GC测定止咳丸中(-)薄荷酮和薄荷脑的含量

Determination of (-)menthone and menthol in Coughpill by GC

关键词:  气相色谱法  止咳丸  (-)薄荷酮  薄荷脑

Key words:  GC  coughpill  (-)menthone  menthol

摘要:

目的 建立止咳丸中(-)薄荷酮、薄荷脑含量测定方法。方法 色谱柱HP-FFAP毛细管柱(25 m×0.2 mm，0.3 µm)；程序升温：初始温度90 ℃，保持2 min，以6 ℃·min^-1的速率升至150 ℃，再以30 ℃·min^-1的速率升温至220 ℃，保持4 min；载气为高纯氮，氢火焰离子化检测器(FID)，进样口温度：230 ℃；检测器温度：250 ℃；分流比为10∶1，进样量1.0 μL。 结果 (-)薄荷酮在0.044 86～0.897 2 mg·mL^-1(r=0.999 7)内平均回收率为98.12％，RSD=0.86％；薄荷脑在0.064 88～0.973 2 mg·mL^-1(r=0.999 8)内平均回收率为100.91%，RSD=1.16％，均呈良好线性关系。 结论 本法快速、简便、准确、可靠，可用于控制止咳丸的质量。

Abstract:

OBJECTIVE To establish a method for the determination of (-)menthone and menthol in coughpill. METHODS The analysis was carried out on an HP-FFAP capillary column(25 m×0.2 mm, 0.3 µm). Column temperature was at 90 ℃(2 min), 6 ℃·min^-1→150 ℃, 30 ℃·min^-1→220 ℃(4 min).Carrier was N2. Detector was FID. Temperature of the column entrance was 230 ℃. Temperature of the detector was 250 ℃. Fractional flow ratio was 10∶1. Sample quantity was 1.0 μL. RESULTS The linear range of (-)menthone was 0.044 86-0.897 2 mg·mL^-1(r=0.999 7). The average recovery was 98.12%, RSD=0.86%. The linear range of menthol was 0.064 88-0.973 2 mg·mL^-1(r=0.999 8). The average recovery was 100.91%, RSD=1.16%. CONCLUSION This method is simple, quick, accurate and reliable for the quality control of coughpill.