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纸质出版日期:2012
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王宏洁, 赵海誉, 司南, 等. HPLC测定不同种蟾皮药材中不同部位蟾蜍噻咛的含量[J]. 中国实验方剂学杂志, 2012,18(11):66-68.
WANG Hong-jie, ZHAO Hai-yu, SI Nan, et al. Determination of Bufothionine in Different Parts from Two Species of Toad Skin Using HPLC[J]. Chinese journal of experimental traditional medical formulae, 2012, 18(11): 66-68.
王宏洁, 赵海誉, 司南, 等. HPLC测定不同种蟾皮药材中不同部位蟾蜍噻咛的含量[J]. 中国实验方剂学杂志, 2012,18(11):66-68. DOI:
WANG Hong-jie, ZHAO Hai-yu, SI Nan, et al. Determination of Bufothionine in Different Parts from Two Species of Toad Skin Using HPLC[J]. Chinese journal of experimental traditional medical formulae, 2012, 18(11): 66-68. DOI:
目的: 对不同种蟾皮不同部位中蟾蜍噻咛的含量进行了比较研究。 方法 :采用高效液相色谱法测定了不同种蟾皮中不同部位蟾蜍噻咛的含量。样品中蟾蜍噻咛峰通过与对照品进行HPLC-DAD 3D及HPLC-MS-MS比对分析进行了确定。提取方法通过正交试验确定为50倍量50%甲醇超声60 min。样品分析选用了WondsilTM C18 色谱柱(4.6 mm×250 mm
5 μm)
以乙腈-水(6 :94)为流动相
检测波长226 nm。 结果 :该方法具有良好的线性(r=0.999 7)、精密度(RSD
0.59%)、稳定性(RSD
0.72%)和重复性(RSD
1.56%);平均加样回收率为98.57%
RSD为2.03%
表明该方法准确可靠。经测定
中华大蟾蜍与黑框蟾蜍不同部位均含有蟾蜍噻咛成分
含量为0.07%~0.17%。 结论 :蟾蜍噻咛在不同种蟾皮药材中的不同部位含量差异不大。
Objective: To determine bufothionine in different parts of the dried toad skin from two species. Method: A quantification method was developed by HPLC with photodiode array (PDA) detection. Bufothionine was identified unambiguously by HPLC-DAD 3D and HPLC-MS-MS analysis in comparison with reference standard. The extraction method was optimized as 50 times 50% MeOH ultrasonic 60 min. The analysis was performed on WondsilTM C18 column (4.6 mm×250 mm
5 μm) with ACN-H2O (6 : 94) as mobile phase and detection wavelength was at 226 nm. Result : The samples were analyzed with good linear regression relationship (r=0.999 7)
precisions (RSD
0.59%)
repeatability (RSD
1.56%)
stability (RSD
0.73%) and recovery (98.57%; RSD
2.03%). Bufothionine was detected in different parts of toad skin from Bufobufo gargarizans cantor and Bufo melanostictus Schneider. The contents were from 0.07% to 0.17%. Conclusion : The content of bufothionine revealed no significant differences among the different parts in these two species of toad skin.
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