当前位置: 首页 > 文章 > HPLC波长切换法同时测定四黄止痢颗粒中5种成分的含量 中兽医医药杂志 2020 (3) 58-62
Position: Home > Articles > Simultaneous determination of five constituents in Sihuangzhili granules by HPLC with switching wavelength Journal of Traditional Chinese Veterinary Medicine 2020 (3) 58-62

HPLC波长切换法同时测定四黄止痢颗粒中5种成分的含量

作  者:
郑举;刘红云;陈静;洪功飞;吴蕾;蔡一杰;明文庆
单  位:
关键词:
四黄止痢颗粒;大黄素;大黄酸;黄芩苷;甘草酸铵;(R,S)-告依春;高效液相色谱;波长切换法
摘  要:
为了建立和完善四黄止痢颗粒的质量标准,建立HPLC波长切换法同时测定四黄止痢颗粒中大黄素、大黄酸、黄芩苷、甘草酸铵、(R,S)-告依春5个成分的含量方法。采用WondaSil C_(18)(4.6 mm×250 mm,5μm),以乙腈(A)-0.05%磷酸水溶液(B)为流动相,梯度洗脱,流速1 mL/min,变换波长检测[0~10 min,245 nm测定(R,S)-告依春;10~25 min,278 nm测定黄芩苷;25-45 min,254 nm测定甘草酸铵、大黄酸、大黄素]。各待测组分分离度良好;(R,S)-告依春、黄芩苷、甘草酸铵、大黄酸、大黄素5个成分的进样量分别在0.0475~0.475μg(r=0.999 3)、0. 067 8~0. 678μg(r=0.999 0)、0.229 0~2.290 0μg(r=0.999 4)、0.016 5~0.165 0μg(r=0.999 8)、0.015 2~0.152 0μg(r=0. 999 5)与峰面积呈良好的线性关系;加样回收率分别为98.2%(RSD=1.6%)、100.7%(RSD=1.0%)、99.5%(RSD=1.1%)、100.5%(RSD=0.8%)、99.3%(RSD=1.0%)。说明该方法可用于四黄止痢颗粒中多指标成分的质量控制。
译  名:
Simultaneous determination of five constituents in Sihuangzhili granules by HPLC with switching wavelength
作  者:
ZHENG Jü;LIU Hongyun;CHEN Jing;HONG Gongfei;WU Lei;CAI Yijie;MING Wenqing;Anhui Province Animal Disease Prevention and Control Center;Anhui Province Institute of Veterinary Drug and Feedstuff;
关键词:
Sihuangzhili granules;;empdin;;rhein;;baicalin;;ammonium glycyrrhizate;;(R,S)-goitrin;;high performance liquid chromatography;;wavelength shift
摘  要:
In order to eatablish and perfecct the quality standard of Sihuangzhili granules,develop an HPLC with switching wavelength for simultaneous determination of empdin,rhein,baicalin,ammonium glycyrrhizate,(R,S)-goitrins in Sihuangzhili granules was established. The chromatographic separation was carried out on WondaSil-C_(18) column(4.6 mm×250 mm,5 μm)with a mobile phase consisting of acetonitrile(A)-0.05% phosphoric acid solution(B) in a gradient mode at a flow rate of 1 mL·min~(-1). The detection wavelength was set at 245 nm for(R,S)-goitrin baicalin in the first 10 min,278 nm for baicalin during 10 ~25 min,254 nm for empdin,rhein and ammonium glycyrrhizate during 25-45 min. Excellent chromatographic separation was achieved and the ranges for linear correlation of(R,S)-goitrin,baicalin,ammonium glycyrrhizate,empdin,rhein were 0.047 5~0. 475 μg(r=0. 999 3),0.0678~0. 678 μg(r=0.999 0),0.229 0~2.290 μg(r=0.99 94),0.016 5~0.165 μg(r=0.999 8),0.015 2~0.152 μg(r=0.9995)respectively. The average recoveries(n=6)of the five components were 98.2%(RSD=1.6%),100.7%(RSD=1.0%),99.5%(RSD=1.1%),100.5%(RSD=0.8%),99.3%(RSD=0.8%). The results showed this method could be used for quality control of multicomponent in Sihuangzhili granules.

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