HPLC法与GC法测定清眩片中藁本内酯含量的比较  

Determination of Ligustilide in Qingxuan Tablet by HPLC and GC

作　　者：彭建彪 龙凯 许春梅 赵远翠 PENG Jianbiao;LONG Kai;XU Chunmei;ZHAO Yuancui(HongHe Prefeture Institute for Food and Drug Control,Mengzi 661199,China)

机构地区：[1]云南省红河州食品药品检验所,云南蒙自661199

出　　处：《中国民族民间医药》2023年第24期41-45,共5页Chinese Journal of Ethnomedicine and Ethnopharmacy

摘　　要：目的:比较HPLC法与GC法测定清眩片中藁本内酯含量的优劣,为清眩片中藁本内酯含量测定提供参考。方法:以藁本内酯为对照品,分别采用HPLC法与GC法对方中川芎进行含量测定。HPLC法色谱条件:用十八烷基硅烷键合硅胶柱(依利特SinoChrom ODS-BP 4.6 mm×250 mm,5μm);流动相:甲醇-水(70∶30);检测波长:326 nm;流速:1.0 mL/min;柱温:30℃。GC法色谱条件:采用(50%)二苯基-(50%)二甲基聚硅氧烷为固定液的毛细管柱(HP-50+0.50μm,0.32 mm,30 m);程序升温,起始温度为110℃,维持2 min,以7℃/min的速率升温至180℃,再以10℃/min的速率升温至220℃,维持5 min;进样口温度250℃;检测器(FID)温度260℃;以氮气为载气,流速为5.0 mL/min。结果:HPLC法藁本内酯在0.0776~1.5510μg范围内呈现良好的线性关系,相关系数R^(2)=0.9999,平均回收率为99.79%(RSD=0.29%,N=6)。GC法藁本内酯在0.0078~0.1551μg范围内呈现良好的线性关系,相关系数R^(2)=0.9992,平均回收率为105.75%(RSD=1.93%,N=6)。结论:两种方法均可以准确测定清眩片中藁本内酯的含量,HPLC法准确度与精密度都优于GC法,可以作为清眩片中藁本内酯含量测定的首选方法。GC法具有灵敏度高、分析成本低等优势可以作为清眩片中藁本内酯含量测定的备选方法。Objective To compare the content of ligustilide in Qingxuan tablets by HPLC and GC,and to provide reference for the content determination of ligustilide in Qingxuan tablets.Methods The content of ligusticum Chuanxiong was determined by HPLC and GC using ligustilide as reference.HPLC chromatographic conditions:silica gel column(SinoChrom ODS-BP 4.6 mm×250 mm,5μm)was bonded with octadecyl silane.Mobile phase:methanol-water(70∶30);Detection wavelength:326 nm;Flow rate:1.0 mL/min,Column temperature:30℃.GC chromatographic conditions:(50%)diphenyl-(50%)dimethyl polysiloxane as fixed liquid capillary column(HP-50+0.50μm,0.32 mm,30 m);The initial temperature was 110℃for 2 minutes,and the temperature was heated to 180℃at the rate of 7℃/min,and then heated to 220℃at the rate of 10℃/min for 5 minutes.Inlet temperature 250℃;Temperature of detector(FID):260℃;Nitrogen was used as carrier gas at a flow rate of 5.0 mL/min.Results The ligustilide was linear in the range of 0.0776-1.5510μg by HPLC.The correlation coefficient R^(2) was 0.9999.The average recovery was 99.79%(RSD=0.29%,N=6).The ligustilide showed a good linear relationship in the range of 0.0078-0.1551μg with the correlation coefficient R^(2)=0.9992.The average recovery was 105.75%(RSD=1.93%,N=6).Conclusions Both methods can accurately determine the content of ligustilide in Qingxuan tablets.HPLC method is superior to GC method in accuracy and precision,and can be used as the first choice for the determination of ligustilide in Qingxuan tablets.GC method has the advantages of high sensitivity and low analysis cost and can be used as an alternative method to determine the content of ligustilide in Qingxuan tablets.

关 键 词：清眩片 藁本内酯 含量测定 HPLC GC 

分 类 号：R284.1[医药卫生—中药学]