GC测定消炎止痒醑中樟脑的含量

Determination of Camphor in Xiaoyanzhiyang Xu by GC

关键词:  气相色谱法  消炎止痒醑  樟脑  含量测定

Key words:  gas chromatography(GC)  Xiaoyanzhiyang Xu  camphor  determination

摘要:

目的 建立GC测定消炎止痒醑中樟脑的含量。方法 采用毛细管气相色谱法。色谱柱为CP-Sil 5 CB石英毛细管色谱柱(25 m×0.32 mm，0.4 μm)；FID火焰离子化检测器；载气为氮气；氢气与氮气的流量比通常为1∶1~1∶1.5；氢气和空气流量比为1∶10；流速：1 mL·min^-1；分流比：20∶1；温度设置：进样口温度为250 ℃，柱温为280 ℃(程序升温：从60 ℃开始, 保持1 min，再以12 ℃·min^-1的速度升温至280 ℃，保持3 min)，检测器温度为300 ℃；进样量：1 μL。结果 樟脑在50~400 mg·L^-1内呈现良好的线性关系，r=0.999 9；平均回收率为99.64%(RSD为1.19%)；在6 h内稳定。结论 本方法简单易行、快速、准确性和重复性好，可用于消炎止痒醑的质量控制。

Abstract:

OBJECTIVE To establish a method for determine camphor in Xiaoyanzhiyang Xu by GC. METHODS Use capillary gas chromatography. Chromatographic column is CP-Sil 5 CB quartz chromatographic column(25 m×0.32 mm, 0.4 μm); FID flame ionization detector; carrier gas is nitrogen; usually specific flux of hydrogen and nitrogen is 1∶1~1∶1.5; flow ratio of hydrogen and air is 1∶10; velocity of flow: 1 mL·min^-1; split ratio: 20∶1; temperature setting: sampling input temperature 250 ℃; column temperature 280 ℃(temperature programming process: start from 60 ℃, retain 1 min, achieve 280 ℃ by temperature rising speed 12 ℃·min^-1, retain 3 min); detector temperature 300 ℃; sample size: 1 μL. RESULTS The linear range of Camphor was 50~400 mg·L^-1，r=0.999 9; the recovery of Camphor was 99.64%(RSD=1.19%) and it was stable in 6 hours. CONCLUSION The method is simple and easy, fast, accurate and repeatable. It can be used as quality control method for Xiaoyanzhiyang Xu.