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[摘要]
目的:建立GC内标法同时测定复方樟脑乳膏中樟脑、薄荷脑、水杨酸甲酯主要成分的含量。方法:采用SHIMADZU SH-Rtx-Wax毛细管色谱柱(30 m × 0.25 mm × 0.25 μm),载气为氮气,流速 1 mL·min-1,空气流速 200 mL·min-1,氢气流速 32 mL·min-1,FID为检测器,检测器温度250 ℃,进样口温度250 ℃,分流比10:1,程序升温(起始温度为 160 ℃,维持 13.5分钟,以每分钟 60 ℃的速率升温至 240 ℃,维持 15分钟),正十三烷为内标。结果:复方樟脑乳膏中樟脑、薄荷脑、水杨酸甲酯分离度良好,方法专属性强,线性范围宽,精密度好,准确度高,耐用性好。樟脑、薄荷脑、水杨酸甲酯分别在 0.89 mg· mL-1 ~ 1.85 mg· mL-1(r = 0.999 9)、0.75 mg· mL-1 ~ 1.70 mg· mL-1(r = 0.999 0)、0.38 mg· mL-1 ~ 1.33 mg· mL-1(r = 0.999 8)浓度范围内与其峰面积及内标溶液峰面积的比值呈线性关系,低、中、高浓度平均回收率分别为 100.5 %(RSD = 0.7 %)、99.9%(RSD = 0.9%)、102.3%(RSD = 1.0%)。结论:该方法操作简单,准确度高,重现性好,可用于复方樟脑乳膏的质量控制。
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[Abstract]
Objective: To establish a method for the determination of camphor、Menthol and Methyl Salicylate in compound camphor cream by GC internal standard method. Methods:GC method was performed on SHIMADZU SH-Rtx-Wax capillary column (30 m × 0.25 mm × 0.25 μm) column,with nitrogen as the carrier gas,the flow rate was 1. 0 mL·min-1,air 200 mL·min-1,hydrogen 32 mL·min-1,and FID as the detector(temperature is 250 ℃),Injector temperature is 250 ℃,split ratio 10:1.The temperature programme: Initial temperature was 160 ℃,which was retained 13.5 minutes,and then 60 ℃ per minute up to 240 ℃,retaining 15 minutes. N-tridecane was used as the internal standard. Results: Camphor,menthol,methyl salicylate,n-tridecane and various accessories in compound camphor cream were well separated.The method was specific,linear,accurate,precise and robust.The linear ranges of camphor、Menthol and Methyl Salicylate were 0.89 mg· mL-1 ~ 1.85 mg· mL-1 (r = 0.999 9),0.75 mg· mL-1 ~ 1.70 mg· mL-1 (r = 0.999 0),0.38 mg· mL-1 ~ 1.33 mg· mL-1 (r = 0.999 8), respectively.The average recoveries(n = 3) of low,middle and high concentrations were 100.5%(RSD = 0.7%)、99.9%(RSD = 0.9%)、102.3%(RSD = 1.0%) Conclusion:The method was simple with high accuracy and good reproducibility, and provides a reliable way for evaluating the quality of compound camphor cream.
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