OBJECTIVE：To establish a method for the determination of organic residues of benzene， toluene， p-xylene， o-xylene， styrene， 1，2-diethylbenzene and divinylbenzene in Xueshuantong for injection （freeze-dried）. METHODS：HS-GC-MS/MS was performed on the column of HP-INNOWAX capillary column by programmed temperature， the detector was MS， injector temperature was 180℃， carrier gas was helium at a flow rate of 1.5 ml/min， and the split ratio was 2 ∶ 1， headspace bottle equilibrium temperature was 80 ℃， equilibrium time was 30 min； injection way was headspace， sample volume was 20 ml， and the injection volume was 1 ml； MS detector mwas selected ion monitoring， ionization was EI， ionization voltage was 70 eV， interface temperature was 250 ℃，ion source temperature was 230 ℃， and quadrupole temperature was 150 ℃. RESULTS： The linear range was 0.020 8-0.832 0 μg/ml for benzene（r＝0.999 4），0.107 4-4.297 6 μg/ml for  toluene（r＝0.999 5）， 0.088 5-3.539 2 μg/ml for p-xylene（r＝0.999 5）， 0.104 5-4.128 0 μg/ml for o-xylene（r＝0.999 7），0.103 2-4.128 0 μg/ml for styrene（r＝0.999 8），0.090 9-3.635 2 μg/ml for 1，2-diethylbenzene （r＝0.999 6） and 0.096 0-3.840 0 μg/ml for divinylbenzene（r＝0.999 5）； RSDs of precision， stability and reproducibility tests were lower than 5％； recoveries were 91.85％-99.06％（RSD＝2.6％，n＝6），96.46％-102.56％（RSD＝2.2％，n＝6），101.49％-106.98％（RSD＝2.0％，n＝6），95.91％-101.73％（RSD＝2.2％，n＝6）， 93.40％-101.85％（RSD＝3.1％，n＝6）， 103.11％-111.82％（RSD＝2.9％，n＝6）， and 87.58％-94.66％（RSD＝3.5％，n＝6）， respectively. CONCLUSIONS： The method is simple， rapid and accurate， and can be used for the determination of organic residues of benzene， toluene， p-xylene， o-xylene， styrene， 1，2-diethylbenzene and divinylbenzene in Xueshuantong for injection （freeze-dried）.