OBJECTIVE:To establish a method for the determination of 7 residual solvents (ethanol, n-hexane, benzene, toluene, xylene, styrene, divinylbenzene) in Liuwei dihuang glycoside. METHODS: The column was DB-624 capillary column, carrier gas was nitrogen, flow rate was 5.0 ml/min; detector was a hydrogen flame ionization detector with temperature of 250 ℃ (programmed temperature); equilibrium temperature was 80 ℃, sample loop temperature was 90 ℃, and transfer line temperature was 100 ℃; the equilibrium time of vial heating was 30 min, sample loop filling time was 0.05 min, injection time was 1.0 min; the carrier gas pressure was 95 kpa, and the vial pressure was 60 kpa. RESULTS: The linear range was 25-500 μg/ml for ethanol(r=0.998 7), 0.025-10 μg/ml for n-hexane (r=0.998 8),0.025-10 μg/ml for benzene (r=0.999 9), 0.1-40 μg/ml for toluene(r=1.000 0), 0.25-100 μg/ml for xylene(r=0.999 9),0.5-500 μg/ml for styrene(r=1.000 0) and 0.5-500 μg/ml for divinylbenzene (r=1.000 0); RSDs of precision, stability and reproducibility tests were lower than 4%; recoveries were 99.60%-102.70% (RSD=1.08%,n=9),90.70%-100.30%(RSD=4.51%,n=9),100.10%-109.80%(RSD=3.82%,n=9), 99.50%-110.00% (RSD=4.40%,n=9),100.00%-109.10%(RSD=3.50%,n=9), 93.40%-102.30%(RSD=3.73%,n=9) and 99.70%-101.70% (RSD=0.79%,n=9), respectively; the low limits of detection were 1.000, 0.025,0.025,0.025,0.100,0.025,0.250 μg/ml respectively. CONCLUSIONS: The method is simple, stable and reproducible, and can be used for the determination of residual solvents (ethanol, n-hexane, benzene, toluene, xylene, styrene, divinylbenzene) in Liuwei dihuang glycoside.
关键词
六味地黄苷糖顶空气相色谱法残留溶剂
Keywords
Liuwei dihuang glycosideHeadspace gas chromatographyResidual solvent