二维相关光谱和导数光谱色谱图法识别及解混高效液相色谱二极管阵列色谱峰  

Two dimensional correlation spectroscopy and derivative spectroscopy chromatography for peak identification and unmixing in high-performance liquid chromatography with diode array chromatography

作　　者：芦丽 向健华 方方 宫旭 孙晶 LU Li;XIANG Jianhua;FANG Fang;GONG Xu;SUN Jing(Jiangsu Institute for Food and Drug Control,Nanjing 210019,China;Key Laboratory of Chemical Impurity Spectrometry,National Medical Products Administration,Nanjing 210019,China;School of Traditional Chinese Medicine,China Pharmaceutical University,Nanjing 211198,China)

机构地区：[1]江苏省食品药品监督检验研究院,南京210019 [2]国家药品监督管理局化学药杂质谱重点实验室,南京210019 [3]中国药科大学中药学院,南京211198

出　　处：《化学分析计量》2024年第10期86-93,共8页Chemical Analysis And Meterage

基　　金：江苏省药品监督管理局药品监管科学科研计划项目(202314)。

摘　　要：基于高效液相色谱-二极管阵列检测器(HPLC-DAD)获得的色谱-光谱数据,建立了一种二元完全重叠液相色谱峰的快速解析定量方法:将HPLC-DAD采集的时间t、波长λ、吸光度S的三维光谱色谱数据,光谱经过背景补偿加Savitzky-Golay平滑预处理,得到光谱波长方向的吸光度强度处理值随时间变化的光谱图,与对照品光谱计算光谱相似度,实现重叠峰的快速智能化识别;利用导数光谱色谱图法对预处理的色谱-光谱矩阵进行解析,获得原点波长,再利用二维相关光谱技术提取特征光谱后,得到基于特征光谱的原点波长的色谱流出曲线,进而得到分离后的色谱峰,实现重叠色谱峰的定量测定。该方法充分利用HPLC-DAD获得的三维色谱-光谱数据信息,能够将二元完全重叠色谱峰有效解析分离和定量测定,明显提高解析结果的准确度,并利用色谱工作站实现了数据采集、解析识别、定量分析一体化智能分析,方法简单高效。Based on the chromatographic-spectral data obtained by high performance liquid chromatography-diode array detector(HPLC-DAD),a rapid analytical quantitative method for binary completely overlapping liquid chromatographic peaks was established:The data were processed by background compensation and Savitzky-Golay smoothing preprocessing.The spectral similarity was calculated with the reference spectrum to achieve rapid and intelligent identification of overlapping peaks.Derivative spectrum chromatogram method was used to analyze the pretreated chromatogram-spectrum matrix to obtain the origin wavelength.After the characteristic spectrum was extracted by twodimensional correlation spectrum technology,the chromatogram outflow curve based on the origin wavelength of the characteristic spectrum was obtained,and then the separated chromatographic peak was obtained,so as to realize the quantitative determination of overlapping chromatographic peaks.This method makes full use of the three-dimensional chromatographic-spectral data information obtained by HPLC-DAD,which can effectively analyze and separate and quantitatively determine the completely overlapping chromatographic peaks of two components,and significantly improve the accuracy of the analytical results.The intelligent analysis of data acquisition,analytical identification and quantitative analysis is realized by using chromatographic workstation.The method is simple and efficient.

关 键 词：二维相关谱技术 导数光谱色谱图法 高效液相色谱-二极管阵列检测器 化妆品 重叠峰 识别 解混 

分 类 号：O657.7[理学—分析化学]