Page 39 - Modern Derivatization Methods for Separation Sciences

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Derivatization: Saponification of CrEL in alcoholic KOH and derivatization with 1-naphthylamine

Clean-up: Liquid-liquid extraction

Detection: UV 280 nm

Analytical parameters: LOQ, 0.01% (v/v); percentage deviation, <8%; precision, <7%.

Busulfan in human plasma [28].
Derivatization: Precolumn derivatization with sodium diethyldithiocarbamate

Clean-up: Liquid-liquid extraction

Detection: UV detection, 251 nm

Analytical parameters: Range, 60-3000 ng/ml; limit of detection, 20 ng/ml (signal-to-noise ratio of 6);
coefficients of variance, 4.41-13.5%; mean derivatization and extraction yield, 93.4-107%.

Anticholesteremic Agents

Simvastatin and its active metabolite in human plasma [29].

Derivatization: Esterification with 1-bromoacetylpyrene in the presence of 18-crown-6

Clean-up: C8 and phenylboronic acid solid-phase extraction and column-switching

HPLC Detection: Fluorescence

Analytical parameters: Range, 0.1-10 ng/ml; C. V.%(Intra-day),<11.0%; accuracies, 91.7-117%.

Antihypertensive Agents

Captopril in human plasma and urine [30].

Derivatization: The first method, precolumn derivatization of captopril with the fluorescent label
monobromobimane (MBB); the second method, postcolumn reaction with the fluorescent reagent
ophthaldialdehyde (OPA)

Clean-up: Protein precipitation and reducing disulfide bond with tributylphosphine for total captopril
analysis

Detection: Fluorescence

Analytical parameters: In plasma, LOQ, 12.5 ng/ml; for the MBB method (limit of detection 30 pg) and
25 ng/ml; for the OPA method (limit of detection 50 pg); in urine, LOQ, 250 ng/ml (limit of detection
50 pg).

Propranolol and 4-hydroxypropranolol in human plasma [31].

Derivatization: Diastereomeric derivatization with 2,3,4,6-tetra-Oacetyl-beta-glucopyranosyl
isothiocyanate

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