title: Validation of a NIR quantification method for the determination of chlorogenic acid in Lonicera japonica solution in ethanol precipitation process.
abstract: The feasibility of near-infrared spectroscopy (NIRS) for chlorogenic acid content analysis in ethanol precipitation process of water extract of Lonicera japonica was verified in this work. A calibration and validation set was designed for the conception and evaluation of the method adequacy. An experimental protocol was then followed, involving two different NIR instruments for data acquisition. On the basis of this protocol, the model was developed based on partial least squares regression (PLS) and the determination coefficient (R(2)(cal) and R(2)(val)), standard error of calibration and prediction (SEC and SEP) were 0.9962, 0.9955, 111.1 μg/mL and 107.1 μg/mL for Holographic Grating NIR instrument, and 0.9984, 0.9971, 53.6 μg/mL and 83.3 μg/mL for Fourier Transform NIR instrument. However, such above criteria did not clearly demonstrate the model's prediction error over each analyzed content range. Consequently, a novel approach based on accuracy profile which allowed the acquisition of the lower limit of quantification (LLOQ) was used to validate the robustness and accuracy of PLS model. The resulting accuracy profile showed that PLS model was able to determine chlorogenic acid content by two NIR systems, whose LLOQ was about 1550 μg/mL. It was concluded that the two NIR systems were suitable for use as Process Analytical Technology (PAT) to understand ethanol precipitation process of water extract of Lonicera japonica.
authors.affiliation: Beijing University of Chinese Medicine, Beijing 100102, China.
authors.forename: Zhisheng
authors.initials: Z
authors.lastname: Wu
authors.forename: Bing
authors.initials: B
authors.lastname: Xu
authors.forename: Min
authors.initials: M
authors.lastname: Du
authors.forename: Chenglin
authors.initials: C
authors.lastname: Sui
authors.forename: Xinyuan
authors.initials: X
authors.lastname: Shi
authors.forename: Yanjiang
authors.initials: Y
authors.lastname: Qiao
mesh_terms: D002138:Calibration; D002726:Chlorogenic Acid / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid; D000431:Ethanol / Q000737:chemistry*; D031239:Lonicera / Q000737:chemistry*; D012996:Solutions; D019265:Spectroscopy, Near-Infrared
chemical_list: D012996:Solutions; D002726:Chlorogenic Acid; D000431:Ethanol