The invention provides a preparation method of ZnCdSe/ZnS quantum dots. The method comprises the following steps that 1, a zinc source, a cadmium source, organic acid and/or organic amine and an organic solvent are stirred and heated to be dissolved after shielding gas is introduced to obtain a zinc and cadmium mixed pro-solution; 2, the solution is heated to 200-350 DEG C, and then a selenium source is injected into the solution within 30 s; 3, a sulfur source or sulfur and zinc source mixed solution is added drop by drop; 4, the temperature of 200-350 DEG C is kept constant, then cooling is performed to reach the room temperature, and separation and purification are performed to obtain ZnCdSe/ZnS quantum dots. The preparation method of the ZnCdSe/ZnS quantum dots is safety to implement, simple, controllable, low in cost, and capable of achieving repetition and amplification; the obtained quantum dots are uniform and controllable in size and appearance, the monodipserity is good, the fluorescence quantum yield is high, and the good stability on the high-temperature, washing and water dissolution modification and other conditions is good.