Simultaneous Determination of 6 Residual Organic Solvents in Xingnaojing Injection by Headspace GC / 中国药房

ABSTRACT

OBJECTIVE:To establish the method for simultaneous determination of 6 residual organic solvents in Xingnaojing injection,such as methanol,ethanol,isopropanol,n-butanol,ethyl acetate and acetonitrile.METHODS:Headspace GC method was adopted.The determination was performed on DB-624 capillary column by temperature programming with the injector temperature of 200 ℃;flame ionization detector was adopted with the temperature of 250 ℃;carrier gas was nitrogen with flow rate of 25 mL/min and split ratio of 35 ∶ 1;headspace sampling size was 1 mL,and heating temperature of headspace sampling was 80 ℃;equilibrium time was 15 min.RESULTS:The linear ranges of methanol,ethanol,isopropanol,n-butanol,ethyl acetate and acetonitrile were 15.00-240.00 μg/mL (r =0.999 9),25.00-400.00 μg/mL (r =0.999 9),25.00-400.00 μg/mL (r =0.999 9),25.00-399.99 μg/mL(r=0.999 9),25.00-399.99 μg/mL(r=0.999 8) and 5.00-80.00 μg/mL(r=0.999 9).The LOQ were 5.98,3.94,2.05,2.13,1.39,1.24 μg/mL,and the LOD were 2.01,2.11,1.18,1.56,1.15,0.01 μg/mL,respectively.RSDs of precision tests were all less than 2.0％,stability and repetitive tests only ethyl acetate was detected,RSD＜2.0％;the recoveries were 93.59％-99.02％ (RSD=2.62％,n=6),92.42％-98.40％ (RSD=2.43％,n=6),94.81％-104.64％ (RSD=3.47 ％,n=6),94.56％-106.73％ (RSD=4.21％,n=6),97.04％-106.33％(RSD=3.50％,n=6)and 98.40％-107.97％ (RSD=3.37％,n=6).CONCLUSIONS:The method is specific,rapid,simple and accurate,and can be used for simultaneous determination of 6 residual organic solvents in Xingnaojing injection.