基于一测多评法定量的四季三黄片质量评价研究

Study on the Quality Evaluation of Sijisanhuang Tablets Based on Quantitative Analysis of Multi-components by Single Marker

关键词:  四季三黄片  一测多评  黄芩苷  汉黄芩苷  黄芩素  汉黄芩素  质量评价

Key words:  Sijisanhuang tablets  QAMS  baicalin  scutellarin  bacicalein  wogonin  quality evaluation

摘要:

目的 建立同时测定四季三黄片中黄芩苷、去甲汉黄芩素苷、千层纸素A-7-O-β-D葡萄糖醛酸苷、汉黄芩苷、黄芩素、汉黄芩素、千层纸素A等7种成分的一测多评法。方法 采用HPLC，岛津VP-ODS色谱柱(4.6 mm×250 mm，5μm)，以乙腈-0.1%三氟乙酸溶液为流动相，梯度洗脱；流速1.0 mL·min^-1；柱温30℃；检测波长276 nm。以黄芩苷为内参物，建立去甲汉黄芩素苷、千层纸素A-7-O-β-D葡萄糖醛酸苷、汉黄芩苷、黄芩素、汉黄芩素和千层纸素A的相对校正因子，同时采用一测多评法和外标法测定四季三黄片中7个成分的含量，并将2种方法的测定结果进行比较。结果 7种成分在各自范围内线性关系良好(r>0.9998)，平均加样回收率97.0%~102.1%，RSD为1.2%~2.5%。共测定了4个企业29批四季三黄片中7种成分的含量，结果一测多评法与外标法测定结果无明显差异。不同企业样品间各成分含量存在明显差异。结论 建立的含量方法能够反映出投料用黄芩饮片的质量状况，进而全面有效地评价四季三黄片的质量，为其质量标准的提升奠定基础。

Abstract:

OBJECTIVE To establish a quantitative analysis of multi-components by single marker(QAMS) method for simultaneous determination of baicalin, unmethylated bacicalein, melaeuca A-7-O-β-D-glucuionide, scutellarin, bacicalein, wogonin, melaeuca A in Sijisanhuang tablets. METHODS The separation was performed on HPLC with Shimadzu VP-ODS column(4.6 mm×250 mm, 5 μm), with the mobile phase consisting of acetonitrile-0.1% trifluoroacetic acid elution for gradient elution. The flow rate was 1.0 mL·min^-1, the column temperature was 30 ℃, and the detection wavelengths were 276 nm. The relative correction factors of unmethylated bacicalein, melaeuca A-7-O-β-D-glucuionide, scutellarin, bacicalein, wogonin, melaeuca A were calculated by using the baicalin as the internal standard. At the same time, the external standard method was used to determine the content of the seven components, and the differences between the two methods were compared. RESULTS The linear ranges of seven components were well(r>0.999 8). And the average recoveries were 97.0%-102.1%, RSDs were 1.2%-2.5%, respectively. There were no significant difference in assay results between QAMS and the external standard method. There were obvious differences in the contents of each component among samples from different enterprises. CONCLUSION The QAMS method can reflect the quality of Radix Scutellariae for feeding, and then comprehensively and effectively evaluate the quality of Sijisanhuang tablets, so as to lay a foundation for improving its quality standard.