Design and implementation of an automated liquid-phase microextraction-chip system coupled on-line with high performance liquid chromatography.
An automated liquid-phase microextraction (LPME) device in a chip format has been developed and coupled directly to high performance liquid chromatography (HPLC). A 10-port 2-position switching valve was used to hyphenate the LPME-chip with the HPLC autosampler, and to collect the extracted analytes, which then were delivered to the HPLC column. The LPME-chip-HPLC system was completely automated and controlled by the software of the HPLC instrument. The performance of this system was demonstrated with five alkaloids i.e. morphine, codeine, thebaine, papaverine, and noscapine as model analytes. The composition of the supported liquid membrane (SLM) and carrier was optimized in order to achieve reasonable extraction performance of all the five alkaloids. With 1-octanol as SLM solvent and with 25 mM sodium octanoate as anionic carrier, extraction recoveries for the different opium alkaloids ranged between 17% and 45%. The extraction provided high selectivity, and no interfering peaks in the chromatograms were observed when applied to human urine samples spiked with alkaloids. The detection limits using UV-detection were in the range of 1-21 ng/mL for the five opium alkaloids presented in water samples. The repeatability was within 5.0-10.8% (RSD). The membrane liquid in the LPME-chip was regenerated automatically between every third injection. With this procedure the liquid membrane in the LPME-chip was stable in 3-7 days depending on the complexity of sample solutions with continuous operation. With this LPME-chip-HPLC system, series of samples were automatically injected, extracted, separated, and detected without any operator interaction.
Department of Pharmacy, Faculty of Health and Medical Sciences, University of Copenhagen, Universitetsparken 2, 2100 Copenhagen, Denmark.
Bin
B
Li
Department of Pharmacy, Faculty of Health and Medical Sciences, University of Copenhagen, Universitetsparken 2, 2100 Copenhagen, Denmark. Electronic address: nickolaj.petersen@sund.ku.dk.
Nickolaj Jacob
NJ
Petersen
Department of Analytical Chemistry, Faculty of Chemistry, University of Seville, P.O. Box 41012, Seville, Spain.
María D Ramos
MD
Payán
Department of Pharmacy, Faculty of Health and Medical Sciences, University of Copenhagen, Universitetsparken 2, 2100 Copenhagen, Denmark.
Steen Honoré
SH
Hansen
Department of Pharmacy, Faculty of Health and Medical Sciences, University of Copenhagen, Universitetsparken 2, 2100 Copenhagen, Denmark; School of Pharmacy, University of Oslo, P.O Box 1068 Blindern, 0316 Oslo, Norway.
Stig
S
Pedersen-Bjergaard
D000470:Alkaloids / Q000302:isolation & purification* / Q000652:urine*; D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation*; D004867:Equipment Design; D006801:Humans; D057230:Limit of Detection; D059627:Liquid Phase Microextraction / Q000295:instrumentation*; D046210:Microfluidic Analytical Techniques / Q000295:instrumentation; D009892:Opium / Q000737:chemistry
D000470:Alkaloids; D009892:Opium
Automated liquid-phase microextraction; High performance liquid chromatography; Microfluidic chip; On-line sample pretreatment; Opium alkaloids