The invention provides a method for determining total fluorine compound precursor substances in an atmospheric particulate matter sampling filter membrane; the method comprises the following steps of1) extracting a sample: carrying out ultrasonic extraction on the atmospheric particulate matter sampling filter membrane, and collecting to obtain an extracting solution; 2) purification of the sample: carrying out purifying, concentrating and purifying on the extracting solution obtained in the step 1) to obtain a sample detection solution; and 3) determination of the sample: detecting the sample detection solution obtained in the step 2) by adopting an ultra-high performance liquid phase chromatography-triple quadrupole series mass spectrometer, and obtaining the content of the total fluorine compound precursor substance by adopting an internal standard method. The invention belongs to the technical field of environmental monitoring, and by virtue of the provided measurement method, full extraction and measurement of six kinds of total fluorine compound precursor substances, such as 4:2FTS and the like in the atmospheric particulate matter sampling filter membrane can be realized, the separation effect is good, and the detection efficiency is improved; and the method has the advantages of being accurate in measurement result, high in repeatability, high in sensitivity, high in recovery rate, low in detection limit, high in substrate interference resistance and the like.