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纸质出版日期:2016
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卢君蓉, 李文兵, 季宁平, 等. 基于多成分同时检测的良附丸质量控制[J]. 中国实验方剂学杂志, 2016,22(22):49-53.
LU Jun-rong, LI Wen-bing, JI Ning-ping, et al. Quality Control of Liangfuwan Based on Multi-components Determination[J]. Chinese journal of experimental traditional medical formulae, 2016, 22(22): 49-53.
卢君蓉, 李文兵, 季宁平, 等. 基于多成分同时检测的良附丸质量控制[J]. 中国实验方剂学杂志, 2016,22(22):49-53. DOI: 10.13422/j.cnki.syfjx.2016220049.
LU Jun-rong, LI Wen-bing, JI Ning-ping, et al. Quality Control of Liangfuwan Based on Multi-components Determination[J]. Chinese journal of experimental traditional medical formulae, 2016, 22(22): 49-53. DOI: 10.13422/j.cnki.syfjx.2016220049.
目的:建立一种同时检测良附丸中主要成分的定性、定量方法,为其质量控制标准提供参考。方法:采用薄层色谱法(TLC),以硅胶GF254为薄层板,石油醚(60~90℃)-乙酸乙酯(5:1)为展开剂,于254,365 nm波长下检视,对良附丸中高良姜素、山柰素、香附烯酮、圆柚酮和α-香附酮5种特征性成分同时进行定性鉴别;高效液相色谱法(HPLC),采用Phenomenex C18色谱柱(4.6 mm×250 mm,5 μm),流动相甲醇(A)-0.2%磷酸水溶液(B)梯度洗脱(0~30 min,55% A;30~45 min,55%~70% A;45~70 min,70% A),检测波长242 nm,流速1.0 mL·min-1,柱温30℃,对5种特征性成分含量进行同时测定。结果:该法可在同一条件下实现对良附丸中5个特征性成分的同时检测,不同批次良附丸的高良姜素质量分数在3.33~3.81 mg·g-1,山柰素质量分数在1.13~1.29 mg·g-1,香附烯酮质量分数在0.57~1.12 mg·g-1,圆柚酮质量分数在0.02~0.09 mg·g-1,α-香附酮质量分数在0.36~0.54 mg·g-1。结论:该方法简便、可行、重复性好,可为进一步完善良附丸质量标准,为其二次开发奠定基础。
Objective: To establish a qualitative and quantitative method which can simultaneously measure the main components of Liangfuwan
and provide a reference for its quality control. Method: Thin layer chromatography (TLC) method was used for qualitative determination of 5 characteristic components:galangin
kaempferol
cyperotundone
nootkatone and α-cyperone. In the TLC method
silica gel GF254 was used as thin layer plate and petroleum ether (60-90℃)-ethyl acetate (5:1) was used as the developing agent; the results were viewed under the wavelength of 254 nm and 365 nm. High performance liquid chromatography (HPLC) determination method was established to simultaneously determine the contents of the above components. HPLC method was performed on Phenomenex C18 column (4.6 mm×250 mm
5 μm)
with methanol (A)-0.2%phosphoric acid aqueous solution (B) as mobile phase for gradient elution (0-30 min
55%A; 30-45 min
55%-70%A; 45-70 min
70% A) at a flow of 1.0 mL·min-1. The detection wavelength was 242 nm and column temperature was 30℃. Result: The method could be used to simultaneously determine five components in Liangfuwan under the same condition
and the mass fraction was 3.33-3.81
1.13-1.29
0.57-1.12
0.02-0.09
0.36-0.54 mg·g-1 respectively for galangin
kaempferol
cyperotundone
nootkatone and α-cyperone. Conclusion: This method is simple
feasible and reproducible
which can provide a good reference for further improvement of quality control of Liangfuwan.
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