OBJECTIVE： To establish a method for the determination of drug loading and encapsulation efficiency of Epirubicin hydrochloride-sorafenib-loaded Polylactic Acid-glycolic Acid Polymer （PLGA） embolic microspheres. METHODS： HPLC method was adopted to determine the contents of epirubicin hydrochloride and sorafenib in the preparation， and then drug loading and encapsulation efficiency were calculated by formula. The determination was performed on Phenomenex Luna 5u C8（2） 100A column with mobile phase consisted of methanol-water （containing 0.05％ trifluoroacetic acid and 0.14％ dium dodecyl sulfate） （75 ∶ 25，V/V） at the flow rate of 1.0 mL/min. The detection wavelength was set at 252 nm， and the column temperature was maintained at 25 ℃. The injection volume was 10 μL. RESULTS： The linear ranges were 2.020-101.00 μg/mL for epirubicin hydrochloride （r＝0.999 8） and 2.048-102.40 μg/mL for sorafenib （r＝0.999 7）， respectively. The limits of quantification were 3.297 0， 2.546 8 μg/mL， respectively. The detection limits were 0.989 1， 0.764 1 μg/mL， respectively. RSDs of precision， stability and repeatability tests were all less than 2.0％. The recoveries were 96.41％-101.80％（RSD＝1.64％，n＝9）， 99.46％-101.45％（RSD＝0.70％，n＝9）， respectively. Drug loading of two components in 3 batches of samples were no lower than 1.17％，encapsulation efficiency no lower than 58％. CONCLUSIONS： The method is simple， accurate， can be used to determine drug loading and encapsulation efficiency of Epirubicin hydrochloride-sorafenib PLGA embolic microspheres.