傅立叶变换近红外光谱法测定腐乳中总酸、蛋白质和水分

应用傅立叶变换近红外光谱技术,建立了腐乳中总酸、蛋白质和水分的分析模型。测定32份腐乳的近红外光谱数据,得到原始光谱信息,通过光谱预处理方法消除原始光谱噪声,最后采用偏最小二乘法建立回归方程。最终得到总酸、蛋白质和水分近红外光谱分析模型的决定系数(R2)依次为99.37%、99.70%、99.73%,交叉验证均方根差(RMSECV)依次为0.00871、0.11、0.0714。用该模型对11个未知腐乳样品进行外部验证,其总酸、蛋白质和水分外部验证的决定系数(R2)依次为98.74%、99.38%、99.48%,预测标准偏差(RMSEP)依次为0.00862、0.113、0.0683。内部交叉验证和外部验证均证明,近红外定量分析有较高的准确度,能满足腐乳生产中总酸、蛋白质和水分的检测精度要求。     

近红外光谱法快速测定豆粕中混入的玉米粉含量

通过对豆粕样品和混有部分玉米粉的豆粕样品的近红外光谱分析，结果表明：混合样品中淀粉的含量与样品在２０６０ｎｍ，２０９０ｎｍ和 ２１６６ｎｍ处的光谱数据具有高的相关系数，然后应用回归分析计算出线性方程，再根据玉米粉中的淀粉含是一计算混合样品中的玉米粉含量。     

傅里叶变换近红外光谱法测定大麦中蛋白质、淀粉和赖氨酸含量

采用傅里叶变换近红外光谱法测定大麦中蛋白质、淀粉、赖氨酸的含量，并用光谱影响值法(leverage)对异常值进行判断和处理。蛋白质、淀粉和赖氨酸含量近红外光谱分析模型的测定系数R。分别为0．985、0．973和0．978；检验集的化学值与模型预测值的相关系数r分别为0．9853、0．9644和0．9172，分析模型的预测相对标准偏差RSD分别为4．0％、2．4％和5．4％，该结果可替代经典分析方法，满足农产品快速分析的需要。     

用近红外透射光谱技术测定精米蛋白质含量研究

应用近红外透射光谱技术．采用3种不同回归统计分析方法建立业米蛋白质含量(PC)定量回归方程。结果表明,用改进的最小二乘法(MPLS)、偏最小二乘法(PLS)和主成分回归法(PCR)进行饺正时．校正标准误差(SEC)、交叉检验标准误差(SECV)分别为0．1258、0．134O(MPLS)．0．1177、0．1175(PLS)．0．1207、0．1275(PCR)校正相关系数(RSQ)和交叉验证相关系数(1-VR)分别为0．9941、0．9931(MPLS)．0．9950、0．9942(PLS)．0．9947、0．9942(PCR)。由此可见,3种回归统计方法在建立业米蛋白质含量回归方程时差异不明显．都具有较好的预测效果。近红外透射光谱法作为一种快速而准确的定量分析手段,在稻米加工企业品质管理、大米品质分析和大米贸易检测上有广阔的应用前景。     

近红外光谱分析原油中水分和硫含量模型的建立及验证

取原油样品120个,分别按照GB/T 11133-2015和GB/T 17040-2008中所述方法测定了上述原油样品中的水分和硫的含量。通过优化的近红外光谱(NIRS)条件采集了上述原油样品的NIR光谱图。采用杠杆值算法剔除4个异常样品。在建立水分含量分析模型时,采用的条件为:用Savitzky-Golay法对光谱进行滤波预处理,建模光谱区间为6 200～8 200cm-1,主成分数为6,用偏最小二乘回归法(PLS)交叉验证建立分析模型。硫含量分析模型的建立条件为:采用二阶导数-Norris Derivative对光谱进行预处理,建模光谱区间为4 400～4 700cm-1,主成分数为6,用PLS交叉验证建立分析模型。水分和硫含量模型的预测值与测定值的相关性较好。水分模型的决定系数(R2c)为0.989 9,校正标准偏差(RMSEC)为0.084 2,说明其预测效果较好,可用于原油中水分含量的预测。硫含量模型的R2c为0.996 3,RESEC为0.069 6,说明此模型的预测效果也较好,可用原油中硫含量的预测。应用所建立的两个模型对10个未知原油样品中水分和硫含量进行了预测,并与其测定值比较,结果表明两者之间的相对偏差均小于10%。     

同时测定水溶液中葡萄糖、果糖和蔗糖的近红外光谱法

通过对27个葡萄糖、果糖和蔗糖水溶液的混合体系进行近红外光谱分析，建立了葡萄糖、果糖和蔗糖含量测定的偏最小二乘法(PLS)模型；葡萄糖、果糖和蔗糖的线性范围分别为0—300g/L、0—200g/L、0—300g/L，模型校正集的标准误差(SEC)分别为1．4、1．8、1．4g/L；用该模型对6个样品进行分析，葡萄糖、果糖和蔗糖含量测定的相对标准偏差(RSD)分别为1．2％、2．6％和1．8％。     

利用油水稳定化和支持向量回归增强近红外光谱测定油中水分的方法

近红外光谱(NIRS)可以检测溶解于油中的水分含量,但油中水分较多时会散射而非吸收NIRS,从而引起较大误差。为此,筛选非离子型表面活性剂(Span-80)将含水油液稳定分散成小颗粒,利用其NIRS数据建立水分含量的支持向量回归模型。实验中油水稳定化将NIRS测定变压器油中水分含量的上限从传统的0.1%提升到1%(V/V),通过应用连续投影算法,在511个NIRS变量中筛选出15个有效变量(占原变量的2.9%),建立的支持向量回归模型对验证集的预测均方根误差为2.93%,相关系数为0.9944,相对分析误差为9.4732。     

用近红外光谱仪快速测定调和汽油中芳烃、烯烃的含量

介绍了带有CCD检测器的近红光普仪在调和汽油分析中的应用，并与标准测定方法测定的数据对比，验证了近红外光谱法测定汽油性质的可靠性，同时表明该方法具有分析速度快，重现性好等特点。     

傅里叶变换红外光谱法同时测定奶粉中蛋白质和脂肪含量

利用傅里叶变换红外光谱法同时测定奶粉中蛋白质和脂肪含量.以硫氰化钾为内标物,其特征峰2 061.8 cm-1为参比峰,蛋白质和脂肪的特征峰为分析峰,分别将蛋白质和脂肪的分析峰的校正面积(As)与参比峰的校正面积(AKSCN)比(R=As/AKSCN)对蛋白质和脂肪含量作工作曲线.确定酰胺Ⅰ带1 654.8 cm-1(1 600.0～1 733.3 cm-1)与参比峰(1 981.0～ 142.9 cm-1)的组合A1654.8/AKSCN最适合进行蛋白质定量分析,其线性回归方程C=3.871 R+10.88,相关系数为0.992 3;脂肪的C=0伸缩振动1 747.4 cm-1(1 719.0～1 766.7 cm-1)与参比峰(1 985.7～2 133.3 cm-1)的组合A1 747/AKSCN最适合脂肪定量分析,其线性回归方程C=29.13 R+3.531,相关系数为0.986 6.此方法的测定结果与凯氏定氮法和碱性乙醚提取法测定结果相比相对误差均小于±2.4%.     

近红外光谱法测定黄芩提取物中黄芩苷含量

近红外光谱技术(NIR)是近年来快速发展的一种新型光谱分析技术,具有快速、高效、无污染、非破坏性以及实时分析等优点~([1]),已在农业、烟草、石油化工、医药等多领域得到广泛应用.尤其在药物分析方面,体现出近红外光谱分析的巨大潜力~([2]).     

Use of indirect multivariate calibration for quality control of agricultural products by near infrared spectroscopy

In the near infrared (NIR) region, (=800–2500 nm) of the spectrum, most organic molecules have weak but reproducibly measurable absorption bands. This phenomenon has been increasingly exploited for the rapid, quantitative analysis of major constituents of agricultural products. As there is strong spectral overlap and an interaction of constituents in NIR, the calibration of instrumentation has to be performed indirectly with a training set of samples applying multivariate methods. A software package for IBM compatible personal computers includes programs to select samples to be used for calibration, to compute multiple linear regression equations, to cross-validate regression equations and to detect unusual samples. These methods are applied to rapidly determine the oil content of over a thousand rapeseed samples of the harvest of 1986. A considerable saving of time, labour, and costs can be achieved, the agreement with the standard laboratory method is very satisfactory.     

复方氯丙那林质量检控的近红外光谱快速分析

基于近红外光纤漫反射技术,利用偏最小二乘法分别建立了复方氯丙那林胶囊的三种药效成分盐酸氯丙那林、盐酸溴己新和盐酸去氯羟嗪的快速同时测定方法。所建立的盐酸氯丙那林、盐酸溴己新和盐酸去氯羟嗪的定量分析多元校正模型的相关系数分别为99.7%、99.4%和99.0%,校正集的均方根残差分别为0.028、0.145和0.250,预测均方根误差分别为0.055、0.120和0.210。由于该方法是在不经任何预处理的情况下的光纤快速同时分析,因此可用于复方氯丙那林的过程质量控制。     

Determination of moisture, starch, protein, and fat in common beans (Phaseolus vulgaris L.) by near infrared spectroscopy

The presence of moisture, starch, protein, and fat was determined in common beans (Phaseolus vulgaris L.) by near infrared (NIR) spectroscopy without any previous sample pretreatment except grinding. A set of 96 samples was used to calibrate the instrument by modified partial least-squares regression. The following statistical results were achieved: standard error of calibration (SEC) = 0.31 and square correlation coefficient (R2) = 0.96 for moisture; SEC = 0.76 and R2 = 0.92 for starch; SEC = 0.39 and R2 = 0.98 for protein; and SEC = 0.14 and R2 = 0.80 for fat. To validate the calibration, a set of 25 bean samples was used. Standard errors of prediction were 0.39, 0.90, 0.56, and 0.13 for moisture, starch, protein, and fat, respectively, and R2 for the regression of measurements by the reference method versus NIR analysis were 0.94, 0.88, 0.94, and 0.74 for moisture, starch, protein, and fat, respectively. To compare the results obtained for all 4 components of the validation set by NIR spectroscopy with those obtained by the reference methods, linear regression and paired t tests were applied, and the methods did not give significantly different results, P = 0.05.     

Simultaneous measurement of glucose and glutamine in aqueous solutions by near infrared spectroscopy

A method is described for measuring the concentrations of both glucose and glutamine in binary mixtures from near infrared (NIR) absorption spectra. Spectra are collected over the range from 5000–4000/cm (2.0–2.5μm) with a 1-mm optical path length. Glucose absorbance features at 4710, 4400, and 4300/cm and glutamine features at 4700, 4580, and 4390/cm provide the analytical information required for the measurement. Multivariate calibration models are generated by using partial least squares (PLS) regression alone and PLS regression combined with a preprocessing digital Fourier filtering step. The ideal number of PLS factors and spectral range are identified separately for each analyte. In addition, the optimum Fourier filter parameters are established for both compounds. The best overall analytical performance is obtained by combining Fourier filtering and PLS regression. Glucose measurements are established over the concentration range from 1.66–59.91 mM, with a standard error of prediction (SEP) of 0.32 mM and a mean percent error of 1.84%. Glutamine can be measured over the concentration range from 1.10–30.65 mM with a SEP of 0.75 mM and a mean percent error of 6.67%. These results demonstrate the analytical utility of NIR spectroscopy for monitoring glucose and glutamine levels in mammalian and insect cell cultures.     

Implementation of enhanced correlation maps in near infrared chemical images: Application in pharmaceutical research

Recent developments in Hyperspectral Imaging equipment have made possible the use of this analytical technique for fast scanning of sample surfaces. This technique has turned out to be especially useful in Pharmacy, where information about the distribution of the components in the surface of a tablet can be obtained. One particular application of Hyperspectral Chemical Imaging is the search for singularities inside pharmaceutical tablets, e.g. coating defects. Nevertheless, one problem has to be faced: how to analyze a sample without any previous knowledge about it, or having only the minimum information about the tablet.In this work a new methodology, based on correlation coefficients, is introduced to obtain valuable information about one Hyperspectral Image (detection of defects, punctual contaminants, etc.) without any previous knowledge. The methodology combines Principal Component Analysis (PCA), correlation coefficient between one specific pixel included in the image and the rest of the image; and a new enhanced contrast function to obtain more selective chemical and spatial information about the image. To illustrate the applicability of the proposed methodology, real tablets of ibuprofen have been studied.The proposed methodology is presented as a control technique to detect batch variability, defects in final tablets and punctual contaminants, being a potential supplementary tool for quality controls. In addition, the usefulness of the proposed methodology is not exclusive to NIR-CI devices, but to any hyperspectral and multivariate image system.     

Curing reaction of glycidylthioether resins: Kinetic model study by near infrared spectroscopy and multivariate curve resolution

The reactivity of sulfur‐based epoxy monomers was studied by monitoring of a model system involving phenylglycidylthioether and aniline. The reaction was carried out under isothermal conditions and monitored in situ by near infrared spectroscopy. Using multivariate curve resolution‐alternating least squares made it possible to obtain the concentration and spectral profiles of each species throughout the reaction. To obtain the kinetic rate constants, the values of the recovered concentration profiles were fitted to a kinetic model proposed for the reaction. Reactivity was evaluated by comparing the concentration profiles and kinetic rate constants obtained with the same parameters obtained for phenylglycidylether/aniline as a reference system. © 2006 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 4846–4856, 2006     

近红外光谱测定复方对乙酰氨基酚片的有效成分

复方对乙酰氨基酚是临床上常用的解热镇痛药,常用剂型有片剂和注射剂,其片剂含有对乙酰氨基酚、阿司匹林和咖啡因等三种有效成分。对于该制剂的质量控制,《中国药典》[1]利用分光光度法测定对乙酰氨基酚的含量,用氢氧化钠标准溶液、高氯酸标准溶液分别滴定阿司匹林和咖啡因从而     

Quantitative determination of acyclovir in plasma by near infrared spectroscopy

The aim of this study was to assess the feasibility of near infrared spectroscopy (NIRS) for analysis of acyclovir in plasma. This methodology was based on the direct measurement of the transmission spectra of liquid samples and a multivariate calibration model (partial least squares, PLS) to determine the acyclovir concentration in plasma sample. The PLS calibration set was built on using the spiked samples by mixing different amounts of acyclovir. Concentration of acyclovir in the plasma samples was calculated employing a 6-factors PLS calibration using the spectral information in the range of 6102-5450 cm^− 1. The root mean square errors of prediction (RMSEP) found was 1.21 for acyclovir. The developed PLS-NIRS procedure allows the determination of 120 samples/h does not require any sample pretreatment and avoids waste generation.     

Tuning the decay time of lanthanide-based near infrared luminescence from micro- to milliseconds through d-->f energy transfer in discrete heterobimetallic complexes

Inert and optically active pseudo-octahedral Cr(III)N6 and Ru(II)N6 chromophores have been incorporated by self-assembly into heterobimetallic triple-stranded helicates HHH-[CrLnL3]6+ and HHH-[RuLnL3]5+. The crystal structures of [CrLnL(3)](CF(3)SO(3))(6) (Ln=Nd, Eu, Yb, Lu) and [RuLnL3](CF3SO3)5 (Ln=Eu, Lu) demonstrate that the helical structure can accommodate metal ions of different sizes, without sizeable change in the intermetallic MLn distances. These systems are ideally suited for unravelling the molecular factors affecting the intermetallic nd-->4f communication. Visible irradiation of the Cr(III)N6 and Ru(II)N6 chromophores in HHH-[MLnL3]5/6+ (Ln=Nd, Yb, Er; M=Cr, Ru) eventually produces lanthanide-based near infrared (NIR) emission, after directional energy migration within the complexes. Depending on the kinetic regime associated with each specific d-f pair, the NIR luminescence decay times can be tuned from micro- to milliseconds. The origin of this effect, together with its rational control for programming optical functions in discrete heterobimetallic entities, are discussed.