A novel chemiluminescence micro-total analytical system (μTAS) is described for the determination of atropine and pethidine. Reagents were moved though the 200-μm wide channels of a glass chip using a negative pressure pumping system. Linear calibrations were obtained for the system over three-orders of magnitude, with detection limits of 3.8x10 - 9 and 7.7x10 - 8 M, respectively for atropine and pethidine and R.S.D. of <5%. This is the first report on the use of μTAS to determine atropine with chemically oxidised tris (2,2'-bipyridine)ruthenium(II) chemiluminescence.