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A new method for the analysis of beta(2)-agonists in human urine by pressure-assisted capillary electrochromatography
Minghua Lu1, Lan Zhang, Xin Li
1Ministry of Education Key Laboratory of Analysis and Detection for Food Safety, Analytical and Testing Center, Fuzhou University, Fuzhou, Fujian, China.
Abstract:
A new pressure-assisted capillary electrochromatography coupled with electrospray ionization-mass spectrometry method using a silica-based monolithic column as separation media was developed for the analysis of beta(2)-agonists in human urine. Experimental conditions including the mobile phase, separation voltage, assisted pressure, and sheath liquid were optimized for the analysis: mobile phase composed of 82% (v/v) ACN and 18% (v/v) 20mmol/L ammonium acetate (pH 6.0); separation voltage 25kV; assisted pressure 2 bar; and the sheath liquid consisting of 7.5mmol/L acetic acid in isopropanol/water 50/50% (v/v) that was delivered at a flow rate of 3.0microL/min. Six beta(2)-agonists were separated within 12.5min with LODs (defined as S/N=3) in the range of 0.25-2.0ng/mL. The absolute LODs of the developed method for analyzing six beta(2)-agonists ranged from 5.75 to 46.0fg. Method repeatability of run-to-run and column-to-column was satisfactory. The recovery obtained from the analysis of spiked urine samples was between 88.2% and 106% with RSDs lower than 6.68%. The method was successfully applied to the analysis of real urine sample from volunteers.
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