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Two new simultaneous spectrophotometric methods for determination of Olanzapine and Ephedrine depend on third (D3) and fourth (D4) derivative of zero spectrum of two drugs were developed. The peak â€“ to- base line, peak to peak and area under peak were found proportional with concentration of the drugs up to (4-24 Âµg/ml-1) at known experimental wavelengths. The results showed that the method was precise and accurate through RSD% (0.5026-4.0273),( 0.2399 6.9888) and R.E %(-2.3889-0.8333) ,) -2.9444-0.2273) while the LOD (0.0057- 0.8510 Î¼g.ml-1), ( 0.0953-0.9844 Î¼g.ml-1) and LOQ (0.0173- 2.5788Î¼g.ml-1),( 0.5774-2.9829 Î¼g.ml-1) were found for the two drugs respectively. The methods were applied ide to the determination of Olanzapine and Ephedrine in pharmaceutical preparations successfully.