Literature to read:
Evans, Charles R.; Jorgenson, James W.. Multidimensional LC-LC and LC-CE for high-resolution separations of biological molecules. Analytical and Bioanalytical Chemistry (2004), 378, 1952-1957(NB)
Pitarch, Elena; Hernandez, Felix; ten Hove, Jan; Meiring, Hugo; Niesing, Willem; Dijkman, Ellen; Stolker, Linda; Hogendoorn, Elbert. Potential of capillary-column-switching liquid chromatography-tandem mass spectrometry for the quantitative trace analysis of small molecules. Application to the on-line screening of drugs in water. Journal of Chromatography, A (2004), 1031, 1-9
Holm,A; Large volume injection in capillary LC (part of PhD thesis 2004) - a copy will be provided at the lecture.
Holm, A.; Molander, P.; Lundanes, E.; Greibrokk, T. Determination of rotenone in river water utilizing packed capillary column switching liquid chromatography with UV and time-of-flight mass spectrometric detection. Journal of Chromatography, A (2003), 983, 43-50.
Holm, Anders; Molander, Paal; Lundanes, Elsa; Ovrebo, Steinar; Greibrokk, Tyge. Fast and sensitive determination of urinary 1-hydroxypyrene by packed capillary column switching liquid chromatography coupled to micro-electrospray time-of-flight mass spectrometry. Journal of Chromatography, B: Analytical Technologies in the Biomedical and Life Sciences (2003), 794, 175-183.
Holm, Anders; Solbu, Kasper; Molander, Paal; Lundanes, Elsa; Greibrokk, Tyge. Sensitive biomonitoring of phthalate metabolites in human urine using packed capillary column switching liquid chromatography coupled to electrospray ionization ion-trap mass spectrometry. Analytical and Bioanalytical Chemistry (2004), 378, 1762-1768.
Laboratory exercises and evaluation:
The supervisor will show the student the set-up of a micro column switching with UV deteksjon. The student will under supervison test the system using a test mixture of compounds and the conditions provided by the supervisor (method 1). Thereafter, the student is given a new test mixture, and the student must find the appropriate conditons to focus the componds on the precolumn and separate the compounds on the analytical column. To pass the module, the student must show that the method can be used to inject up to 500 ?L without breakthrough and without loss in efficiency (compared with the efficiency found in method 1). The repeatability of retention times and peak area must be better than 3% RSD (n > 3). At the end of the module, the student will be examined with regard to choosing capillary dimensions, stationary phases, mobile phases and injection volume and other theoretical subjects, to control that the student can relate theoretical and practical knowledge. Additionally, a 1-2 pages report must be written and approved to pass the module.
Schedule:
The module starts with a 2 hrs lecture Thursday Oct. 27 at 10.15 (?108). Thereafter, all activites will take place in the laboratory (?U118 or ?122).
Requirements:
You must have taken KJM4420 or KJM3420 (or an equivalent course) to participate in this module.
To be able to take this module, you must have taken module no. 7.