溪黄草破壁饮片指纹图谱及化学成分含量测定研究
Study on Fingerprint and Chemical Component Content Determination of Xihuangcao Broken Wall Decoction Pieces
黄志业 1邹怡 2廖芷晴 1袁焕合 1张广立 1张前亮3
作者信息
- 1. 广东省药品检验所,广东 广州 510000
- 2. 中山大学新华学院,广东 广州 510000
- 3. 中山市中智中药饮片有限公司,广东 中山 528400
- 折叠
摘要
目的:建立溪黄草破壁饮片的指纹图谱含量测定方法,为溪黄草破壁饮片的质量控制提供参考依据.方法:采用同一HPLC建立溪黄草破壁饮片指纹图谱及咖啡酸与迷迭香酸的含量测定方法,以Platisil C18(5 μm,4.6×250 mm)为色谱柱,流动相选择乙腈-含0.1%磷酸的水溶液,梯度洗脱,流速为1.0 mL/min,柱温为35℃,检测波长为327 nm.色谱数据采用国家药典委员会中药色谱指纹图谱相似度评价分析系统,生成标准指纹图谱.结果:10批溪黄草破壁饮片有7个共有峰,相似度为0.867～0.983,并指认出2个色谱峰.咖啡酸在 0.0354～0.1239 mg/mL(R2=0.9999)、迷迭香酸在 0.0866～0.3030 mg/mL(R2=0.9999)范围内呈良好的线性关系.重复性试验、稳定性试验和精密度试验的RSD均＜2%,加样回收率为咖啡酸91.4%～94.6%,RSD=1.3%、迷迭香酸93.6%～97.5%,RSD=1.6%.结论:本方法准确可靠,重现性好,为溪黄草的质量控制提供科学依据.
Abstract
Objective:To establish a method for the determination of the content of cut-wall cut-pieces by HPLC fingerprint,and to provide a reference for the quality control of cut-wall cut-pieces.Method:A HPLC method was established for the determination of CAFFEIC ACID and rosmarinic acid in cut crude drug of Herba Secalinis.The chromatographic column was Platisil C18(5 μm,4.6×250 mm)and the mobile phase was acetonitrile-0.1％phosphoric acid,the flow rate was 1.0 mL/min,the column temperature was 35℃,and the detection wavelength was 327 nm.The chromatographic data were analyzed by the similarity evaluation system of chromatographic fingerprints of Chinese Materia Medica of the State Pharmacopoeia Commission,and the standard fingerprints were generated.Result:There were 7 common peaks in the 10 batches of cut-off pieces,the similarity was 0.867～0.983,and 2 chromatographic peaks were identified.There was a good linear relationship between caffeic acid and rosmarinic acid in the range of 0.0354～0.1239 mg/mL(R2=0.9999)and 0.0866～0.3030 mg/mL(R2=0.9999).The RSD of repeatability test,stability test and precision test were all<2％.The recoveries of caffeic acid,rosmarinic acid and rosmarinic acid were 91.4％～94.6％,1.3％;93.6％～97.5％ and 1.6％,respectively.Conclusion:The method is accurate,reliable and reproducible,and provides scientific basis for the quality control of Saussurea Chinense.
关键词
溪黄草/破壁饮片/HPLC/指纹图谱/咖啡酸/迷迭香酸/含量测定Key words
xihuangcao/broken wall drink slice/hplc/fingerprint spectrum/caffeic acid/rosmarinic acid/content determination引用本文复制引用
出版年
2024
NETL
NSTL
万方数据