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[Rapid analysis of terbutaline by combined solid phase extraction/liquid chromatography tandem mass spectrometry]
X Y Chen1, H Y Yang, D F Zhong
1Laboratory of Drug Metabolism and Pharmacokinetics, Shenyang Pharmaceutical University, Shenyang 110016, China.
Aim:
To develop a liquid chromatography-electrospray ionization tandem mass spectrometry method for rapid analysis of terbutaline at level of 50 pg.mL-1 in human plasma.
Methods:
Samples containing terbutaline and salbutamol (internal standard, IS) were extracted using C18 solid-phase extraction cartridges, followed by liquid chromatographic separation and mass spectrometric detection. The mobile phase consisted of acetonitrile-water-formic acid (20:80:1), at a flow-rate of 0.4 mL.min-1. Selected reaction monitoring with mass transitions m/z 226-->151 and m/z 240-->148 were used for terbutaline and IS, respectively.
Results:
The chromatographic analysis time for each sample was approximately 3.8 min. The assay was linear from 0.05 to 8.0 ng.mL-1. The between-run precision and accuracy of the quality controls (QCs, 0.1, 0.4 and 4.0 ng.mL-1) were characterized by relative standard deviation (RSD) of 2.5% to 7.1% and relative errors of -3.1% to 5.7%, respectively. The within-run precision of QCs was characterized by RSD of 4.2% to 6.6%. This method was applied to the analysis of samples taken up to 60 h after oral administration of 10 mg bambuterol in healthy volunteers.
Conclusion:
The method is shown to be suitable for clinical investigation of terbutaline pharmacokinetics, which offers advantages of specificity, speed, and greater sensitivity over previously reported methods.