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[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-C18色谱柱(250 mm×4.6 mm,5 μm);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 mL/min;柱温:30℃;进样量为10 μL。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、3.29~65.80 μg/mL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。
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[Abstract]
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-C18 column (250 mm×4.6 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.
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