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At-Line Monitoring of the Extraction Process of Rosmarini Folium via Wet Chemical Assays UHPLC Analysis and Newly Developed Near-Infrared Spectroscopic Analysis Methods

机译:在线监测迷迭香叶提取过程的湿化学分析UHPLC分析和最新开发的近红外光谱分析方法

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摘要

The present study demonstrates the applicability of at-line monitoring of the extraction process of Rosmarinus officinalis L. leaves (Rosmarini folium) and the development of near-infrared (NIR) spectroscopic analysis methods. Therefore, whole dried Rosmarini folium samples were extracted by maceration with 70% (v/v) ethanol. For the experimental design three different specimen-taking plans were chosen. At first, monitoring was carried out using three common analytical methods: (a) total hydroxycinnamic derivatives according to the European Pharmacopoeia, (b) total phenolic content according to Folin–Ciocalteu, and (c) rosmarinic acid content measured by UHPLC-UV analysis. Precision validation of the wet chemical assays revealed a repeatability of (a) 0.12% relative standard deviation (RSD), (b) 1.1% RSD, and (c) 0.28% RSD, as well as an intermediate precision of (a) 4.1% RSD, (b) 1.3% RSD, and (c) 0.55% RSD. The collected extracts were analyzed with a NIR spectrometer using a temperature-controlled liquid attachment. Samples were measured in transmission mode with an optical path length of 1 mm. The combination of the recorded spectra and the previously obtained analytical reference values in conjunction with multivariate data analysis enabled the successful establishment of partial least squares regression (PLSR) models. Coefficients of determination (R2) were: (a) 0.94, (b) 0.96, and (c) 0.93 (obtained by test-set validation). Since Pearson correlation analysis revealed that the reference analyses correlated with each other just one of the PSLR models is required. Therefore, it is suggested that PLSR model (b) be used for monitoring the extraction process of Rosmarini folium. The application of NIR spectroscopy provides a fast and non-invasive alternative analysis method, which can subsequently be implemented for on- or in-line process control.
机译:本研究证明了迷迭香叶(Rosmarini folium)的提取过程的在线监测和近红外(NIR)光谱分析方法的发展的适用性。因此,通过用70%(v / v)乙醇浸软提取整个干燥的迷迭香叶样品。对于实验设计,选择了三个不同的标本采集计划。首先,使用三种常见的分析方法进行监测:(a)根据欧洲药典的总羟基肉桂酸衍生物,(b)根据Folin–Ciocalteu的总酚含量,以及(c)通过UHPLC-UV分析测得的迷迭香酸含量。湿化学分析的精密度验证显示:(a)相对标准偏差(RSD)为0.12%,(b)RSD为1.1%和(c)0.28%RSD为重复性,以及(a)4.1%的中间精度RSD,(b)1.3%RSD和(c)0.55%RSD。使用温度控制液体附件,使用NIR光谱仪分析收集的提取物。以透射模式以1mm的光程长度测量样品。记录的光谱和先前获得的分析参考值的结合以及多变量数据分析,使得能够成功建立偏最小二乘回归(PLSR)模型。测定系数(R 2 )为:(a)0.94,(b)0.96和(c)0.93(通过测试装置验证获得)。由于Pearson相关分析显示参考分析相互关联,因此仅需要一种PSLR模型。因此,建议将PLSR模型(b)用于监测迷迭香叶的提取过程。近红外光谱技术的应用提供了一种快速,无创的​​替代分析方法,随后可将其用于在线或在线过程控制。

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