炒九香虫配方颗粒含量测定和特征图谱测定方法研究  

Study on the Method of Content Determination and Characteristic Atlas Determination of Stir-Baked Aspongopus Formula Granules

作　　者：马智玲 王晓亚 杜微波 张志强 沈建梅 Ma Zhiling;Wang Xiaoya;Du Weibo;Zhang Zhiqiang;Shen Jianmei(Beijing Tcmages Pharmaceutical Co.,Ltd.,Beijing 101301,China;Traditional Chinese Medicine Formula Particles Key Technology National United Engineering Research Center,Beijing 101301,China;Beijing Engineering and Technology Research Center of Formula Granules of Chinese Medicine,Beijing 101301,China)

机构地区：[1]北京康仁堂药业有限公司,北京101301 [2]中药配方颗粒关键技术国家地方联合工程研究中心,北京101301 [3]北京市中药配方颗粒工程技术研究中心,北京101301

出　　处：《山东化工》2023年第8期167-170,共4页Shandong Chemical Industry

摘　　要：目的:建立炒九香虫配方颗粒含量测定和特征图谱分析方法。方法:采用高效液相色谱法(UPLC)对炒九香虫配方颗粒中的犬尿喹啉酸进行含量测定,流动相为乙腈-0.1%甲酸水溶液,流速为0.4 mL·min^(-1),柱温为30℃,检测波长为240 nm。更换检测波长为254 nm建立炒九香虫配方颗粒的特征图谱,质谱解析指认共有峰。结果犬尿喹啉酸在2.92~292.64μg/mL呈良好的线性关系(R 2=0.9995),平均回收率97.2%(RSD为3.6%,n=9),精密度、稳定性、重复性的RSD均小于2%;炒九香虫配方颗粒特征图谱中有5个共有峰,其中3个成分指认为犬尿喹啉酸(2号)、1,2-脱氢-N-乙酰基多巴胺(3号)、九香虫酰胺A(5号)。结论:所建立的方法操作简便、专属性和重复性好,准确度高,可用于炒九香虫配方颗粒的质量控制,为炒九香虫配方颗粒的质量标准制定提供实验参考。Objective:To establish a method for determination and characteristic spectrum analysis of Stir-baked Aspongopus formula granules.Methods:The content of kynurenic acid in Stir-baked Aspongopus formula granules was determined by High-performance liquid chromatography(UPLC)methed,The mobile phase was acetonitrile-0.1%formic acid aqueous solution,the flow rate was 0.4 mL·min^(-1),the column temperature was 30℃,and the detection wavelength was 240 nm.The detection wavelength was changed to 254 nm to establish the characteristic spectrum of Fried Hyacinth Formula Granule,and the common peak was identified by mass spectrometry.Results:There was a good linear relationship between kynurenic acid in canine urine from 2.92 g/mL to 292.64 g/mL(R 2=0.9995).The average recovery was 97.2%(RSD=3.6%,n=9),The RSD of precision,stability and repeatability tests were less than 2.0%.There were 5 common peaks in the Characteristic Spectra of the Stir-baked Aspongopus Formula Granules,among which three components were identified as kynurenic acid(No.2),1,2-dehydro-N-acetyldopamine(No.3)andaspongamide A(No.5).Conclusion:The method is simple,specific,repeatable and accurate.It can be used for the quality control of Fried Jiuxiangchong Granule and provide reference for the quality standard of Stir-baked Aspongopus formula Granule.

关 键 词：炒九香虫 配方颗粒 犬尿喹啉酸 含量测定 特征图谱 

分 类 号：TQ461[化学工程—制药化工]