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J Chromatogr A. 1998 Oct 9;823(1-2):401-9.

Automated sample preparation for the determination of budesonide in plasma samples by liquid chromatography and tandem mass spectrometry.

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Department of Bioanalytical Chemistry, Preclinical R&D, Lund, Sweden.


An automated bioanalytical method for the determination of the glucocorticosteroid drug budesonide in plasma samples at pM levels was investigated. The method was built using three separate automated analytical steps with manual transfer of samples between them. In the first step, a Tecan RSP150 (Genesis) pipetting robot was used to transfer 1 ml of centrifuged plasma samples and deuterated budesonide internal standard solutions into tubes and to homogenise the resulting admixture. In the second step, a solid-phase extraction was performed using an ASPEC Xli (Gilson) with 100 mg Isolute C18 columns. In order to avoid conventional time-consuming evaporation and reconstitution steps, the solid-phase extraction was coupled on-line to a trace enrichment system for further purification and concentration of the sample extracts. The concentrated samples were eluted in 300 microliters ethanol into injection vials, which were capped and transferred to the autosampler in the detection system. In the third step, the pre-treated samples were chromatographed in a gradient LC system and detected using a tandem MS system (Finnigan TSQ 7000), with an atmospheric pressure chemical ionisation interface. The described Analytical System consisting of one Tecan robot, two ASPEC systems and one LC-MS-MS system may analyse up to about 800 samples a week with less routine work for the analyst. The concentration range studied was 15 to 2500 pM in 1 ml spiked plasma samples and the limit of quantitation for the described method was determined as 15 pM, as defined by accuracy and precision better than 20%.

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