ELSEVIER Journal of Chromatography A, 729 (1996) 125-136
JOURNALOF
CHROMATOGRAPHY A
Fully automated determination of selective retinoic acid receptor
ligands in mouse plasma and tissue by reversed-phase liquid
chromatography coupled on-line with solid-phase extraction
a,~ C
H.M.M. Arafa , F.M.A. Hamada b, M.M.A. Elmazar, H. Nau a
~'htstitut f iir Toxikologie und Embryopharmakologie, Freie Universitiit Berlin, Garystrasse 5, D-1419.5 Berlin, Germany
hPharmacy College, AI-Azhar University, Cairo, Egypt
~Pharmacy College, King Saud Universi~, Riyadh, Saudi Arabia
Abstract
A fully automated reversed-phase HPLC method was developed for the quantitative assay of three retinoids (Am-580,
CD-2019 and CD-437) which selectively activate the retinoic acid receptors RARa, RARfl and RART, respectively. Mouse
plasma, embryo and maternal tissues were prepared for injection by on-line solid-phase extraction (SPE) and valve-switching
techniques. Following automatic injection, the sample was loaded on preconditioned disposable cartridges, cleaned-up and
then transferred onto the analytical column to be eluted in the backflush mode, separated by gradient elution and detected by
UV, while a new cartridge was concomitantly conditioned. The overall recovery was quantitative allowing for external
standardization. The calibration curves were linear in all biological samples tested so far, with a correlation coefficient (r)
>0.99. The intra-day precision was -<7.8% (n=5-6) and the inter-day variability was -<9.4% (n=3). The lower limit of
detection was 2.5 ng/ml or ng/g for CD-2019 and CD-437, and 5 ng/ml for Am-580 with a S/N ratio of 5 using a sample
weight of 25/.d or mg. The method is now in routine use in our laboratory for the assessment of the pharmacokinetic profiles
of these retinoids. The small sample size required, the simple sample prepration and the rapid analysis with high degree of
automation make this method convenient for microanalysis of biological samples both in animal and human studies.
Keywords: Sample preparation; Retinoids; Retinol
1. Introduction
Retinoids, natural and synthetic analogs of vitamin
A alcohol (retinol; ROH), are implicated in a wide
variety of key biological processes including cell
growth and differentiation, embryogenesis and epi-
thelial homeostasis [1,2]. Clinically, retinoids have
proven efficacy in the treatment of dermatological
diseases such as acne, psoriasis and photoaged skin
*Corresponding author.
[3,4], as well as in certain malignancies [5]. The
molecular mechanisms of such compounds are
thought to be mediated, for the most part, through
regulation of gene expression by two subclasses of
nuclear retinoic acid receptors RARs and RXRs
[6,7]. Both of these subclasses contain three receptor
subtypes arbitarily designated a, fl, and y, which are
encoded by separate genes [8[.
The clinical usefulness of retinoids is limited by a
number of side effects such as bone and lipid
toxicities [9], and teratogenicity [10,11]. Therefore,
new retinoid congeners with superior therapeutic
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