八珍丸HPLC特征指纹图谱研究及多成分定量分析  

Fingerprint and Multi-components Quantitative Determination of Bazhen Pills by HPLC

作　　者：孙燕 Sun Yan(Pharmacy Department of Dongying Second People＇s Hospital,Shandong Dongying 257335,Chin)

机构地区：[1]东营市第二人民医院药剂科,山东东营257335

出　　处：《中国药师》2018年第8期1369-1373,共5页China Pharmacist

摘　　要：目的:建立八珍丸HPLC指纹图谱,并进行多成分定量分析,为八珍丸的质量控制提供可靠依据。方法:采用SHIMADZU VP-ODS(250 mm×4.6 mm,5μm)色谱柱,以乙腈-甲醇-水(60∶38∶2)(A)-0.6%磷酸水溶液(B)作为流动相进行梯度洗脱,流速1.0 ml·min-1,柱温35℃,检测波长230 nm、320 nm、220 nm。结果:利用《中药色谱指纹图谱相似度评价系统2004A版》进行分析,共确定八珍丸HPLC指纹图谱17个共有峰,通过与混合对照品比较指认其中6个指标成分分别是:芍药苷(4号峰)、毛蕊花糖苷(6号峰)、阿魏酸(8号峰)、甘草苷(9号峰)、白术内酯Ⅰ(13峰)和白术内酯Ⅲ(17号峰)。对12批样品的指纹图谱进行相似度分析,各批样品相似度均在0.9以上。芍药苷、毛蕊花糖苷、阿魏酸、甘草苷、白术内酯Ⅰ和白术内酯Ⅲ线性范围分别为0.010~0.250μg(r=0.999 7)、0.124~3.100μg(r=0.999 1)、0.058~1.450μg(r=0.999 5)、0.069~1.475μg(r=0.999 0)、0.032~0.800μg(r=0.999 8)和0.027~0.675μg(r=0.999 3)。12批八珍丸中芍药苷、毛蕊花糖苷、阿魏酸、甘草苷、白术内酯Ⅰ和白术内酯Ⅲ含量分别为0.099~0.118 mg·g-1、1.383~1.449 mg·g-1、0.300~0.395 mg·g-1、0.504~0.604 mg·g-1、1.013~1.080 mg·g-1和0.205~0.299 mg·g-1。结论:所建立的八珍丸HPLC指纹图谱检测和定量测定分析方法快速、准确、专属性强、灵敏度高,可以用于评价该制剂的质量。Objective： To establish an HPLC fingerprint method and a multi-component quantitative determination method for Bazhen pills,so as to provide reliable basis for the quality control. Methods： A SHIMADZU VP-ODS（ 250 mm × 4. 6 mm,5 μm） column was used,the mobile phase was acetonitrile-methanol-water（ 60 ∶ 38 ∶ 2）（ A）-0. 6% phosphoric acid solution（ B） with gradient elution. The flow rate was 1. 0 ml·min-1,the column temperature was 35 ℃,and the detection wavelengths were 230 nm,320 nm and 220 nm. Results： Chinese Medicine Fingerprint Similarity Evaluation System 2004 A edition was used for the analysis and totally 17 common peaks were identified. Compared with the mixed reference materials,6 indicators were identified： paeoniflorin（ peak 4）,acteoside（ peak 6）,ferulic acid（ peak 8）,liquiritin（ peak 9）,atractylactone I（ peak 13） and atractylactone III（ peak 17）. The similarity of the fingerprints of 12 batches of samples was analyzed,and that of each batch was above 0. 9. The linear range of paeoniflorin,acteoside,ferulic acid,liquiritin,atractylactone I and atractylactone III was 0. 010-0. 250 μg（ r = 0. 999 7）,0. 124-3. 100 μg（ r =0. 999 1）,0. 058-1. 450 μg（ r = 0. 999 5）,0. 069-1. 475 μg（ r = 0. 999 0）,0. 032-0. 800 μg（ r = 0. 999 8） and 0. 027-0. 675 μg（ r= 0. 999 3）,respectively. The contents of paeoniflorin,acteoside,ferulic acid,liquiritin,atractylactone I and atractylactone III in the12 batches of Bazhen pills were 0. 099 0-0. 118 0 mg · g-1,1. 383 0-1. 449 0 mg · g-1,0. 300 0-0. 395 0 mg · g-1,0. 504 0-0. 604 0 mg·g-1,1. 013 0-1. 080 0 mg·g-1 and 0. 205 0-0. 299 0 mg·g-1,respectively. Conclusion： The established method is rapid and accurate with strong specificity and high sensitivity,which can be used for the quality control of the preparation.

关 键 词：八珍丸 高效液相色谱法 指纹图谱 相似度分析 芍药苷 毛蕊花糖苷 阿魏酸 甘草苷 白术内酯Ⅰ 白术内酯Ⅲ 

分 类 号：TQ460.72[医药卫生—药物分析学]