摘要
使用双梯度液相色谱系统和紫外检测器,建立在线二维液相色谱方法,同时测定桂枝茯苓胶囊中芍药苷、丹皮酚、苦杏仁苷和肉桂酸的含量。采用双梯度液相色谱的其中一个泵为一维分离泵,以乙腈为有机相,0.08%磷酸+0.08%三乙胺为水相,梯度洗脱,采用C-18色谱柱(3.0mm×150mm,3μm),流速0.5mL·min-1;利用双梯度液相色谱的另外一个泵为二维分离泵,以乙腈为有机相,以20mmol,pH3.0的磷酸二氢钾为水相,梯度洗脱,采用PA1IC18色谱柱(4.6mm×150mm,3Ixm),流速0.8mL·min-1;检测波长218,230,275nm,采用波长切换方式。芍药苷、丹皮酚、苦杏仁苷和肉桂酸的线性范围分别为5.55~222,6.6~264,3.3~132,0.315~12.6mg·L-1;r分别为0.9997,0.9995,0.9998,0.9997;4个成分的平均回收率在96.12%~103.9%。该方法快速,测定结果准确可靠,可用于评价药物质量。
To establish the online two-dimensional liquid chromatography by using double gradient liquid chromatography sys- tem and UV detector, in order to simultaneously determine the content of paeoniflorin, paenol, amygdaloside and cinnamic acid. A pump of the two-dimensional liquid chromatography was adopted as the one-dimensional separation pump. C18 (3.0 mm × 150 ram, 3 μm) was used as the analytical column, with acetonitrile as the organic phase and 0. 08% phosphoric acid + 0. 08% triethylamine as the aqueous phase for gradient elution at the flow rate of 0. 5 mL · min- 1. Another pump of the two-dimensional liquid chromatography was adopted as the two-dimensional separation pump. PAII C18 was used as the analytical column, with acetonitrile as the organic phase and 20 mmol, pH 3.0 monopotassium phosphate as the aqueous phase for gradient elution at the flow rate of 0. 8 mL · min - 1. The de- tection wavelengths were set at 218, 230, 275 nm by using wavelength time-switching program. The linearity range of paeoniflorin, amygdaloside, paeonol and cinnamic acid were 5.55-222 (r =0.999 7), 6. 6-264(r =0. 999 8), 3.3-132(r =0. 999 5) and 0. 315- 12. 6 mg · L-1 (r =0. 999 7), respectively. The average recoveries of the four components were between 96. 12% and 103.9%. The experiment proved that this method was so rapid avd accurate in determination results that it could be used for evaluating drug quality.
出处
《中国中药杂志》
CAS
CSCD
北大核心
2013年第23期4088-4093,共6页
China Journal of Chinese Materia Medica
关键词
二维液相色谱
双梯度液相色谱
桂枝茯苓胶囊
苦杏仁苷
肉桂酸
two-dimensional liquid chromatography
double gradient liquid chromatography
Guizhi Fuling capsule
amygdal-oside
cinnamic acid