HPLC结合多元化学计量学鉴别水洗和日晒咖啡
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作者单位:

(1.湖南中医药大学药学院 长沙 410208;2.湖南中医药大学中西结合学院 长沙 410208;3.湖南省中药饮片标准化及功能工程技术研究中心 长沙 410208)

作者简介:

杨浩澜(2000—),男,本科

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基金项目:

国家自然科学基金项目(81704064);湖南省教育厅科学研究优秀青年项目(20B434);湖南省中药学一流学科资助项目(校行科字[2018]3号)


Identification of Washed and Sun-dried Coffee by HPLC Combined with Multi-chemometrics
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(1.College of Pharmacy, Hunan University of Chinese Medicine, Changsha 410208;2.College of Integrated Traditional Chinese and Western Medicine, Hunan University of Chinese Medicine,Changsha 410208;3.Center for Standardization and Functional Engineering of Traditional Chinese Medicine in Hunan Province,Changsha 410208)

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    摘要:

    建立了一种通过筛选差异成分准确鉴别水洗和日晒咖啡的方法。采集咖啡样本的高效液相(HPLC)色谱图,使用Kennard-Stone算法将两类不同加工方式咖啡样品的全谱原始信号和共有峰峰面积数据分别按7 ∶ 3的比例划分为校正集和测试集,首先建立主成分分析(PCA)及偏最小二乘判别分析(PLS-DA)模型,再通过多元算法对PLS-DA模型进行优化,最后将最佳模型判别函数中X变量的相关系数×100-1标记于色谱图上,标识为两类咖啡的差异成分,并对其中含量最高的成分进行定性。结果表明,采用共有峰峰面积数据无法建立合格的预测模型以区分水洗和日晒咖啡,而采用90个区间下的反向区间偏最小二乘法(BiPLS)优化后的全谱原始信号建立的模型则具有良好的鉴别能力,其对测试集样本预测的准确度达83.33%,Q2值为0.813。标准品定性结果提示绿原酸为两类咖啡的重要差异成分之一。相较于以单个或多个化合物的含量信息作为样品差异评价标准的传统方法,本法可准确挖掘产品的差异信息,为整体评判产品质量提供了新思路。

    Abstract:

    A method was established to identify washed and sun-dried coffee comprehensively and accurately by screening differential components. High performance liquid chromatography(HPLC) of coffee samples were collected for multi-chemometrics analysis, and then the full raw signals and common peaks' area data that came from the two different processing types of coffee samples were divided into calibration set and test set respectively using the Kennard-Stone algorithm in the ratio of 7:3. Principal component analysis (PCA) and partial least squares-discriminant analysis (PLS-DA) models were established based on those data primitively. In the following work, the raw data were processed to optimize PLS-DA model by using the sole algorithm and combinatorial algorithm, such as variable importance in projection (VIP), backward interval partial least squares (BiPLS), successive projections algorithm (SPA), uninformative variable elimination-partial least squares (UVE-PLS), competitive adaptive reweighted sampling-partial least squares (CARS-PLS) separately, and BiPLS-VIP/CARS/SPA/UVE together. After that, the correlation coefficients ×100-1 of X-variables in the discriminant function of the optimum model were labeled on the chromatogram, which was used for screening quality markers between the two types of coffee, and the highest correlation component was qualitative analyzed. The results demonstrated that a qualified prediction model could not be established using the full raw signals to distinguish washed and sun-dried coffee, while the BiPLS algorithm at 90 intervals was the best optimum proposal among all kinds of algorithms, which had good discriminatory ability with an accuracy of 83.33%, a Q2 value of 0.813 and an root mean square error of cross validation (RMSEcv) value of 0.217. The qualitative results of the standards illustrated that chlorogenic acid is one of the important differential components of coffee with two different processing methods. Above all, compared to the traditional method of using the single or multiple compounds contents information as quality evaluation criteria, this identification method could dig out the differential components entirely and accurately, which providing a new thought with reference value for the product quality assessment comprehensive.

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杨浩澜,包亮英,刘实琪,刘亦菲,朱炎贞,刘芳. HPLC结合多元化学计量学鉴别水洗和日晒咖啡[J].中国食品学报,2022,22(9):304-311

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  • 收稿日期:2021-09-28
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  • 在线发布日期: 2022-10-26
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