复方石韦片中3种皂苷类成分的含量测定及其制剂过程中的转移率研究
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摘要
目的采用高效液相色谱-蒸发光散射检测器法(HPLC-ELSD)建立复方石韦片中3种皂苷类成分黄芪皂苷I、II和黄芪甲苷的含量测定方法,并考察这3种皂苷类成分在复方石韦片制剂工艺过程中的转移率,完善与提升复方石韦片的质量控制方法。方法采用HPLC-ELSD法,使用Agilent 5-HC C_(18)(2)色谱柱(250 mm×4.6 mm,5μm),以乙腈-水为流动相进行梯度洗脱,体积流量1.0 mL/min,柱温30℃,进样量20μL。ELSD参数:载气体积流量1.5 L/min,漂移管温度90℃,同时测定黄芪药材及复方石韦片成品、颗粒、浸膏样品中黄芪皂苷I、II及黄芪甲苷的含量,并计算3种皂苷类成分在复方石韦片制剂过程中的转移率。结果建立了复方石韦片及其制剂过程中黄芪皂苷I、II和黄芪甲苷的含量测定方法,该条件下3个成分均达到基线分离,线性关系良好,平均加样回收率分别为99.58%、99.31%、99.51%,RSD值分别为3.0%、2.5%、2.5%。黄芪皂苷I在制剂过程中转移率较低,黄芪甲苷在制剂过程中转移率较高,且均大于100%。结论本研究建立同时测定复方石韦片中黄芪皂苷I、II和黄芪甲苷3种皂苷类成分的方法重现性好,专属性强,简便易行,同时可用于考察复方石韦片制剂工艺过程中3种皂苷类成分的转移率,完善了复方石韦片中皂苷类成分的质量控制标准,并为其他含黄芪中药制剂的质量控制提供参考。
Objective High performance liquid chromatography-evaporative light scattering detector(HPLC-ELSD) method was used to establish the determination method for the three kinds of saponins(astragaloside I, II, and IV) in Compound Shiwei Tablets(CST),and investigate the three saponins components' s transfer rate in the preparation process of CST in order to improve the quality control method of CST. Methods A HPLC-ELSD method was operated on the column of Agilent 5-HC C_(18)(2)(250 mm × 4.6 mm, 5 μm),with acetonitrile-water as the mobile phase for gradient elution, at a flow rate of 1.0 mL/min, with column temperature of 30 ℃ and injection volume of 20 μL. The ELSD parameters were as follow: the carrier gas flow rate was 1.5 L/min, the drift tube temperature was 90 ℃. Determinate the content of astragaloside I, II, and IV in products, granules and extracts of CST, and calculate the transfer rate of three saponins in the preparation process of CST. Results A method for the determination of astragaloside I, II, and IV in CST was established. Under this condition, all three components reached baseline separation with good linear relationship. The average recovery rates were 99.58%, 99.31% and 99.51%, and RSD values were 3.0%, 2.5% and 2.5%, respectively. Astragaloside I had lower transfer rate during the preparation process, and the transfer rate of astragaloside IV was the higher in the preparation process, both of which were greater than 100%. Conclusion This study established a method for simultaneous determination of three kinds of saponins of astragaloside I, II, and IV in CST. The method has good reproducibility and strong specificity, which is simple and easy,and can be used to inspect the transfer rates of three kinds of saponins in the preparation process and improve the quality control standard of saponins in CST, and provide reference for the quality control of other traditional Chinese medicine preparations containing astragalus.
Objective High performance liquid chromatography-evaporative light scattering detector(HPLC-ELSD) method was used to establish the determination method for the three kinds of saponins(astragaloside I, II, and IV) in Compound Shiwei Tablets(CST),and investigate the three saponins components' s transfer rate in the preparation process of CST in order to improve the quality control method of CST. Methods A HPLC-ELSD method was operated on the column of Agilent 5-HC C_(18)(2)(250 mm × 4.6 mm, 5 μm),with acetonitrile-water as the mobile phase for gradient elution, at a flow rate of 1.0 mL/min, with column temperature of 30 ℃ and injection volume of 20 μL. The ELSD parameters were as follow: the carrier gas flow rate was 1.5 L/min, the drift tube temperature was 90 ℃. Determinate the content of astragaloside I, II, and IV in products, granules and extracts of CST, and calculate the transfer rate of three saponins in the preparation process of CST. Results A method for the determination of astragaloside I, II, and IV in CST was established. Under this condition, all three components reached baseline separation with good linear relationship. The average recovery rates were 99.58%, 99.31% and 99.51%, and RSD values were 3.0%, 2.5% and 2.5%, respectively. Astragaloside I had lower transfer rate during the preparation process, and the transfer rate of astragaloside IV was the higher in the preparation process, both of which were greater than 100%. Conclusion This study established a method for simultaneous determination of three kinds of saponins of astragaloside I, II, and IV in CST. The method has good reproducibility and strong specificity, which is simple and easy,and can be used to inspect the transfer rates of three kinds of saponins in the preparation process and improve the quality control standard of saponins in CST, and provide reference for the quality control of other traditional Chinese medicine preparations containing astragalus.
引文
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[2]李忠思,李云霞,商春丽.复方石韦片的质量控制[J].现代药物与临床,2010,25(3):220-223.
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[4]秦雪梅,李震宇,孙海峰,等.我国黄芪药材资源现状与分析[J].中国中药杂志,2013,38(19):3234-3238.
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[11]史静超,李浩铮,王永辉,等.不同产地蒙古黄芪中黄芪甲苷、黄芪皂苷I、黄芪皂苷II和黄芪皂苷III含量的比较与分析[J].世界科学技术-中医药现代化,2015,17(5):1016-1021.
[12]丁菲菲,邓雁如,张晓静,等.HPLC-ELSD法同时测定黄芪及金芪降糖片中5种皂苷类成分的含量[J].中药材,2015,38(1):156-159.
[13]褚莉,段树卿,宋佳,等.复方石韦片HPLC指纹图谱的建立及其在制剂过程中的应用[J].中草药,2019,50(2):396-401.
[14]史志辉,肖会敏,何悦,等.皮肤病血毒片制备中7种成分转移率研究[J].安徽医药,2017,21(7):1204-1209.
[15]赵静,何倩灵,谭琴,等.基于木蝴蝶药材特征图谱研究其主要成分在芪贞慢咽宁颗粒工艺过程中的含量变化[J].中药材,2017,40(7):1665-1669.
[16]路新华,龙晓英,罗佳波,等.穿心莲注射液制备工艺过程中3种穿心莲内酯含量变化追踪[J].中国实验方剂学杂志,2014,20(9):43-46.
[17]覃红萍,桑彤,黄红泓.不同碱化处理方法对黄芪中四种皂苷类成分含量影响的研究[J].中国卫生检验杂志,2012,22(10):2310-2313.
[18]陈有根,辛敏通,杨滨,等.黄芪药材中黄芪甲苷含量测定方法的改进[J].中国新药杂志,2008,(21):1857-1859.
[19]刘和平,彭招华,张润容,等.黄芪药材中黄芪甲苷UPLC-ELSD含量测定方法的优化[J].中国实验方剂学杂志,2015,21(5):92-94.
[20]郑娜,师亚玲,吉艳霞,等.温度和酸度对黄芪皂苷IV、III、I稳定性和转化的影响[J].中南药学,2014,12(11):1062-1065.
[2]李忠思,李云霞,商春丽.复方石韦片的质量控制[J].现代药物与临床,2010,25(3):220-223.
[3]李云章.山庄牌复方石韦片[J].中草药,1997,28(3):190.
[4]秦雪梅,李震宇,孙海峰,等.我国黄芪药材资源现状与分析[J].中国中药杂志,2013,38(19):3234-3238.
[5]高云峰,高娜.黄芪生理活性成分及其药理作用研究进展[J].新农业,2017,20(1):20-21.
[6]唐冕,许晓芬.药用黄芪皂苷类化学成分及药理作用研究进展[J].中医药导报,2018,24(20):117-122.
[7]王靖雯,徐伟,肖朝江,等.灰毛康定黄芪地下部分化学成分研究[J].中草药,2019,50(7):1527-1531.
[8]杜国军,秦雪梅,李震宇,等.蒙古黄芪主产区2种不同种植模式黄芪药材的质量比较[J].中草药,2013,44(23):3386-3393.
[9]许京,叶迎,王瑞海,等.甘肃一年生、二年生红芪和黄芪HPLC-ELSD指纹图谱比较[J].中国实验方剂学杂志,2018,24(6):71-76.
[10]崔雪莹,刘阿娜,陈迩东,等.HPLC-ELSD法测定黄芪中四种皂苷类成分的含量[J].山东中医杂志,2017,36(5):411-413.
[11]史静超,李浩铮,王永辉,等.不同产地蒙古黄芪中黄芪甲苷、黄芪皂苷I、黄芪皂苷II和黄芪皂苷III含量的比较与分析[J].世界科学技术-中医药现代化,2015,17(5):1016-1021.
[12]丁菲菲,邓雁如,张晓静,等.HPLC-ELSD法同时测定黄芪及金芪降糖片中5种皂苷类成分的含量[J].中药材,2015,38(1):156-159.
[13]褚莉,段树卿,宋佳,等.复方石韦片HPLC指纹图谱的建立及其在制剂过程中的应用[J].中草药,2019,50(2):396-401.
[14]史志辉,肖会敏,何悦,等.皮肤病血毒片制备中7种成分转移率研究[J].安徽医药,2017,21(7):1204-1209.
[15]赵静,何倩灵,谭琴,等.基于木蝴蝶药材特征图谱研究其主要成分在芪贞慢咽宁颗粒工艺过程中的含量变化[J].中药材,2017,40(7):1665-1669.
[16]路新华,龙晓英,罗佳波,等.穿心莲注射液制备工艺过程中3种穿心莲内酯含量变化追踪[J].中国实验方剂学杂志,2014,20(9):43-46.
[17]覃红萍,桑彤,黄红泓.不同碱化处理方法对黄芪中四种皂苷类成分含量影响的研究[J].中国卫生检验杂志,2012,22(10):2310-2313.
[18]陈有根,辛敏通,杨滨,等.黄芪药材中黄芪甲苷含量测定方法的改进[J].中国新药杂志,2008,(21):1857-1859.
[19]刘和平,彭招华,张润容,等.黄芪药材中黄芪甲苷UPLC-ELSD含量测定方法的优化[J].中国实验方剂学杂志,2015,21(5):92-94.
[20]郑娜,师亚玲,吉艳霞,等.温度和酸度对黄芪皂苷IV、III、I稳定性和转化的影响[J].中南药学,2014,12(11):1062-1065.