一测多评法测定猪胆粉中4种指标成分的含量  

Determination of 4 Index Components in Suis Fellis Pulvis by Quantitative Analysis of Multi-Components by Single-Marker

作　　者：王汝上 钟铖 陈瑞君 段子浩 钟泓玲 李政海 WANG Ru-Shang;ZHONG Cheng;CHEN Rui-Jun;DUAN Zi-Hao;ZHONG Hong-Ling;LI Zheng-Hai(Guangzhou Consun Drug Research Ltd.,Guangzhou 510663 Guangdong,China)

机构地区：[1]广州康臣药物研究有限公司,广东广州510663

出　　处：《广州中医药大学学报》2023年第4期984-991,共8页Journal of Guangzhou University of Traditional Chinese Medicine

基　　金：广西重点研发计划项目(编号:桂科AB20159029)。

摘　　要：【目的】建立一测多评法同时测定猪胆粉中牛磺猪去氧胆酸、牛磺鹅去氧胆酸、甘氨猪去氧胆酸、甘氨鹅脱氧胆酸钠4种指标成分的含量,并完成方法学验证。【方法】采用Agilent 1260型高效液相色谱仪、DAD检测器和Agilent ZORBAX SBAq C18(4.6 mm×250 mm,5μm),以乙腈-0.03 mol/L磷酸二氢钠(p H3.45)为流动相梯度洗脱,检测波长为200 nm,流速为1.0 mL/min,柱温为25℃。以牛磺猪去氧胆酸为内参物,通过外标法测定内参物含量,建立相对校正因子计算牛磺鹅去氧胆酸、甘氨猪去氧胆酸、甘氨鹅脱氧胆酸钠的含量,同时对比一测多评法与外标法测定11批猪胆粉中4种指标成分的含量。【结果】猪胆粉中牛磺猪去氧胆酸与牛磺鹅去氧胆酸、甘氨猪去氧胆酸、甘氨鹅脱氧胆酸钠的相对校正因子(f)分别为1.214、1.260、1.243;各指标成分依次在0.181 6~4.540 6、0.162 9~4.073 4、0.746 1~18.653 0、0.495 9~12.397 5μg范围内线性关系良好(r>0.999);平均加样回收率分别为100.00%、100.11%、97.30%、98.23%;相对标准偏差(RSD)分别为1.11%、4.15%、1.13%、1.17%;该方法精密度、重复性、稳定性的RSD均小于5.0%。11批猪胆粉中4种指标成分一测多评法计算值与外标法实测值间结果相对偏差均小于5%,表明2种检测方法结果无显著性差异。【结论】一测多评法检测猪胆粉中牛磺猪去氧胆酸、牛磺鹅去氧胆酸、甘氨猪去氧胆酸、甘氨鹅脱氧胆酸钠的含量,可降低对照品的使用成本,该方法高效快捷、准确度高,方法简便。Objective A quantitative analysis of multi-components by single-marker was developed for the simultaneous determination of 4 index components in suis fellis pulvis, namely taurodeoxycholic acid,taurochenodeoxycholic acid,glycine porcine deoxycholic acid and glycochenodeoxycholate,and methodological validation was completed. Methods The separation was performed on an Agilent 1260 high performance liquid chromatograph with a DAD detector and an Agilent ZORBAX SB-Aq C18(4.6 mm×250 mm, 5 μm),using acetonitrile-0.03 mol/L sodium dihydrogen phosphate(pH3.45)as the mobile phase in a gradient elution with a detection wavelength of 200 nm,a flow rate of 1.0 mL/min and a column temperature of 25 ℃;the content of the internal reference material was determined by an external standard method using taurodeoxycholic acid as the internal reference material. The relative calibration factors were established to calculate the contents of taurochenodeoxycholic acid,glycine porcine deoxycholic acid and glycochenodeoxycholate,and the contents of the four index components in 11 batches of suis fellis pulvis were compared with the external standard method.Results The relative correction factors(f)of taurodeoxycholic acid,taurochenodeoxycholic acid,glycine porcine deoxycholic acid and glycochenodeoxycholate insuis fellis pulvis were 1.214,1.260 and 1.243,respectively;the relative standard deviations(RSDs)of each index component were good in the ranges of 0.181 6-4.540 6,0.162 9-4.073 4, 0.746 1-18.653 0 and 0.495 9-12.397 5 μg, respectively(r>0.999);The mean recoveries were100.00%,100.11%,97.30% and 98.23%,respectively;the relative standard deviations(RSDs)were 1.11%,4.15%,1.13% and 1.17%,respectively;the RSDs of precision,reproducibility and stability of the method were less than 5.0%. The relative deviations between the calculated values and the measured values of the external standard method were less than 5% for the 4 index components in the 11 batches of suis fellis pulvis,indicating that there was no significant difference bet

关 键 词：猪胆粉 一测多评法 高效液相色谱 含量测定 质量控制 

分 类 号：R282.5[医药卫生—中药学]