气相色谱法同时测定麝香追风止痛膏中5种挥发性成分的含量  

Content Determination of 5 Volatile Constituents in Shexiang Zhuifeng Zhitong Plaster by GC

作　　者：黄传俊[1,2] 陈云 曾博程 刘勇 曾凡华 王文娟 叶修文 杜君 代晓进 杨红菊 谯志文 周年华 HUANG Chuanjun;CHEN Yun;ZENG Bocheng;LIU Yong;ZENG Fanhua;WANG Wenjuan;YE Xiuwen;DU Jun;DAI Xiaojin;YANG Hongju;QIAO Zhiwen;ZHOU Nianhua(Dept.of Pharmaceutical Affair,Hubei Provincial Hospital of TCM,Wuhan 430061,China;Hubei Institute of TCM,Wuhan 430074,China;Chongqing CISCO Pharmaceutical Research Institute Co.,Ltd.,Chongqing 401520,China)

机构地区：[1]湖北省中医院药事部,武汉430061 [2]湖北省中医药研究院,武汉430074 [3]重庆思科药物研究所有限公司,重庆401520

出　　处：《中国药房》2018年第14期1931-1935,共5页China Pharmacy

基　　金：重庆市社会民生科技创新专项项目(No.cstc2016shmszx130065)

摘　　要：目的:建立同时测定麝香追风止痛膏中5种挥发性成分含量的方法。方法:采用气相色谱法,色谱柱为PEG-20M毛细管柱,检测器为氢火焰离子化检测器,载气为氮气(纯度:99.999%),柱流量为1.5 m L/min,吹扫流量为3.0 m L/min,分流比为5∶1,进样口温度为200℃,检测器温度为250℃,程序升温,进样量为2μL,尾吹流量为40 m L/min。结果:樟脑、龙脑、异龙脑、薄荷脑、水杨酸甲酯检测质量浓度线性范围分别为19.78~247.26μg/m L(r=0.999 6)、15.88~198.52μg/m L(r=0.999 9)、8.60~107.56μg/m L(r=0.999 9)、20.11~251.32μg/m L(r=0.999 8)、12.09~151.11μg/m L(r=0.999 3);定量限分别为329.68、264.69、143.41、335.09、402.96 ng/m L,检测限分别为98.90、79.41、43.02、100.53、120.89 ng/m L;中间精密度、稳定性、重复性试验的RSD均小于3%;加样回收率分别为97.85%~101.52%(RSD=1.54%,n=6)、99.55%~103.75%(RSD=1.38%,n=6)、98.88%~104.23%(RSD=1.94%,n=6)、98.11%~102.64%(RSD=1.92%,n=6)、96.55%~99.61%(RSD=1.44%,n=6);耐用性试验的RSD均小于3%。结论:该方法操作简便,精密度、稳定性、重复性、耐用性好,可用于麝香追风止痛膏中5种挥发性成分含量的同时测定。OBJECTIVE:To establish the method for simultaneous determination of 5 volatile constituents in Shexiang zhuifeng zhitong plaster.METHODS:Gas chromatography was adopted.The determination was performed on PEG-20M capillary column with flame ionization detector as detector,nitrogen(99.999%)as carrier gas,with column flow rate of 1.5 mL/min,purge flow of 3.0 mL/min,split ratio of 5∶1,injector temperature of 200℃,detector temperature of 250℃,temperature programming,sample size of 2μL,tail blowing flow of 40 mL/min.RESULTS:The linear range of camphor,borneol,isoborneol,menthol and menthyl salicylate were 19.78-247.26μg/mL(r=0.999 6),15.88-198.52μg/mL(r=0.999 9),8.60-107.56μg/mL(r=0.999 9),20.11-251.32μg/mL(r=0.999 8)and 12.09-151.11μg/mL(r=0.999 3),respectively.The limits of quantitation were 329.68,264.69,143.41,335.09,402.96 ng/mL;the limits of detection were 98.90,79.41,43.02,100.53,120.89 ng/mL,respectively.RSDs of precision,stability and reproducibility tests were all lower than 3%.The recoveries were 97.85%-101.52%(RSD=1.54%,n=6),99.55%-103.75%(RSD=1.38%,n=6),98.88%-104.23%(RSD=1.94%,n=6),98.11%-102.64%(RSD=1.92%,n=6),96.55%-99.61%(RSD=1.44%,n=6),respectively.RSDs of durability test were all lower than 3%.CONCLUSIONS:The method is simple,precise,stable,reproducible and durable,and can be used for simultaneous determination of 5 volatile constituents in Shexiang zhuifeng zhitong plaster.

关 键 词：麝香追风止痛膏 樟脑 龙脑 异龙脑 薄荷脑 水杨酸甲酯 气相色谱法 含量测定 

分 类 号：R284.1[医药卫生—中药学]