GC同时测定麝香通心滴丸中龙脑、异龙脑和麝香酮的含量

Simultaneous Determination of Borneol, Isoborneol and Muscone in Shexiang Tongxin Dripping Pills by GC

关键词:  气相色谱法  麝香通心滴丸  龙脑  异龙脑  麝香酮

Key words:  GC  Shexiang Tongxin Dripping pills  borneol  isoborneol  muscone

摘要:

目的 建立同时测定麝香通心滴丸中龙脑、异龙脑及麝香酮含量的气相色谱法。方法 采用HP-5MS毛细管色谱柱（30 m×0.32 mm，0.25 μm），检测器为FID检测器，检测器温度为250℃，进样口温度220℃。柱温以100℃为初始温度，保持2 min，以2℃·min^-1升温至110℃，保持3 min，以50℃·min^-1升温至205℃，保持7 min，以20℃·min^-1升温至250℃，保持2 min；载气为氮气，流速为1 mL·min^-1；进样方式为分流进样，分流比为10：1；进样量为1 μL，以萘为内标。结果 龙脑、异龙脑、麝香酮的浓度分别在0.054 68~0.437 4 mg·mL^-1（r=0.999 9），0.070 67~0.565 4 mg·mL^-1（r=0.999 9），0.004 512~0.036 10 mg·mL^-1（r=0.999 7）内线性良好；平均回收率分别为97.91%（RSD=2.05%），100.79%（RSD=2.78%），105.36%（RSD=3.78%）。结论 该方法有效可靠，可用于麝香通心滴丸中龙脑、异龙脑和麝香酮的含量测定。

Abstract:

OBJECTIVE To establish a GC method for the simultaneous determination of borneol, isoborneol and muscone in Shexiang Tongxin Dripping Pills. METHODS Sample of Shexiang Tongxin Dripping pills were determined by HP-5MS capillary column(30 m×0.32 mm, 0.25 μm). FID was used as detector with a temperature of 250℃, and the inlet temperature was 220℃. The column temperature was programmed to start at 100℃ maintained for 2 min, rised to 110℃ at a rate of 2℃·min^-1, maintained for 3 min, and then rised to 205℃ at a rate of 50℃·min^-1, maintained for 7 min, and then rised to 250℃ at a rate of 20℃·min^-1 maintained for 2 min. Nitrogen(1 mL·min^-1) was used as the carrying gas, and the split ratio was 10:1. The injection volume was 1 μL and naphthalene was used as internal standard. RESULTS The linear ranges of borneol, isoborneol and muscone were 0.054 68-0.437 4 mg·mL^-1(r=0.999 9), 0.070 67-0.565 4 mg·mL^-1(r=0.999 9), 0.004 512-0.036 10 mg·mL^-1(r=0.999 7), respectively. The average recovery rates(n=6) were 97.91%(RSD=2.05%), 100.79% (RSD=2.78%), 105.36%(RSD=3.78%), respectively. CONCLUSION This method is reliable and accurate, which can be used for the determination of borneol, isoborneol and muscone in Shexiang Tongxin Dripping Pills.