UPLC-PDA同时测定柴胡中8种多炔类化合物的含量

Quantitative analysis of eight polyacetylenes derived from Bupleuri Radix by ultra-performance liquid chromatography coupled with photodiode array detector

建立柴胡中多炔类化合物定量测定方法。采用Waters BEH C_(18)柱(2.1 mm×100 mm,1.7μm),甲醇-水溶液为流动相进行梯度洗脱,体积流量0.3 m L·min^(-1),检测波长315 nm,柱温40℃。采用传统提取分离方法,制备得8种多炔类化合物,其中化合物7和8为新化合物。在线性范围内8种多炔类化合物线性良好(r>0.999 0);日内精密度和日间精密度均小于1.9%;平均回收率范围在93.21%~108.4%。同时,对收集到的17个柴胡药材样品进行定量测定,发现不同种属、不同产地柴胡中所含多炔类成分种类及含量差异较大。建立的含量测定方法具有良好的精密度、准确度、重复性,可用于柴胡中多炔类化合物的定量测定及质量控制,为选择多炔类成分较多的柴胡药材提供一种简便方法。

To establish quantitative methods for determination of polyacetylenes in Bupleuri Radix,an ultra-performance liquid chromatography method coupled with photodiode array detector（ UPLC-PDA） was developed. The analysis was performed on a Waters BEH C18 column（2. 1 mm × 100 mm,1. 7 μm） using a gradient system of methanol and water. The flow rate was 0. 3 m L·min^-1 and the detection wavelength was 315 nm. Eight polyacetylenes were prepared using traditional extraction and isolation method,of which compounds 7 and 8 were two new polyacetylenes. All calibration curves showed good linearity（ r 0. 999 0） within the concentration range. Both the intra-and inter-day precisions for eight analytes were less than 1. 9%,respectively,with the mean recovery at the range of 93. 21%-108. 4%. Meanwhile,17 bupleurum samples were examined with this process. The results showed a variety either the chemotaxonomic or content of polyacetylenes. The method indicated good linearity,limit of detection and quantification,precision,accuracy and recovery. The developed method allows quantitative assessment and quality control of polyacetylenes,and might be a good alternative according to detection levels in polyacetylenes from Bupleurum Radix.