清眩丸中5种挥发性成分含量测定气相色谱法的建立  

Establishment of gas chromatography for content determination of five volatile components in Qingxuan pills

作　　者：刘杰[1] 刘长河[1] 王艳艳[1] LIU Jie;LIU Changhe;WANG Yanyan(Institute of Chinese Materia Medica,Henan Academy of Traditional Chinese Medicine,Zhengzhou 450004,China)

机构地区：[1]河南省中医药研究院中药研究所,郑州450004

出　　处：《中国药房》2022年第17期2097-2101,共5页China Pharmacy

基　　金：河南省中医药科学研究专项课题(No.2018ZY3070)。

摘　　要：目的建立测定清眩丸中薄荷酮、薄荷脑、胡薄荷酮、胡椒酮和藁本内酯5种挥发性成分含量的方法。方法以7批清眩丸为检测样品,采用气相色谱法进行测定。气相色谱柱为DB-5石英毛细管柱,载气为氮气,进样口温度为200℃,进样量为1μL,分流比为10∶1,程序升温(初始温度100℃保持2 min,以5℃/min升温至220℃并保持2 min),火焰离子化检测器温度为250℃。结果薄荷酮、薄荷脑、胡薄荷酮、胡椒酮和藁本内酯与相邻成分色谱峰均达到基线分离;5种成分的线性范围依次为0.008~0.388、0.010~0.527、0.006~0.327、0.006~0.312、0.053~2.672 mg/mL(r均大于0.9990);平均加样回收率依次为96.33%(RSD=1.23%,n=6)、96.92%(RSD=1.38%,n=6)、97.53%(RSD=1.81%,n=6)、96.80%(RSD=1.89%,n=6)、95.61%(RSD=0.77%,n=6);5种成分的含量依次为0.009~0.070、0.040~0.157、0.017~0.150、0.008~0.049、0.144~0.932 mg/g。结论本研究建立的气相色谱法简便、准确,能同时测定清眩丸中5种挥发性成分的含量。OBJECTIVE To establish a method for the determination of 5 volatile components as menthone,menthol,pulegone,piperitone and ligustilide in Qingxuan pills.METHODS Seven batches of Qingxuan pills were taken as test samples and determined by gas chromatography.The gas chromatographic column was DB-5 sillica capillary column,the carrier gas was nitrogen,the inlet temperature was 200℃.The sample size was 1μL,and the split ratio was 10∶1.The temperature was programmed(the initial temperature was kept at 100℃for 2 min,and then raised to 220℃at 5℃/min for 2 min),and the temperature of the flame ionization detector was 250℃.RESULTS The chromatographic peaks of menthone,menthol,pulegone,piperitone and ligustilide reached the baseline separation;the linear ranges of the five components were 0.008-0.388,0.010-0.527,0.006-0.327,0.006-0.312,0.053-2.672 mg/mL(all r>0.9990);the average recoveries were 96.33%(RSD=1.23%,n=6),96.92%(RSD=1.38%,n=6),97.53%(RSD=1.81%,n=6),96.80%(RSD=1.89%,n=6)and 95.61%(RSD=0.77%,n=6);the contents of the five components were 0.009-0.070,0.040-0.157,0.017-0.150,0.008-0.049 and 0.144-0.932 mg/g,respectively.CONCLUSIONS The gas chromatography method established in this study is simple and accurate,which can simultaneously determine the contents of five volatile components in Qingxuan pills.

关 键 词：清眩丸 薄荷酮 薄荷脑 胡薄荷酮 胡椒酮 藁本内酯 气相色谱法 

分 类 号：R917[医药卫生—药物分析学]