炒椿皮配方颗粒HPLC特征图谱及含量测定方法的建立  

Establishment of Characteristic HPLC Chromatogram and Content Determination Method of Processed Ailanthi Cortex Formula Granules

作　　者：杨明霞 王永丽[1,2] 侴桂新 YANG Ming-xia;WANG Yong-li;CHOU Gui-xin(Institute of Chinese Materia Medica,Shanghai University of Traditional Chinese Medicine,Shanghai 201203,China;Shanghai R&D Centre for Standardization of Chinese Medicines,Shanghai 201203,China)

机构地区：[1]上海中医药大学中药研究所,上海201203 [2]上海中药标准化研究中心,上海201203

出　　处：《中国现代中药》2023年第5期1079-1085,共7页Modern Chinese Medicine

基　　金：中药组分及对照品制备基金项目(2019ZX09735002-004)。

摘　　要：目的:建立炒椿皮配方颗粒高效液相色谱法(HPLC)特征图谱及含量测定方法。方法:采用HPLC,色谱柱为资生堂MGⅡC_(18)(250 mm×4.6 mm,5μm),以乙腈-0.1%磷酸水溶液为流动相梯度洗脱,流速为1.0 mL·min^(-1),柱温为30℃,检测波长为254 nm,进样量为10μL,以铁屎米酮为参照,建立炒椿皮配方颗粒的特征图谱,利用对照品对其共有峰进行指认,并对炒椿皮饮片、标准汤剂和配方颗粒的相关性进行评价。同时以铁屎米酮为对照品,以乙腈-0.1%磷酸水溶液(29∶71)为流动相,检测波长为360 nm,进样量为20μL,建立其含量测定方法。结果:所建立的炒椿皮配方颗粒HPLC特征图谱共确定了9个特征峰,指认了其中3个,各样品特征图谱与对照图谱相似度为0.984~1.000。含量测定结果表明,铁屎米酮质量浓度为1.018~12.216μg·mL^(-1)时与峰面积呈良好线性关系;铁屎米酮平均加样回收率为99.22%,RSD<2%;10批炒椿皮配方颗粒中铁屎米酮质量分数为0.2097~0.2159 mg·g^(-1)。结论:建立的特征图谱及含量测定方法操作简便、专属性强、重复性好,可为炒椿皮配方颗粒的质量控制提供参考。Objective:To establish the characteristic High Performance Liquid Chromatography(HPLC)chromatogram and content determination method of processed Ailanthi Cortex formula granules.Methods:HPLC analysis was performed using SHISEIDO MGⅡC_(18) column(250 mm×4.6 mm,5μm).Gradient elution was carried out using acetonitrile-0.1%phosphoric acid solution as the mobile phase at a flow rate of 1.0 mL·min^(-1).The detection wavelength was 254 nm and the sample size was 10μL.The characteristic chromatogram of processed Ailanthi Cortex formula granules was established with canthin-6-one as the reference,and the common peaks were identified,while the correlation between the processed Ailanthi Cortex decoction pieces,the standard decoction of processed Ailanthi Cortex and processed Ailanthi Cortex formula granules was evaluated.Moreover,the content determination method was established with canthin-6-one as the standard and acetonitrile-0.1%phosphoric acid solution(29:71)as the mobile phase.The detection wavelength was 360 nm and the sample size was 20μL.Results:A total of nine characteristic peaks were determined in the established characteristic HPLC chromatogram of processed Ailanthi Cortex formula granules,and three of them were identified.The similarities between the characteristic chromatograms of the samples and the reference chromatogram were 0.984-1.000.The content determination results showed that there was a good linear relationship between the peak area and the concentration of canthin-6-one in the range of 1.018-12.216μg·mL^(-1),the average recovery rate was 99.22%with the RSD lower than 2%.The mass fraction of canthin-6-one in the 10 batches of processed Ailanthi Cortex formula granules was 0.2097-0.2159 mg·g^(-1).Conclusion:The established characteristic chromatogram and the content determination method are convenient,specific and reproducible,which may provide references for quality control of processed Ailanthi Cortex formula granules.

关 键 词：炒椿皮 配方颗粒 特征图谱 含量测定 铁屎米酮 

分 类 号：R286[医药卫生—中药学]