GC法同时测定蒙药扎冲十三味丸中4种挥发性成分的含量

Simultaneous determination of Mongolian medicine Zhachong-shisanwei pills by GC The content of four volatile components in the laboratory

目的:建立同时测定蒙药扎冲十三味丸中丁香酚、β-细辛醚、麝香酮及去氢木香内酯含量的气相色谱法。方法:采用HP-5MS毛细管色谱柱(30 m×0.32 mm×0.25μm),检测器为FID检测器,进样口温度220℃,检测器温度为250℃。柱温初始温度为50℃,维持1 min之后以10℃·min^(-1)的速率上升至120℃,维持1 min,再以20℃·min^(-1)的速率上升至250℃,维持1 min;载气为氮气,流速为1 mL·min^(-1),分流进样,分流比为10∶1;进样量为1μL,氢气流速为20 mL·min^(-1);空气流速为400 mL·min^(-1);尾吹气流速为25 mL·min^(-1)。结果:丁香酚、β-细辛醚、麝香酮及去氢木香内酯检测质量浓度线性范围分别为0.02796~0.16776μg·μL^(-1)(r=0.9997)、0.0059~0.0354μg·μL^(-1)(r=0.9994)、0.0109~0.0654μg·μL^(-1)(r=0.9997)、0.0025~0.015μg·μL^(-1)(r=0.9998),在此范围内线性良好;平均回收率分别为97.28(RSD=2.97%)、108.34(RSD=1.75%)、99.99(RSD=2.65%)、96.18(RSD=3.01%)。结论:该方法有效可靠,可用于蒙药扎冲十三味丸中丁香酚、β-细辛醚、麝香酮及去氢木香内酯的含量测定。

Objective:To establish a gas chromatography method for the simultaneous determination of eugenol,β-asarone,muskone and dehydroxylolactone in Zhachong-13wei pills.Methods:HP-5MS capillary column(30 m×0.32 mm×0.25μm)was used for chromatographic analysis.The detector was FID detector.The temperature of injection nozzle was220℃,and the temperature of detector was 250℃.The initial column temperature was 50℃,and then increased to 120℃at a rate of 10℃·min^(-1)for 1min,and then increased to 250℃at a rate of 20℃·min^(-1)for 1min.The carrier gas was nitrogen,the flow rate was 1 mL·min^(-1),and the split injection ratio was 10∶1.The injection volume was 1μL,and the flow rate of hydrogen was 20 mL·min^(-1).The air flow rate was 400 mL·min^(-1);The tail blowing flow rate was 25 mL·min^(-1).Results:The ranges of eugenol,β-asarone,muskone and dehydroxylolide were 0.02796~0.16776μg·μL^(-1)r=0.9997),0.0059~0.0354μg·μL^(-1)r=0.9994),0.0109~0.0654μg·μL^(-1)r=0.9997),and 0.0025~0.015μg·μL^(-1)r=0.9998),respectively.The average recoveries were 97.28(RSD=2.97%),108.34(RSD=1.75%),99.99(RSD=2.65%)and 96.18(RSD=3.01%),respectively.Conclusions:The method is effective and reliable,and can be used for the content determination of eugenol,β-asarone,muskone and dehydroxylolactone in Zhachong-shisanwei pills.