Abstract: The mass spectrometry param eters for determine diethylstilbestrol, malachite green, leumalachite green was optimized and a high-performance liquid chromatography-mass spectrometry method was established for the determination of three compounds. The results showed that such a method had the advantages of time-saving, with high sensitivity and accuracy, and it was suitable for quantitative analysis of diethylstilbestrol, malachite green, leumalachite green at same time,especially suitable for large quantities of samples.