HPLC-ELSD同时测定知母药材中4种主要皂苷的含量

尹茶; 吴婷婷; 朱东亮; 刘职瑞; 柴逸峰

doi:10.3969/j.issn.1006-0111.2012.06.010

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HPLC-ELSD同时测定知母药材中4种主要皂苷的含量

尹茶, 吴婷婷, 朱东亮, 刘职瑞, 柴逸峰

文章导航 > 药学实践与服务 > 2012 > 30(6): 433-436

尹茶, 吴婷婷, 朱东亮, 刘职瑞, 柴逸峰. HPLC-ELSD同时测定知母药材中4种主要皂苷的含量[J]. 药学实践与服务, 2012, 30(6): 433-436. doi: 10.3969/j.issn.1006-0111.2012.06.010

引用本文:

YIN Cha, WU Ting-ting, ZHU Dong-liang, LIU Zhi-rui, CHAI Yi-feng. Determination of four major steroid glycosides in Anemarrhena asphodeloides by HPLC-ELSD[J]. Journal of Pharmaceutical Practice and Service, 2012, 30(6): 433-436. doi: 10.3969/j.issn.1006-0111.2012.06.010

Citation:

YIN Cha, WU Ting-ting, ZHU Dong-liang, LIU Zhi-rui, CHAI Yi-feng. Determination of four major steroid glycosides in Anemarrhena asphodeloides by HPLC-ELSD[J]. Journal of Pharmaceutical Practice and Service, 2012, 30(6): 433-436. doi: 10.3969/j.issn.1006-0111.2012.06.010

HPLC-ELSD同时测定知母药材中4种主要皂苷的含量

doi: 10.3969/j.issn.1006-0111.2012.06.010

1.
第二军医大学出版社, 上海 200433
2.
解放军263医院药械科, 北京 101149
3.
第二军医大学药学院药物分析教研室, 上海 200433

基金项目: 国家自然科学基金(81072614),上海市自然科学基金(09dZ1975100).

Determination of four major steroid glycosides in Anemarrhena asphodeloides by HPLC-ELSD

1.
Publishing house, Second Military Medical University, Shanghai 200433, China
2.
Department of Pharmacy, the 263rd Hospital of PLA, Beijing 101149, China
3.
Department of Pharmaceutical Analysis, School of Pharmacy, Second Military Medical University, Shanghai 200433, China

摘要: 目的建立同时测定知母药材中4种主要皂苷成分的HPLC-ELSD方法。方法采用Agilent Zorbax SB-C₁₈柱(4.6 mm×250 mm, 5 μm), 以水(冰醋酸调节pH 3.3)(A)-乙腈(B)为流动相进行梯度洗脱,0~8 min,12%~23% B;8~25 min,23% B;25~35 min,23%~45% B;35~40 min,45%~95% B。蒸发光散射检测器漂移管温度55℃,以氮气为雾化气,压力为4.0 Bar。结果知母皂苷B、知母皂苷E1、知母皂苷BⅡ、知母皂苷A Ⅲ浓度分别在42.10~252.6 μg/ml(r=0.999 3)、48.80~292.8 μg/mlr=0.999 1)、192.2~1 153 μg/ml(r=0.999 7)、8.512~85.12 μg/ml(r=0.998 5)的范围内呈良好的线性关系。4种成分精密度试验RSD<1%,48 h内稳定性RSD<1%,加样回收率为96.04%~102.8%。结论该含量测定方法简便,分离效果好,能同时测定知母皂苷B、知母皂苷E1、知母皂苷BⅡ和知母皂苷AⅢ 4种有效成分的含量,结果准确可靠。
- 知母 /
- 多成分含量测定 /
- 知母皂苷B /
- 知母皂苷E1 /
- 知母皂苷BII /
- 知母皂苷AIII /
- 高效液相蒸发光检测
Abstract: Objective To develop a new high performance liquid chromatography (HPLC) coupled with Evaporative Light Scattering Detector (ELSD) method for simultaneous determination of four major steroid glycosides (Timosaponin B, Timosaponin E1, Timosaponin BⅡ and Timosaponin AⅢ). Methods HPLC analysis was performed on an Agilent Zorbax SB-C₁₈ column (4.6 mm×250 mm, 5 μm) with a mobile phase of water (adjust to pH 3.3 by acetic acid) (A) and acetonitrile (B). The gradient elution program was as follow:0~8 min, 12%~23% B;8~25 min, 23% B;25~35 min, 23%~45% B;35~40 min, 45%~95% B. The temperature of drift tube was 55℃ and the nebulizer nitrogen flow rate was 4.0 Bar. Results The linearity was obtained over 42.10~252.6 μg/ml (r=0.999 3) for Timosaponin B, 48.80~292.8 μg/ml (r=0.999 1) for Timosaponin E1, 192.2~1153 μg/ml (r=0.999 7) for Timosaponin BⅡ and 8.512~85.12 μg/ml (r=0.998 5) for Timosaponin AⅢ. The RSDs of precision and stability of the samples were both less than 1% in 48 hours. The average recovery was between 96.04%~102.8%. Conclusions The present method, with satisfactory efficacy, was simple which could simultaneously determine multiple steroid glycosides in Anemarrhena asphodeloides Bge. from different areas.
- Anemarrhena asphodeloides Bge. /
- multiple components assaying /
- Timosaponin B /
- Timosaponin E1 /
- Timosaponin BII /
- Timosaponin AIII /
- HPLC-ELSD

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[2]	Zhang JY, Meng ZY, Zhang MY, et al. Effect of six steroidal saponins isolated from Anemarrhenae rhizoma on platelet aggregation and hemolysis in human blood[J]. Clim Chim Acta, 1999, 289(1):79.
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[8]	沙东旭,刘兆妍,张满来,等. HPLC-ELSD测定知母中知母皂苷BⅡ的含量[J]. 药物分析杂志, 2009,29(12):2106.
[9]	陈千良,孙小明,王文全,等. HPLC-ELSD法同时测定知母药材中2种皂苷含量[J]. 中国中药杂志, 2011,36(4):474.
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HPLC-ELSD同时测定知母药材中4种主要皂苷的含量

doi: 10.3969/j.issn.1006-0111.2012.06.010

1. 第二军医大学出版社, 上海 200433

2. 解放军263医院药械科, 北京 101149

3. 第二军医大学药学院药物分析教研室, 上海 200433

基金项目: 国家自然科学基金(81072614),上海市自然科学基金(09dZ1975100).

收稿日期: 2012-05-18
修回日期: 2012-06-26

关键词:

知母 /

摘要: 目的建立同时测定知母药材中4种主要皂苷成分的HPLC-ELSD方法。方法采用Agilent Zorbax SB-C₁₈柱(4.6 mm×250 mm, 5 μm), 以水(冰醋酸调节pH 3.3)(A)-乙腈(B)为流动相进行梯度洗脱,0~8 min,12%~23% B;8~25 min,23% B;25~35 min,23%~45% B;35~40 min,45%~95% B。蒸发光散射检测器漂移管温度55℃,以氮气为雾化气,压力为4.0 Bar。结果知母皂苷B、知母皂苷E1、知母皂苷BⅡ、知母皂苷A Ⅲ浓度分别在42.10~252.6 μg/ml(r=0.999 3)、48.80~292.8 μg/mlr=0.999 1)、192.2~1 153 μg/ml(r=0.999 7)、8.512~85.12 μg/ml(r=0.998 5)的范围内呈良好的线性关系。4种成分精密度试验RSD<1%,48 h内稳定性RSD<1%,加样回收率为96.04%~102.8%。结论该含量测定方法简便,分离效果好,能同时测定知母皂苷B、知母皂苷E1、知母皂苷BⅡ和知母皂苷AⅢ 4种有效成分的含量,结果准确可靠。

English Abstract

Determination of four major steroid glycosides in Anemarrhena asphodeloides by HPLC-ELSD

1. Publishing house, Second Military Medical University, Shanghai 200433, China

2. Department of Pharmacy, the 263rd Hospital of PLA, Beijing 101149, China

3. Department of Pharmaceutical Analysis, School of Pharmacy, Second Military Medical University, Shanghai 200433, China

Received Date: 2012-05-18
Rev Recd Date: 2012-06-26

Keywords:

Abstract: Objective To develop a new high performance liquid chromatography (HPLC) coupled with Evaporative Light Scattering Detector (ELSD) method for simultaneous determination of four major steroid glycosides (Timosaponin B, Timosaponin E1, Timosaponin BⅡ and Timosaponin AⅢ). Methods HPLC analysis was performed on an Agilent Zorbax SB-C₁₈ column (4.6 mm×250 mm, 5 μm) with a mobile phase of water (adjust to pH 3.3 by acetic acid) (A) and acetonitrile (B). The gradient elution program was as follow:0~8 min, 12%~23% B;8~25 min, 23% B;25~35 min, 23%~45% B;35~40 min, 45%~95% B. The temperature of drift tube was 55℃ and the nebulizer nitrogen flow rate was 4.0 Bar. Results The linearity was obtained over 42.10~252.6 μg/ml (r=0.999 3) for Timosaponin B, 48.80~292.8 μg/ml (r=0.999 1) for Timosaponin E1, 192.2~1153 μg/ml (r=0.999 7) for Timosaponin BⅡ and 8.512~85.12 μg/ml (r=0.998 5) for Timosaponin AⅢ. The RSDs of precision and stability of the samples were both less than 1% in 48 hours. The average recovery was between 96.04%~102.8%. Conclusions The present method, with satisfactory efficacy, was simple which could simultaneously determine multiple steroid glycosides in Anemarrhena asphodeloides Bge. from different areas.

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HPLC-ELSD同时测定知母药材中4种主要皂苷的含量

doi: 10.3969/j.issn.1006-0111.2012.06.010

Determination of four major steroid glycosides in Anemarrhena asphodeloides by HPLC-ELSD

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HPLC-ELSD同时测定知母药材中4种主要皂苷的含量

doi: 10.3969/j.issn.1006-0111.2012.06.010

1. 第二军医大学出版社, 上海 200433 2. 解放军263医院药械科, 北京 101149 3. 第二军医大学药学院药物分析教研室, 上海 200433

English Abstract

Determination of four major steroid glycosides in Anemarrhena asphodeloides by HPLC-ELSD

1. Publishing house, Second Military Medical University, Shanghai 200433, China 2. Department of Pharmacy, the 263rd Hospital of PLA, Beijing 101149, China 3. Department of Pharmaceutical Analysis, School of Pharmacy, Second Military Medical University, Shanghai 200433, China

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目录

1. 第二军医大学出版社, 上海 200433

2. 解放军263医院药械科, 北京 101149

3. 第二军医大学药学院药物分析教研室, 上海 200433

1. Publishing house, Second Military Medical University, Shanghai 200433, China

2. Department of Pharmacy, the 263rd Hospital of PLA, Beijing 101149, China

3. Department of Pharmaceutical Analysis, School of Pharmacy, Second Military Medical University, Shanghai 200433, China