摘要
目的建立HPLC波长切换法同时测定肾炎灵胶囊中柳穿鱼叶苷、地榆皂苷-Ⅰ、女贞苷、特女贞苷、去甲蟛蜞菊内酯和蟛蜞菊内酯。方法采用高效液相色谱法,Agilent Extend-C_(18)色谱柱(250 mm×4.6 mm,5μm);流动相:甲醇–乙腈(1∶1)与0.5%冰醋酸溶液,梯度洗脱;检测波长:330 nm(0~14 min检测远柳穿鱼叶苷)、203 nm(14~20 min检测地榆皂苷-Ⅰ)、224 nm(20~29 min检测女贞苷和特女贞苷)、351 nm(29~45 min检测去甲蟛蜞菊内酯和蟛蜞菊内酯);体积流量:0.8 m L/min;柱温:30℃;进样量为10μL。结果柳穿鱼叶苷、地榆皂苷-Ⅰ、女贞苷、特女贞苷、去甲蟛蜞菊内酯和蟛蜞菊内酯分别在2.97~59.40、19.59~391.80、1.78~35.60、4.96~99.20、1.13~22.60、3.29~65.80μg/m L线性关系良好;平均回收率分别为97.97%、99.78%、96.98%、98.52%、98.10%、99.10%,RSD值分别为0.76%、1.01%、0.66%、1.22%、0.95%、1.56%。结论该方法简便,分析速度快,为完善肾炎灵胶囊的质量标准提供参考。
Objective To develop an HPLC wavelength switching method for simultaneous determination of pectolinarin, ziyu-glycoside I, ligustroflavone, specnuezhenide, demethylwedelolactone, and wedelolactone, in Shenyanling Capsules. Methods HPLC method was adopted for the analysis on Agilent Extend-C18column （250 mm x4.6 mm, 5 μm）. The mobile phase consisted of methanol -acetonitrile （1：1） and 0.5% glacial acetic acid solution with gradient elution. The detection wavelengths were 330 nm in 0 — 14 min （determination of pectolinarin）, 203 nm in 14 — 20 min （determination of ziyu-glycoside I）, 224 nm in 20 — 29 min （ determination of ligustroflavone and specnuezhenide） , and 351 nm in 29 — 45 min （ determination of demethylwedelolactone and wedelolactone）.The flow rate was 0.8 mL/min, and the column temperature was set at 30 ℃ with injection volume of 10 μL. Results Pectolinarin, ziyu-glycoside I, ligustroflavone, specnuezhenide, demethylwedelolactone and wedelolactone had good linearity in the ranges of 2.97 — 59.40 , 19.59 — 391.80, 1.78 — 35.60, 4.96 — 99.20, 1.13 — 22.60, and 3.29 — 65.80 μg/mL, respectively. The average recoveries were 97.97%, 99.78%, 96.98%, 98.52%, 98.10%, and 99.10%, with RSD of 0.76%, 1.01%, 0.66%, 1.22 %, 0.95%, and 1.56%, respectively. Conclusions The method is simple and rapid which provides reference for quality standard of Shenyanling Capsules.
作者
王启明
魏谭军
贾旭明
WANG Qi-ming WEI Tan-jun JIA Xu-ming(Dazhou Hospital of Integrated TCM ＆ WM, Dazhou 635000, China Dazhou Institute for Food and Drug Control, Dazhou 635000, China)
出处
《现代药物与临床》
CAS
2017年第10期1824-1827,共4页
Drugs & Clinic
