双鱼颗粒挥发性成分指纹图谱和定量分析  

Establishment and application of fingerprint and quantitative method of volatile components in Shuangyu Granules

作　　者：林夏[1,2] 崔培超[1,2] 王雪[1,2] 胡晗绯[1,2] 吴云 王正宽[1,2] 王振中[1,2] 肖伟[1,2] LIN Xia;CUI Pei-chao;WANG Xue;HU Han-fei;WU Yun;WANG Zheng-kuan;WANGZhen-zhong;XIAO Wei(Jiangsu Kanion Pharmaceutical Co.,Ltd.,Lianyungang 222001,China;State Key Laboratory of New丒tech for Chinese Medicine Pharmaceutical Process,Lianyungang 222001,China)

机构地区：[1]江苏康缘药业股份有限公司,江苏连云港222001 [2]中药制药过程新技术国家重点实验室,江苏连云港222001

出　　处：《中草药》2019年第9期2081-2086,共6页Chinese Traditional and Herbal Drugs

基　　金：国家"重大新药创制"科技专项(2017ZX09301034);江苏省"六大人才高峰"计划(P003)

摘　　要：目的建立双鱼颗粒挥发性成分指纹图谱及定量测定方法。方法 Agilent DB-1毛细管柱(30 m×0.32 mm,0.25μm);进样量为1μL;分流比为25∶1;进样口温度为230℃;以氮气为载气,体积流量0.6 mL/min;FID检测器温度为250℃;程序升温。结果建立的指纹图谱分离度和重复性良好,确定12个共有峰,各批次样品相似度在0.95以上;采用GC/MS对色谱峰进行定性分析,其中7个成分经对照品比对,分别为桉油精(峰2)、樟脑(峰3)、薄荷酮(峰4)、龙脑(峰5)、薄荷脑(峰6)、(+)-胡薄荷酮(峰9)、甲基正壬酮(峰10),其中1、10、11、12号峰主要来自于鱼腥草,2、5号峰主要来自于艾叶和薄荷,3号峰主要来自于艾叶,4、6、8、9号峰主要来自于薄荷,7号峰主要来自于艾叶、薄荷和鱼腥草。并对其中桉油精、薄荷脑进行定量分析,平均回收率分别为103.9%和98.2%,RSD分别为2.1%和2.3%。10批次样品中桉油精为0.17～0.23mg/g,薄荷脑为0.45～0.67mg/g。结论建立的双鱼颗粒指纹图谱和2个指标成分定量分析方法,快速、简便、准确,能有效评价该制剂的质量。Objective To establish the GC fingerprint and components quantitative determination of Shuangyu Granules(SG) for quality control. Methods Agilent DB-1 capillary column(30 m × 0.32 mm, 0.25 μm) was used with upper column volume of 1 μL and split ratio of 25∶1;Injection port was 230 ℃ and detector temperatures was 250 ℃;The carrier gas was nitrogen and its flow rate was 0.6 m L/min. The column temperature was raised by program. Results The fingerprints with good separation and repeatability included 12 mutual common peaks, and the similarity of each batch was more than 0.95. Seven chemical components were identified by GC/MS and standard compounds, which were eucalyptol(peak 2), camphor(peak 3), menthone(peak 4), borneol(peak 5), menthol(peak 6), pulegone(peak 9), and undecanone(peak 10);Among which, peaks of 1, and 10-12 were from Houttuyniae Herba, peaks of 2 and 5 from Artemisiae Argyi Folium and Menthae Haplocalycis Herba, peak of 3 from Artemisiae Argyi Folium, peak of 4, 6, 8 and 9 from Menthae Haplocalycis Herba, peak of 7 from Menthae Haplocalycis Herba, Artemisiae Argyi Folium and Houttuyniae Herba. Moreover, eucalyptol and menthol were quantified and the average recovery rates of eucalyptol and menthol were 103.9% and 98.2%(RSD were 2.1% and 2.3%), respectively. The content of eucalyptol and menthol in 10 batches samples were 0.17-0.23 mg/g and 0.45-0.67 mg/g, respectively. Conclusion The method of fingerprint and quantitative analysis of two components in SG was rapid, simple, and accurate, which could be used for the quality control of SG.

关 键 词：双鱼颗粒 挥发性成分 气相色谱 指纹图谱 相似度 GC-MS 桉油精 樟脑 薄荷酮 龙脑 薄荷脑 胡薄荷酮 甲基正壬酮 

分 类 号：R286.02[医药卫生—中药学]