A novel method was developed for the determination of chlorocholine chloride（CCC） and mepiquat chloride（MQ） residues in soil and irrigation water based on SPE/HPLC-MS/MS technique.To investigate their enrichment efficiencies to CCC and MQ，4 kinds of SPE columns were used to pretreat samples，including silica gel column,C18 column and weak cation exchange(WCX) column.The results showed that the highest efficiency was obtained by using WCX column with 5 mL of 10 mmol/L ammonium acetate(containing 0.1% formic acid) -methanol(1∶9) as elution.The separations of analytes were performed on a HILIC column（1.7 μm，2.1 mm×50 mm） by a gradient elution using acetonitrile-10 mmol/L ammonium acetate(containing 0.1% formic acid) as moblile phase.The mean recoveries of CCC and MQ were in the range of 73%-91% and 76%-90%,respectively,with RSDs of 8.2%-12.4% and 42%-13.2%,respectively.The calibration curves of CCC and MQ were linear in the range of 1.0-50.0 μg/L with correlation coefficients more than 0.999.The detection limits of CCC and MQ both were 0.125 μg/kg for soil samples and 0.02 μg/L for water samples.The method was applied in the real soil and water samples from Karashahr area，Xinjiang，and no CCC and CQ were detected.The method was reliable，robust and sensitive for the determination of CCC and CQ in soil and water samples.