Microemulsion High Performance Liquid Chromatography (MELC) for Determination of Terbutaline in Urine Samples
Althanyan, Mohammed S. Nasser, A. Assi, H. Clark, Brian J. Assi, Khaled H.
Althanyan, Mohammed S.
Nasser, A.
Assi, H.
Clark, Brian J.
Assi, Khaled H.
Publication Date
2016-02
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2015-10-10
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Abstract
An isocratic oil-in-water microemulsion High Performance Liquid Chromatography (MELC) was developed and validated for the
determination of terbutaline in urine samples. A solid phase extraction (SPE) method which used Oasis HLB cartridges was optimised
to isolate terbutaline from a urine matrix followed by HPLC with fluorescence detection. The urinary assay was performed in
accordance with FDA and ICH regulations for the validation of bioanalytical samples. The method uses the isocratic oil-in-water
micro emulsion to separate the terbutaline from the endogenous urine components. The chromatographic separation was carried
out on C18-Spherisorb (250mm×4.6mm) analytical column maintained at 30 °C. The mobile phase was 94.4% aqueous
orthophosphate buffer (adjusted to pH 3 with orthophosphoric acid), 0.5% ethyl acetate, 1.5% Brij35, 2.5% 1-butanol and 1.1%
Octanesulfonic acid (OSA), all w/w. The terbutaline peak was detected by fluorescence detection, using excitation and emission
wavelengths of 267 and 313 nm, respectively. The linearity of response was demonstrated at six different concentrations of
terbutaline which were extracted from spiked urine, ranging from 60 to 1000ng/ml. The terbutaline was extracted from urine by a
solid phase extraction clean-up procedure on Oasis HLB cartridges, and the relative recovery was >87.64% (n = 5). The limit of
detection (LOD) and limit of quantitation (LOQ) in urine were 20.21 and 61.24ng/ml, respectively. The intra-day and inter-day
precisions (in term of % coefficient of variation) were <3.56% and <2.87%, respectively. In the method development the influence of
the composition of the microemulsion system was also studied and the method was found to be robust with respect to changes of
the microemulsion components.
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Althanyan MS, Nasser A, Assi H et al (2016) Microemulsion High Performance Liquid Chromatography (MELC) for Determination of Terbutaline in Urine Samples. International Journal of Pharmaceutical Sciences Reviews and Research. 36(1): 288-282.
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