GC法同时测定麝香跌打风湿膏中的3种挥发性成分

Simultaneous determination of three volatile constituents in Shexiang Dieda Fengshi adhesive plaster by headspace gas chromatography

目的采用顶空气相色谱法同时测定麝香跌打风湿膏中3种挥发性成分的含量。方法用氯仿超声溶解麝香跌打风湿膏后,以水为顶空溶剂,在80℃下平衡40 min,采用TM-WAX(50 m×0.53 mm,0.5μm)毛细管柱、FID检测器进行气相色谱检测,程序升温,初始温度100℃,以4℃.min-1升至150℃,保持2 min,进样口温度200℃,检测器温度210℃。结果樟脑、薄荷脑、水杨酸甲酯分别在10.0～160、5.17～82.7、7.42～119μg.mL-1时线性关系良好(r樟脑=0.9994,r薄荷脑=0.9992,r水杨酸甲酯=0.9993),3者的平均回收率均在93.3%～101%,RSD均小于3.6%。结论所用方法简单、快速、灵敏度高,适用于同时测定麝香跌打风湿膏中挥发性成分樟脑、薄荷脑、水杨酸甲酯的含量。

OBJECTIVE To establish a method to simultaneously determine volatile constituents in Shexiang Dieda Fengshi adhesive plaster by headspace gas chromatography. METHODS The Shexiangdiedafengshi adhesive plaster were dissolved with chloroform by ultrasonic. Optimal headspace conditions were observed when the vials were equilibrated at 80℃ for 40 rain with water as matrix medi- um. A TM -WAX capillary column（50m×0.53 mm,0.5 μm） was utilized for chromatographic separation. The initial temperature was 100 ~C and then increased to 150℃ at a rate of 4℃·min^-1 and held for 2 rain. The injector temperature and the detector temperature were controlled at 200℃and 210℃,respectively. RESULTS The calibration curve was linear at the range of 10.0 - 160 μg·mL^-1 for camphor（r = 0.9994） ,5.17 - 82.7 μg·mL^-1 for menthol（r = 0.9992）, and 7.42 - 119 μg·mL-~ for methyl salicylate （ r = 0. 9993）. All the average recoveries were limited in 93.3% - 101% and RSD less than 3.6%. CONCLUSION This method is simple, rapid, high sensitivity and suitable for simultaneous determination camphor, menthol and methyl salicylate in adhesive plasters.