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.
作者
刘杰
刘长河
王艳艳
LIU Jie;LIU Changhe;WANG Yanyan(Institute of Chinese Materia Medica,Henan Academy of Traditional Chinese Medicine,Zhengzhou 450004,China)
出处
《中国药房》
CAS
北大核心
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)。
