GC内标法测定复方樟脑乳膏中樟脑、薄荷脑和水杨酸甲酯的含量  

DETERMINATION OF CAMPHOR、MENTHOL AND METHYL SALICYLATE IN COMPOUND CAMPHOR CREAM BY GC INTERNAL STANDARA METHOD

作　　者：王国英 周刚 WANG Guoying;ZHOU Gang(Chemical Inspeetion Room,Inner Mongolia Institute for Drug Control,Hohhot 010020,China)

机构地区：[1]内蒙古自治区药品检验研究院化学药品室,内蒙古呼和浩特010020

出　　处：《内蒙古医科大学学报》2022年第3期234-237,242,共5页Journal of Inner Mongolia Medical University

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×0.25μm),载气为氮气,流速1 mL/min,空气流速200 mL/min,氢气流速32 mL/min,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 min,以60℃/min的速率升温至240℃,维持15 min),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0.89~1.85 mL/min(r=0.9999)、0.75~1.70 mL/min(r=0.9990)、0.38~1.33 mL/min(r=0.9998)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。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×0.25μm)column,with nitrogen as the carrier gas,the flow rate was 1.0 mL/min,air 200 mL/min,hydrogen 32 mL/min,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 0.891.85 mL/min(r=0.9999),0.75~1.70 mL/min(r=0.9990),0.38~1.33 mL/min(r=0.9998),respectively.The average recoveries of low,middle and high concentrations were100.5%(RSD=0.7%)、99.9%(RSD=0.9%)、102.3%(RSD=1.0%).Conclusions The method was simple with high accuracy and good reproducibility,and provides a reliable way for evaluating the quality of compound camphor cream.

关 键 词：复方樟脑乳膏 GC内标法 樟脑 薄荷脑 水杨酸甲酯 

分 类 号：R47.5[医药卫生—护理学]