The invention provides a determination method for 2-chloromethyl-3,5dimethyl-4-methoxyl pyridine hydrochloride and belongs to an acidimetric non-aqueous titration method. The method comprises the following steps: by taking N-N-dimethylformamide as a titration solvent, a thymol blue absolute methanol solution as an indicator and lithium methoxide as a titrating solution, titrating until the blue color appears and calculating the content of 2-chloromethyl-3,5 dimethyl-4-methoxyl pyridine hydrochloride in a sample according to the consumed volume of the titrating solution, the concentration of the titrating solution and the sampling weighing amount of the sample. The method provided by the invention is one of the mainstream analytical methods. The method has the characteristics of being remarkable in finish point which is easy to judge, good in precision, high in accuracy and the like, can be used for accurately detecting the content of the 2-chloromethyl-3,5 dimethyl-4-methoxyl pyridine hydrochloride, and is simple, economic and rapid.