability. As an alternative, we have demonstrated the possibility of performing the derivatizations in an on-line mode by combining a (pre)column, packed with a conventional support (e.g., octadecylsilica), with the separation column.…”

Section: Introductionmentioning

confidence: 99%

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Automated trace enrichment for screening and/or determination of primary, secondary and tertiary amphetamines in biological samples by liquid chromatography

Herráez‐Hernández¹,

Campíns‐Falcó²

1999

Analyst

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A rapid and simple liquid chromatographic method for the automated determination of amphetamines in biological fluids was developed. The proposed procedure is based on the injection of 250 microL of sample into a 20 x 2.1 mm id precolumn (packed with a 30 microns Hypersil C18 stationary phase) for enrichment and purification of the analytes. Next, the analytes are transferred to a 5 microns LiChrospher 100 RP18, 125 x 4 mm id analytical column for their separation under reversed-phase conditions. Water was used to eliminate the matrix components from the precolumn and a 0.2 M phosphate buffer (pH 3) containing 2% triethylamine was the mobile phase for the resolution of the amphetamines. The UV detector was set at 210 nm. The method was applied to the determination of different primary, secondary and tertiary amphetamines in plasma and urine: beta-phenylethylamine, norephedrine, ephedrine, N-methylpseudoephedrine, pseudoephedrine, N-methylephedrine, amphetamine, 3-phenylpropylamine and methamphetamine. The method provides satisfactory linearity and reproducibility within the tested concentration range (1.0-10.0 micrograms mL-1) and limits of detection of 50-500 ng/mL-1.

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Automated trace enrichment for screening and/or determination of primary, secondary and tertiary amphetamines in biological samples by liquid chromatography

Herráez‐Hernández¹,

Campíns‐Falcó²

1999

Analyst

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“…Some other solid-phase derivatization methods have been reported. In these methods, the derivatization reagents were adsorbed or bonded to the solid support . When such methods were used for the derivatization of more hydrophilic analytes, such as amino acids and peptides, and for derivatization of drugs in direct biofluid injection, the detrimental side reaction with water still occurred.…”

Section: Resultsmentioning

confidence: 99%

Derivatization and Fluorescence Detection of Amino Acids and Peptides with 9-Fluorenylmethyl Chloroformate on the Surface of a Solid Adsorbent

et al. 2001

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An approach that exploits the surface of a solid adsorbent is proposed for precolumn FMOC derivatization of amino acids and peptides. Amino acids (Ser, Glu, GABA, Val, Phe, Lys) and two neuropeptides (substance P and Leuenkephalin) were adsorbed on alkaline silica gel cartridges. After drying, they were reacted with 9-fluorenyl-methyl chloroformate (FMOC-Cl) in toluene. After washing off the excess FMOC-Cl with ethyl acetate, the derivatives were eluted with aqueous eluant. The eluates were separated and detected by means of HPLC with fluorescence detection. Compared with the traditional derivatization in the liquid phase, the extent of formation of byproducts of FMOC-Cl with water was greatly decreased, and the excess FMOC-Cl was eliminated completely.

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“…[37][38][39][40][41] Other assays are based on the use of reagents attached to solid supports. 42,43 These materials effect sample clean-up and at the same time, or somewhat later, the reagent part of material is made to react with the analyte. However, the synthesis of the solid-phase reagent is often difficult, and its periodic regeneration is required to obtain a high yield, fewer side production, and reproducible results.…”

Section: Derivatizationmentioning

confidence: 99%

On-Line Coupling of Solid Phase Extraction Sample Processing with High-Performance Liquid Chromatography

Pyrzyńska

Poboży

2002

Critical Reviews in Analytical Chemistry

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Solid-phase derivatization reactions for biomedical liquid chromatography

Cited by 26 publications

References 65 publications

Automated trace enrichment for screening and/or determination of primary, secondary and tertiary amphetamines in biological samples by liquid chromatography

Automated trace enrichment for screening and/or determination of primary, secondary and tertiary amphetamines in biological samples by liquid chromatography

Derivatization and Fluorescence Detection of Amino Acids and Peptides with 9-Fluorenylmethyl Chloroformate on the Surface of a Solid Adsorbent

On-Line Coupling of Solid Phase Extraction Sample Processing with High-Performance Liquid Chromatography

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