黄酒发酵过程理化指标的近红外光谱快速检测方法研究

为提高黄酒发酵过程常规指标的检测效率,提出采用漫反射方式采集黄酒醪液的近红外光谱,并应用近红外技术结合偏最小二乘方法(PLS)建立一种能够同时测定黄酒醪液酒精度、总酸和总糖的定量分析模型。结果显示:优化后3种指标模型的决定系数(R)分别为0.99、0.91和0.98,交互验证标准偏差(RMSECV)分别为0.42、0.32和1.19;模型进行外部验证时,预测标准偏差(RMSEP)分别为0.45、0.35和2.01,预测平均相对偏差分别为3.37%、4.57%和4.66%,满足黄酒发酵过程中对样品分析检测精度的要求。研究结果表明该方法可以用于黄酒醪液常规指标的快速分析,对于解决黄酒自动化生产中指标检测问题具有积极意义。     

光谱预处理对近红外光谱快速检测黄酒酒精度的影响

本文以黄酒近红外透射光谱为研究对象,探讨光谱预处理方法对黄酒酒精度快速定量检测模型的影响,对比分析了采用平滑、一阶导数、二阶导数、多元散射校正、标准正态变换结合去势等五种传统方法和小波变换、傅里叶变换、正交信号校正等三种新方法预处理后光谱的偏最小二乘建模效果.结果表明,正交信号校正处理后,模型交叉验证R和RMSECV分...     

白酒酒精度近红外光谱快速检测方法研究

一、前言本文根据我国白酒的主要特点,以清/浓香型白酒酒精度的快速检测为研究对象,通过国家标准方法比重瓶法测量酒精含量,积累大量实验数据,再与样品的近红外光谱图信息相关联,经过化学计量学软件的处理,采用近红外光谱技术结合偏最小二乘法(NITS-PLS)建立乙醇含量的定量数学模型,得出样品组分的酒精度含量,开发白酒酒精度的快速检测法。所建模型交互验证相关系数(1-VR)达到0.999,定标标准偏差(SEC)为0.200,用所建模型测定样品与比重瓶法分析结果的相对误差不大于0.21%,实验结果表明近红外仪测量清/浓香型白酒酒精度的快速分析法是一…     

近红外光谱技术检测烟叶中的氨基酸

研究应用傅里叶变换近红外光谱法快速测定烟叶中氨基酸含量的可行性,使用偏最小二乘法(PLS)为建模方法,选择3800~8000 cm-1谱段,采用二阶导数和Norris Derivative滤波法进行光谱预处理,建立了烟叶中氨基酸含量的近红外预测模型。采用留一(leave-one-out)交叉验证法进行建模,并以校正集样品的交叉验证相关系数(R)和均方差(RMSECV)为指标优化光谱预处理方法和模型参数,确定最佳预测模型。将近红外光谱技术与常规标准检测方法相比较,结果表明,近红外光谱技术可以较为准确的测定烟叶中氨基酸的含量。     

近红外光谱模型优选应用于甘蔗清糖浆锤度快速分析

利用偏最小二乘法(PLS)和光谱Savitzky-Golay(SG)平滑方法,建立甘蔗清糖浆锤度近红外光谱分析的优化模型。SG平滑模式的扩展、SG平滑模式和PLS因子数的联合大范围筛选能够有效地应用于近红外光谱分析的模型优化。     

近红外透射光谱聚类分析快速鉴别食用油种类

以8种食用油纯油的43个样品为对象,研究了近红外透射光谱结合聚类分析法快速鉴别食用油种类的可行性.采集样品在12 500~4 000 cm-1范围内的傅立叶变换近红外透射光谱,利用光谱模式识别法中的聚类分析法对图谱进行定性分类鉴别.实验证明,光谱经二阶导数预处理后,最短距离法、最长距离法和方差平方和法均可准确无误地将食用油样品分为8类,判别模型对预测集样品的准确率达到100%.研究表明,近红外透射光谱结合聚类分析法可以为快速无损鉴别食用油种类提供一种准确可靠的方法.     

基于近红外光谱的英红九号红茶快速定级方法

目的 以英红九号红茶为研究对象,提出一种基于近红外光谱的红茶质量快速定级方法。方法 首先使用湿化学法对英红九号红茶进行内质成分含量检测,并通过感官审评对参试红茶进行定级,基于内质成分含量建立英红九号红茶定级模型,然后利用近红外光谱构建红茶内质成分的定量模型,以快速预测英红九号红茶的内质成分含量。将内质成分含量预测值输入定级模型,以预测英红九号红茶的质量等级。结果 建立了红茶茶多酚、可溶性糖、游离氨基酸和咖啡碱4个内质成分的偏最小二乘法定量模型,其测试集的决定系数分别为0.974 5、0.887 6、0.963 6、0.860 6,基于感官审评和内质成分的随机森林定级模型测试集的准确率为90.48%。结论 为红茶质量快速定级提供了一种可行方案,增强了基于近红外光谱的红茶定级方法的解释力。#$TAB     

近红外漫反射光谱结合神经网络检测小麦蛋白质含量

为了实现对小麦蛋白质含量的快速检测,提出了基于近红外光谱结合神经网络的小麦蛋白质检测方法.以160个小麦样品为对象,采集其近红外漫反射光谱,并以国标法分析小麦样品蛋白质含量,作为参考值.样品随机分成预测样品集和定标样品集,其光谱经标准归一化、去趋势等预处理后,采用BP神经网络和偏最小二乘法分别建立蛋白质含量定标模型.BP神经网络模型的预测相关系数和预测均方根误差分别为0.98和0.270 4%.而偏最小二乘法模型的预测相关性系数和预测均方根误差分别为0.98和0.303 8%.结果表明,两种方法建立的模型都具有较好的预测相关性和预测效果,其中BP神经网络模型优于偏最小二乘法模型.用非线性BP神经网络结合相应算法建立模型检测小麦蛋白质含量的定标模型可以提高检测准确性.     

近红外漫反射光谱法快速检测火药吸收药混合液中黑索今组分含量

研究了采用近红外( NIR)漫反射光谱技术快速检测火药吸收药混合液中黑索今( RDX)组分含量的方法。将装有混合液样品的烧杯置于光谱仪主机光源窗口上方,直接采集样品光谱图。通过分析纯RDX和样本的近红外光谱,确定908~945 nm、1094~1253 nm和1577~1678 nm作为建模谱区。通过比较不同的光谱预处理办法的效果,选择标准正态变换( SNV )＋一阶导数＋谱线平滑对原始光谱进行预处理。采用偏最小二乘方法(PLS)对RDX组分建立了定量线性校正模型。结果表明：模型的交叉验证决定系数(R2cv)为0.9879,交叉验证均方根误差(RMSECV)为0.2420,预测均方根误差(RMSEP)为0.2127,预测结果的平均相对误差为0.5661％,25 s内完成样品分析。该方法可给改性双基火药的连续自动化生产提供技术支持。     

近红外光谱技术在土壤成分检测中的研究进展

近红外光谱技术(NIRS)是一种快速的例行分析方法,在土壤科学领域内具有广阔的应用前景。本文评述了近红外光谱分析技术在土壤成分检测中的应用,并指出了其在土壤领域内的发展方向。     

傅立叶变换红外光谱法分析市售食品中反式脂肪酸

建立了一种快速测定食品中反式脂肪酸含量的方法,用索氏提取法或氯仿—甲醇提取法提取食品中脂肪,经甲醇-BF3快速甲酯化后,采用Avatar 370傅立叶变换红外光谱对反式脂肪酸进行定性定量分析,回收率为89.5%~103.3%,相对标准偏差为1.80%,重复性好,准确度高,适用于一般食品营养标签的测定。对我国市场上的涂抹奶油、派和蛋糕、饼干、巧克力、冰淇淋、薯片和薯条等6大类食品中20种样品中反式脂肪酸进行测定。结果表明,16种检出样品中反式脂肪酸含量在0.18%~10.34%之间,反式脂肪酸含量随食品种类不同存在显著差异,涂抹奶油、蛋黄派、威化饼干是反式脂肪酸含量较高的食品类别。     

傅里叶变换衰减全反射红外光谱法化学试剂定性鉴别数据库的建立

使用傅里叶变换衰减全反射红外光谱法(ATR-FTIR)进行了近200种有机化学试剂的定性鉴别试验,建立了傅里叶变换衰减全反射红外光谱数据库。使用该方法能够鉴别大多数常见的有机化合物,并具有分辨力高、检验简便的特点。     

Discrimination of soil-borne fungi using fourier transform infrared attenuated total reflection spectroscopy

Fourier transform infrared (FT-IR) attenuated total reflection (ATR) spectroscopy was used to discriminate five commonly encountered soil-borne fungi that cause severe economic damage to agriculture: Colletotrichum, Fusarium, Pythium, Rhizoctonia, and Verticillium. Contrary to previous studies related to microorganism discrimination using FT-IR-ATR spectroscopy, the pathogen samples were not dried on the ATR crystal, which is a time-consuming operation. Rather, after removing some pathogen filaments from the solution using tweezers, these were placed directly on a flat ATR crystal and pressure was applied using a pressure clamp. Following water subtraction, baseline correction, and normalization of the spectra, principal component analysis was used as a data-reduction step and canonical variate analysis was used for discrimination. Discrimination was performed at the genus level and at the strain level for Colletotrichum. For discrimination between the five fungi at the genus level, the success rate for the validation samples ranged from 75% to 89%. For discrimination between the two Colletotrichum strains, the success rate was 78%. Comparison with spectra of similar fungi dried on the ATR crystal showed that both types of spectra were very similar, indicating that drying the samples on the ATR crystal is not required and can be replaced by mathematical post-processing of the spectra. For routine analyses that involve rapid screening of very large amounts of samples, this approach allows for increasing significantly the number of samples that can be analyzed daily.     

Quantification of volatile organics in soil aging experiments using fourier transform infrared spectroscopy

On-line Fourier transform infrared (FT-IR) spectroscopy was applied to monitor the concentration of halogenated volatile organic compounds in a sample-preparation process that simulates long-term, slow accumulation of contaminants in soils (i.e., aging). Artificial aging is conducted by circulating a supercritical fluid solution containing the contaminant(s) of interest through a packed soil column. Mid-infrared spectra of several volatile halocarbons were measured in supercritical Xe and CO(2) to evaluate possible interferences from the strong absorption of CO(2). Although some of the C-X bands were partially masked in supercritical CO(2), all of the compounds studied had distinct spectral features in the region 1400-700 cm(-1) and could be monitored in either solvent. Quantitative measurements of halogenated volatile organics in supercritical CO(2) were demonstrated with CCl(4). Excellent results were obtained over the range 7-280 mM. Representative artificial aging experiments were conducted on two test soils using CCl(4) as the contaminant. On-line (FT-IR) estimates of the aged soil concentrations were 1.3-4.4 times higher than off-line concentrations obtained by gas chromatography/mass spectrometry. The discrepancies were primarily ascribed to post-aging losses that occurred during depressurization and subsequent sample handling. FT-IR spectroscopy is shown to be a powerful tool for monitoring soil loading behavior and for developing artificial aging protocols.     

Rapid nondestructive on-site screening of methylamphetamine seizures by attenuated total reflection fourier transform infrared spectroscopy

The identification and quantification of illicit substances in the field is often desirable. Fourier transform infrared spectroscopy (FT-IR) has both qualitative and quantitative capabilities and field portable instruments are commercially available. Transmission infrared spectra of mixtures containing ephedrine hydrochloride, glucose, and caffeine and attenuated total reflection (ATR) infrared spectra of mixtures composed of methylamphetamine hydrochloride, glucose, and caffeine were used to develop principal component regression (PCR) calibration models. The root mean sum of errors of predictions (RMSEP) of all individual components in a mixture from a single measurement was <6% w/w, which reduced to approximately 3% w/w when triplicates were averaged. Sample mixing and grinding are essential to minimize the effect of heterogeneity, as deviations of up to 20% w/w were observed for single measurements of unground samples. Poor predictions of the components in a mixture occurred when samples were "contaminated" with substances not present in the calibration set, as would be expected. When only a single analyte (drug) was targeted, using a calibration set that contained both contaminated and uncontaminated samples, an RMSEP of approximately 4% w/w was achieved. The results demonstrate that ATR-FT-IR has the potential to quantify methylamphetamine samples, and possibly other licit or illicit substances, in at-seizure and on-site scenarios.     

On-line dissolution determination of Baicalin in solid dispersion based on near infrared spectroscopy and circulation dissolution system

Drug on-line circulation dissolution system with near infrared spectrophotometer for dissolution determination was reported in this paper and subsequently partial least squares (PLS) calibration model was established for concentration prediction of Baicalin in solid dispersion. When the main factor number in PLS calibration model was 6, the correlation coefficients of PLS calibration samples and prediction ones were all 0.9999 and the relative standard deviations were 0.69% and 1.10%, respectively, which showed good robustness and predictability. Combining drug circulation dissolution system with the PLS calibration model, dissolution of Baicalin in raw material drug and solid dispersion were obtained at different times. The results indicated that the dissolution property of Baicalin in solid dispersion (especially at the early time) had been significantly improved. The accumulated dissolution of Baicalin in the solid dispersion at 45 min reached nearly 40%, increasing by 15% compared with raw material drug (about 25%). The aforementioned PLS model associated with drug circulation dissolution system provided a simple, accurate and on-line support for dissolution determination of drug, especially at the early time of rapid dissolution.     

Monitoring the thermal gelation of cellulose ethers in situ using attenuated total reflectance fourier transform infrared spectroscopy

In this work attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy was used to probe the thermal gelation behavior of aqueous solutions of hydroxypropyl methylcellulose (HPMC), specifically thermal gelation and accompanying precipitation. Cloud point measurements are usually evaluated through turbidity in dilute solutions but the method cannot readily be applied to more concentrated or highly viscous solutions. From the ATR-FTIR data, intensity changes of the nu(CO) band marked the onset of gelation and information about the temperature of gelation and the effect of the gel structure on the water hydrogen bonding network was elucidated. Changes in the relative intensities of bands associated with the methoxyl groups and hydrogen-bond-forming secondary alcohol groups indicated that hydrophobic polymer chain interactions were involved in the gelation process. The dominance of inter-molecular H bonding over intra-molecular H bonding within the cellulose ether in solution was also observed. The ATR-FTIR data was in good agreement with measurements of turbidity conducted on the same systems. The work indicates significant potential for the use of ATR-FTIR for the investigation of gelation and cloud point measurements in viscous cellulosic formulations.     

近红外光谱分析技术在聚乙烯醇分析中的应用

采用近红外光谱分析仪对聚乙烯醇进行扫描,测定其光谱图。然后对光谱图进行分析处理,利用化学计量学软件,建立定性和定量分析模型。用光纤将近红外光谱仪和检测探头连接起来,组成一个在线分析系统,可以实现在线分析。介绍了近红外光谱分析的基本原理和基本过程。     

Hydrogen-deuterium exchange in bovine serum albumin protein monitored by fourier transform infrared spectroscopy, part I: structural studies

The structure of the amide I band of bovine serum albumin (BSA) was determined using an H/D exchange experiment. The difference between the dry and hydrated exchange spectrum revealed the fine structure of the amide I band. The band at 1717 +/- 2 cm(-1) is due to the vibration of the COOH moieties from the protein side chains. Band components at 1682 +/- 2 cm(-1), 1655 +/- 2 cm(-1), and 1637 +/- 2 cm(-1) are assigned to the vibrations of the backbone C=O. These three bands belong to vibrations of three different populations of amide groups differing in the number of established H-bonds. The connectivity between the frequencies of various amide vibrations was determined by two-dimensional generalized correlation spectroscopy and spectral decomposition. About 7% of the whole exchangeable hydrogen atom population (NH, NH2, and OH groups from backbone and side chains) remains unexchanged, and these hydrogen atoms belong mainly to the NH groups, which are H-bonded to specific C=O groups. Moreover, this study concerns the approximately 10% of hydrogen atoms belonging to a particular HN...O=C population with a characteristic amide A frequency at 3290 cm(-1) and an amide I band at 1655 +/- 2 cm(-1), usually attributed to the alpha-helical structure that remains unexchanged. At higher temperature the exchange is more efficient. Upon heating, a further 4% of these NH groups are deuterated. The comparison of the exchange spectrum at higher temperature with the structural changes of the protein at the same temperature implies that the change in overall dynamics of the protein improve the level of exchange.