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纸质出版日期:2014
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袁涛, 王森, 管咏梅, 等. HPLC同时测定奇正消痛贴膏中3种成分的含量[J]. 中国实验方剂学杂志, 2014,20(19):72-75.
YUAN Tao, WANG Sen, GUAN Yong-mei, et al. HPLC Wavelength Switching Simultaneous Determination of 3 Active Components in Qizheng Xiaotong Plaster[J]. Chinese journal of experimental traditional medical formulae, 2014, 20(19): 72-75.
袁涛, 王森, 管咏梅, 等. HPLC同时测定奇正消痛贴膏中3种成分的含量[J]. 中国实验方剂学杂志, 2014,20(19):72-75. DOI: 10.13422/j.cnki.syfjx.2014190072.
YUAN Tao, WANG Sen, GUAN Yong-mei, et al. HPLC Wavelength Switching Simultaneous Determination of 3 Active Components in Qizheng Xiaotong Plaster[J]. Chinese journal of experimental traditional medical formulae, 2014, 20(19): 72-75. DOI: 10.13422/j.cnki.syfjx.2014190072.
目的:建立RP-HPLC同时测定奇正消痛贴膏中山栀苷甲酯、8-O-乙酰山栀苷甲酯、2’,4’-二羟基查尔酮的含量。方法:采用Syncronis C18色谱柱(4.6 mm×250 mm,5 μm),以乙腈(A)-0.05%磷酸水梯度洗脱(B)(0~12 min 11%A;12~17 min,11%~18%A;17~25 min,18%A;25~40 min,60%A),检测波长235 nm(0~24 min,检测山栀苷甲酯、8-O-乙酰山栀苷甲酯)和365 nm(24.01~50 min,检测2’,4’-二羟基查尔酮)。结果:在48 min内消痛贴膏中的山栀苷甲酯、8-O-乙酰山栀苷甲酯、2’,4’-二羟基查尔酮分离良好,依次在15.12~90.72(r=0.999 9),15.90~95.40(r=0.999 9),4.50~27.00 mg·L-1(r=0.999 9) 呈良好的线性关系,平均加样回收率分别为97.12%,104.90%,105.63%。结论:该方法简便、可靠、重复性好,适用于测定奇正消痛贴膏中山栀苷甲酯、8-O-乙酰山栀苷甲酯、2’,4’-二羟基查尔酮的含量,可用于制剂质量控制。
Objective: The aim of this study was to develop an HPLC method with programmed UV detection wavelength for the simultaneous determination of shanzhiside methyl ester
8-O-acetyl shanzhiside methyl ester and 2'
4'-dihydroxy chalcone in Qizheng Xiaotong plaster. Method: The samples were separated on a Syncronis C18 Dim.(mm) column(4. 6 mm×250 mm
5 μm)by a linear gradient elution(0-12 min
11% A; 12-17 min
11%-18% A; 17-25 min
18% A; 25-40 min
60% A)using acetonitrile (A) and 0.05% [phosphoric acid solution] (B) as mobile phase at a flow rate of 1.0 mL·min-1 and the eluate was detected by programmed wavelength (0-24 min
235 nm for shanzhiside methyl ester
8-O-acetyl shanzhiside methyl ester;24.01-50 min
365 nm for 2'
4'-dihydroxy chalcone ). Result: Shanzhiside methyl ester
8-O-acetyl shanzhiside methyl ester and 2'
4'-dihydroxy chalcone were well separated excellentlyin less than 48 min within the linear range of 15.12-90.72 mg(r=0.999 9)
15.90-95.40 mg(r=0.999 9) and 4.50-27.00 mg (r=0.999 9)
respectively. The average recoveries of the compounds listed above were 97.12%
104.90%
and 105.63%
respectively. Conclusion: Verys Satisfactory and reproducible results arewere obtained for the simultaneous determination of the 3 active compounds in Qizheng Xiaotong plaster.
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