双香退热口服液GC指纹图谱分析及4种指标成分含量测定

GC Fingerprint Analysis of Shuangxiang Antipyretic Oral Liquid and Content Determination of 4 Index Components

目的建立双香退热口服液指纹图谱方法,并同时进行4种指标成分含量测定。方法采用HP-5弹性石英毛细管柱(30 m×0.32 mm,0.25μm);柱升温程序:起始温度110℃,保持10 min,25℃·min^(-1)的速度升温至230℃,保持9.2 min;进样口温度220℃;FID检测器温度220℃;载气:高纯N_(2)(>99.99%);柱流量1.0 mL×min^(-1);分流比10:1;进样量1μL。结果建立了双香退热口服液GC指纹图谱方法,10批成品中检测到的色谱峰为13个,其中1,2,3,4号峰来源于香薷药材,5,6,7,8号峰来源于厚朴药材,9~13号峰在香薷和厚朴药材及其阴性中均有出现,初步推测此类成分为香薷和厚朴两药材共有成分。以对照品与样品出峰时间比对,标定1号峰为麝香草酚、2号峰为香荆芥酚、7号峰为厚朴酚、8号峰为和厚朴酚,4种指标成分线性范围分别为0.226~2.260 mg·mL^(-1),0.1055~1.0550 mg·mL^(-1),0.0828~0.8280 mg·mL^(-1),0.0720~0.7200 mg·mL^(-1)。平均加样回收率分别为100.1%~103.5%,100.2%~104.4%,99.4%~100.7%,96.3%~99.27%;RSD分别为2.8%,2.1%,2.4%,2.1%。结论本法稳定、合理、可行,为该复方中药质量评价提供科学依据。

OBJECTIVE To establish the fingerprint method of Shuangxiang antipyretic oral liquid and determine the contents of 4 index components simultaneously.METHODS The analysis was carried out on HP-5 capillary column(30 m×0.32 mm,0.25μm).The column temperature rose by program,the initial temperature was 110℃and maintained for 10 min,then the temperature raised to 230℃at a rate of 25℃·min^(-1) and maintained for 9.2 min.Inlet temperature was 220℃,FID detector temperature was 220℃.High purity N_(2)(>99.99%)was used as the carrying gas,and the column flow was 1.0 mL·min^(-1).The split ratio was 10:1,and the injection volume was 1μL.RESULTS The preferable method for GC fingerprint of Shuangxiang antifebrile oral liquid achieved,there were 13 common peaks in the GC fingerprints of 10 batches of samples,among which peaks 1,2,3 and 4 were from Moslae Herba,peaks 5,6,7 and 8 were from Magnoliae Officinalis Cortex,peaks 9-13 appeared in Moslae Herba and Magnoliae Officinalis Cortex and their negative control herbs,it was preliminarily presumed such components were the common components of them.According to the retention time,the No.1 peak was identified as thymol,No.2 peak as carvacrol,No.7 peak as magnolol,No.8 peak as honokiol.The linear ranges of the four index components were 0.226-2.260 mg·mL^(-1),0.1055-1.0550 mg·mL^(-1),0.0828-0.8280 mg·mL^(-1),and 0.0720-0.7200 mg·mL^(-1),respectively.The average recoveries were 100.1%-103.5%,100.2%-104.4%,99.4%-100.7%and 96.3%-99.27%;with the RSD was 2.8%,2.1%,2.4%and 2.1%,respectively.CONCLUSION The method is stable,reasonable and feasible,which provides scientific basis for the quality evaluation of the compound traditional Chinese medicine.