摘要
目的用HPLC-ELSD同时测定北柴胡中柴胡皂苷A、C、D、B1、B2及山奈苷6种苷类成分的含量。方法 Phenomenex C18(250 mm×4.6 mm, 5μm)色谱柱,流动相:乙腈(A)-0.2%醋酸溶液(B),梯度洗脱(0~8 min, 8%A;8~15 min, 8%~20%A;15~30 min, 20%~35%A;30~40 min, 35%~45%A;40~60 min, 45%~75%A),柱温30℃,流速1.0 mL·min^(-1),载气为氮气,体积流量2.3 L·min^(-1),漂移管温度70℃,增益2。结果柴胡皂苷C、柴胡皂苷A、柴胡皂苷D、柴胡皂苷B2、柴胡皂苷B1、山奈苷在5.48~109.6 mg·L^(-1)(r=0.999 4)、9.76~195.2 mg·L^(-1)(r=0.999 6)、11.98~239.6 mg·L^(-1)(r=0.999 9)、0.532~10.64 mg·L^(-1)(r=0.999 7)、0.35~7.0μg·mL^(-1)(r=0.999 5)、0.254~5.08μg·mL^(-1)(r=0.999 6)范围内的线性关系良好。平均回收率分别为99.1%、99.4%、97.2%、100.4%、100.7%、98.6%。21批北柴胡样品含量范围:柴胡皂苷C 0.093 2%~0.243%、柴胡皂苷A 0.103 8%~0.889 6%、柴胡皂苷D 0.288%~1.084 3%、柴胡皂苷B2 0~0.032 6%、柴胡皂苷B1 0~0.031 26%、山奈苷0~0.010 33%。结论该方法测定北柴胡中柴胡皂苷A、C、D、B1、B2及山奈苷6种苷类成分含量灵敏、准确,分离效果较好,无干扰,可作为完善北柴胡中苷类成分的质量标准评价提供依据。
Objective To establish the method for simultaneous determination of saikosaponin A,saikosaponin C,saikosaponin D,saikosaponin B1,saikosaponin B2,kaempferitrin in Bupleurum chinense DC.by HPLC-ELSD.Methods An Phenomenex C18 column(4.6 mm×250 mm, 5 μm)was used with the mixture of acetonitrile-0.2% acetic acid solution as the mobile phase in gradient elution(0-8 min, 8% A;8-15 min, 8%-20% A;15-30 min, 20%-35%A;30-40 min, 35%-45%A;40-60 min, 45%-75%A).The flow rate was 1.0 mL·min^(-1).The column temperature was 30 ℃.Carrier gas was nitrogen with the volume flow rate for 2.3 L·min^(-1).Drift tube temperature was 70 ℃.Gain was 2.Results The calibration curves of Saikosaponin C,Saikosaponin A,Saikosaponin D,Saikosaponin B2,Saikosaponin B1,Kaempferitrin were in good linearity over the ranges of 5.48-109.6 mg·L^(-1)(r=0.999 4),9.76-195.2 mg·L^(-1)(r=0.999 6),11.98-239.6 mg·L^(-1)(r=0.999 9),0.532-10.64 mg·L^(-1)(r=0.999 7),0.35-7.0 mg·L^(-1)(r=0.999 5),0.254-5.08 mg·L^(-1)(r=0.999 6),respectively.The average recoveries were 99.1%、99.4%、97.2%、100.4%、100.7%、98.6%,respectively.Content range of 21 batches of Bupleurum chinense DC.sample were 0.093 2%-0.243% of Saikosaponin C,0.103 8%-0.889 6% of Saikosaponin A,0.288%-1.084 3% of Saikosaponin D,0-0.032 6% of Saikosaponin B2,0-0.031 26% of Saikosaponin B1,0-0.010 33% of Kaempferitrin.Conclusion The method to determine 6 kinds of glycosides in Bupleurum chinense DC.is sensitive, accurate, separation effect is good, It has no interference, it can provide a basis as evaluation standard for quality of Bupleurum chinense DC.
作者
马守芳
孙江伟
高晓洁
白明学
MA Shoufang;SUN Jiangwei;GAO Xiaojie;BAI Mingxue(Zhengzhou hospital of traditional Chinese medicine,Zhengzhou Henan 450000,China;Henan provincial hospital,Zhengzhou Henan 450000,China)
出处
《沈阳药科大学学报》
CAS
CSCD
北大核心
2021年第8期821-826,共6页
Journal of Shenyang Pharmaceutical University
