Derivatization of ethylene dibromide with silica-supported silver picrate for improved high-performance liquid chromatographic detection

Colgan, Stephen T.; Krull, Ira S.; Dorschel, C.; Bidlingmeyer, Brian A.

doi:10.1021/ac00125a004

Cited by 13 publications

(3 citation statements)

References 29 publications

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“…Most analysts assume that percent derivatizations are totally independent of concentration of the substrate and whether the amine substrates are derivatized together or separately. For solid-phase reagents, it has been shown that, at least for one particular silica-adsorbed reagent, percent derivatizations can change drastically with changes in substrate concentration (26). For other reagents, as here, such drastic differences were not observed.…”

Section: Characterization Of Synthesized External Standardsmentioning

confidence: 52%

Polymeric activated ester reagents for off-line and on-line derivatizations of amine nucleophiles in high-performance liquid chromatography with ultraviolet and fluorescence detection

Gao¹,

Chou²,

Krull³

1989

Anal. Chem.

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A novel polymeric activated ester reagent has been developed that improves final detectability and chromatographic performance in high-performance liquid chromatography (HPLC) for virtually all primary and secondary amines or amine analogues. This has involved the synthesis, characterization of final reagent, optimization of derivatization and separation conditions, and determination of analytical figures of merit. The polymeric reagent contained an activated ester linkage to the 9-fluorenyl group, which imparted ultraviolet (UV) and fluorescence (FL) detector properties to the final derivatives. Kinetic studies of these solid-phase (heterogeneous) reactions have been conducted, and specific rate constants were compared with those of the analogous solution reaction for the same substrates. Percent derivatizations have reached 90% and 70% for primary and secondary amines, respectively, under optimized conditions. High reaction reproducibility has been obtained by using the on-line approach, for more than 50 separate injections of the same amine substrate with a single solid-phase reactor. These solid-phase derivatizations have led to detection limits for typical amines in the low-parts-per-billion range. The final, overall methods can provide rapid, automatable, accurate, and precise detection and quantitation of primary/secondary amines and amine-like compounds in real-world sample matrices. As an illustrative example, amphetamine spiked in urine has been derivatized off-line and on-line, with minimum sample preparation, and detected via HPLC-UV/FL with acceptable accuracy and precision.

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Section: Characterization Of Synthesized External Standardsmentioning

confidence: 52%

Polymeric activated ester reagents for off-line and on-line derivatizations of amine nucleophiles in high-performance liquid chromatography with ultraviolet and fluorescence detection

Gao¹,

Chou²,

Krull³

1989

Anal. Chem.

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“…Finegrained fractions of commercial GC packings are employed for preparation of micropacked columns [ 7-10] and commercial sorbents usually used for HPLC have also been used 18, [11][12][13][14][15][16]. A simple and fast method for preparation of short capillary columns packed with solid phase extraction (SPE) sorbents is presented.…”

Section: Introductionmentioning

confidence: 99%

Gas chromatographic analysis of simple mixtures of lower aliphatic and aromatic hydrocarbons on micropacked glass capillary columns

Komárek

1993

J. High Resol. Chromatogr.

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Short CommunicationsNHC4H9). The PCI mass spectrum obtained with methane as reagent gas yielded a molecular ion peak at m/z 217 (M + 1) as the base peak. Other characteristic peaks were also discernible at m/z 245 (M + 29) and 257 (M + 41) ( Figure 3B). Selective ion monitoring (SIM) could be used to quantify 1.0 ng of the derivative.The efficacy of the derivatization reaction for the quantification of the amines was examined using n-butylamine. Comparison with the authentic standard showed that under optimized conditions the yield of BuInA was nearly quantitative. Detection response to BA (as the indolyl derivative) was linear up to 20 pg/ml. The minimum detectable concentration of BA after reaction with an excess of P-2-InAn was 0.05 pg/ml when quantified by the dual detection system.

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“…It is only within the past 10 years that analytical chemists have been attracted to the possible uses of solid-phase reagents for improved derivatizations related to HPLC. We and others have described the significant advantages possible in using this newer approach to achiral derivatizations in analytical chemistry and HPLC (30)(31)(32)(33)(34)(35)(36)(37).…”

Section: Introductionmentioning

confidence: 99%

Chiral polymeric reagents for off-line and on-line derivatizations of enantiomers in high-performance liquid chromatography with ultraviolet and fluorescence detection: an enantiomer recognition approach

Chou¹,

Gao²,

Grinberg³

et al. 1989

Anal. Chem.

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Optically active and detector-sensitive polymeric reagents have been synthesized, loadings determined, derivatizations/separations/detection optimized, and applications to simple amines and amino alcohols described. Such reagents have been designed to contain different chiral centers, usually amino acids, leashed via an activated ester attachment to an insoluble, structurally rigid, organic polymer backbone. 9-Fluorenylmethyl (FMOC) moieties chemically bonded to the amino acids were used as ultraviolet (UV) and fluorescence (FL) sensitive detector probes to the final diastereomers of enantiomer substrates. Such diastereomers can be readily separated by isocratic or gradient elution normal-phase methods. The kinetics for diastereomer formation have been determined, and final UV/FL responses for known mixtures of enantiomers have been compared to demonstrate overall validity of the method. Minimum detection limits, linearity of calibration plots, dual detector responses, and linear diode array spectra and absorbance ratios have also been demonstrated. In some cases, authentic standards have been prepared to calculate absolute percent derivatizations for specific enantiomer pairs. The overall approach permits, for the very first time, off-line or on-line precolumn derivatization for the formation of diastereomers having unique detector properties. It has been proven that the rates and rate constants for such formations are identical for at least those pairs of enantiomers studied. Separations are base-line or near-base-line, permitting accurate and precise quantitative determinations, by both UV and FL, of enantiomer/optical purity and chemical purity.

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Derivatization of ethylene dibromide with silica-supported silver picrate for improved high-performance liquid chromatographic detection

Cited by 13 publications

References 29 publications

Polymeric activated ester reagents for off-line and on-line derivatizations of amine nucleophiles in high-performance liquid chromatography with ultraviolet and fluorescence detection

Polymeric activated ester reagents for off-line and on-line derivatizations of amine nucleophiles in high-performance liquid chromatography with ultraviolet and fluorescence detection

Gas chromatographic analysis of simple mixtures of lower aliphatic and aromatic hydrocarbons on micropacked glass capillary columns

Chiral polymeric reagents for off-line and on-line derivatizations of enantiomers in high-performance liquid chromatography with ultraviolet and fluorescence detection: an enantiomer recognition approach

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