双柱串联气相色谱法同时测定千金止带丸中6种有效成分的含量  

Simultaneous Determination of Six Effective Components in Qianjin Zhidai Pills by Tandem Double Column GC

作　　者：赵佳佳[1] 杨广胜[1] 孙晓[1] 张小龙 陈洪岩[2] Zhao Jiajia;Yang Guangsheng;Sun Xiao;Zhang Xiaolong;Chen Hongyan(Lianyungang First People’s Hospital,Jiangsu Lianyungang 222002,China;Lianyungang Food and Drug Inspection Center;Nanjing University of Chinese Medicine)

机构地区：[1]连云港市第一人民医院,江苏连云港222002 [2]连云港市食品药品检验检测中心 [3]南京中医药大学

出　　处：《中国药师》2019年第8期1542-1544,共3页China Pharmacist

摘　　要：目的:运用双柱串联,建立同时测定千金止带丸中6种有效成分茴香醛、乙酸龙脑酯、反式茴香脑、α-香附酮、木香烃内酯、去氢木香内酯含量的气相色谱方法。方法:色谱柱为HP-5柱(30 m×0.32 mm×0.25μm)串联DB-1301柱(30 m×0.32 mm,0.25μm);采取程序升温,载气为氮气,流速为2.0 ml·min^-1,进样量为1μl,分流比为5∶1,进样口温度为280℃,检测器(FID)温度为300℃。结果:茴香醛、乙酸龙脑酯、反式茴香脑、α-香附酮、木香烃内酯、去氢木香内酯分别在12.83~410.50μg·ml^-1(r=0.999 4)、12.53~401.00μg·ml^-1(r=0.999 4)、12.86~411.60μg·ml^-1(r=0.999 8)、15.37~491.70μg·ml^-1(r=0.999 7)、13.86~443.40μg·ml^-1(r=0.999 6)、13.23~423.20μg·ml^-1(r=0.999 7)范围内呈良好的线性关系;加样回收率分别为99.81%(RSD=1.69%),98.42%(RSD=0.57%),99.27%(RSD=1.11%),99.06%(RSD=0.87%),99.62%(RSD=0.71%),99.21%(RSD=0.93%)(n=6)。结论:该方法操作简便,灵敏度高,准确度好,可为控制该制剂的质量提供依据。Objective: To establish a tandem double column GC method for the simultaneous determination of anisaldehyde,bornyl acetate,trans-anethole,α-cyperone,costunolide and dehydrocostus lactone in Qianjin Zhidai pills.Methods: The determination was performed on an HP-5 column (30 m × 0.32 mm,0.25 μm) coupled with a DB-1301 column(30 m × 0.32 mm,0.25 μm) by programmed temperature.The carrier gas was nitrogen at the flow rate of 2.0 ml·min^-1 .The injection volume was 1 μl and the sample split ratio was 5∶ 1.The inlet temperature was 280 ℃.The detector was a flame ionization detector with the temperature of 300 ℃.Results: The linear range was 12.83-410.50 μg·ml^-1 for anisaldehyde (r = 0.999 4),12.53-401.00 μg·ml^-1 for bornyl acetate (r = 0.999 4),12.86-411.60 μg·ml^-1 for trans-anethole (r = 0.999 8),15.37-491.70 μg·ml^-1 for α-cyperone (r = 0.999 7), 13.86-443.40 μg·ml^-1 for costunolide (r = 0.999 6) and 13.23-423.20 μg·ml^-1 for dehydrocostus lactone (r = 0.999 7).The average recovery of the six effective components was 99.81%(RSD = 1.69%),98.42%(RSD = 0.57%),99.27%(RSD = 1.11%),99.06%(RSD = 0.87%),99.62%(RSD = 0.71%) and 99.21%(RSD = 0.93%)(n = 6),respectively.Conclusion: The method is simple,sensitive and accurate,and can be used for the quality control of Qianjin Zhidai pills.

关 键 词：千金止带丸 双柱串联气相色谱法 含量测定 茴香醛 乙酸龙脑酯 反式茴香脑 Α-香附酮 木香烃内酯 去氢木香内酯 

分 类 号：R927.2[医药卫生—药学]