Fourier transform infrared spectra of drying oils treated by irradiation

Drying oils, such as linseed oil and tung oil, have the potential as coating materials to improve barrier properties of biobased packaging films. Oil drying is a chemical reaction in which polyunsaturated fatty acids undergo autoxidation. During drying, oils polymerize and form water-resistant films. However, drying rates tend to be too slow for practical applications. Metal driers are used in the paint industry to accelerate drying, but often driers are not safe for food contact. The objective of this work was to investigate the effect of ionizing radiation on the oxidation or drying rate of drying oils. The effect of irradiation dose on the drying rate of linseed and tung oils was monitored by FTIR spectroscopy. The peak at 3010 cm (-1) was found to be a useful index of oxidation rate. The decrease in peak intensity with time was fitted with exponential functions of the form Abs = Abs 0 exp (- t/ k), where Abs 0 is the initial absorbance and 1/ k is the rate constant for the oxidation process. Values for k were 9.91 ( R (2) = 0.98), 6.59 ( R (2) = 0.95)n and 6.44 ( R (2) = 0.97) for radiation levels of 0, 50, and 100 kGy, respectively. The k values suggested that the oxidation rate increased as the radiation dose increased from 0 to 50 kGy. A further increase to 100 kGy had only a limited effect.     

Interpretation of Fourier transform Raman spectra of the unsaponifiable matter in a selection of edible oils.

The unsaponifiable matter of edible oils is a source of information for their characterization and authentication. FT-Raman spectroscopy has been applied with success to the determination of the spectra of the unsaponifiable matter of varietal olive oils as well as other refined and crude edible oils. The spectra of the major unsaponifiable series of compounds (squalene, sterolic, and terpenic alcoholic fractions), together with beta-carotene and lutein, have been used to explain the most prominent bands found in the spectra of the unsaponifiable matter of 15 edible oil samples. The order of the scattering intensities of the varietal olive oils agrees with the results obtained by chromatography. An unsupervised multivariate statistical analysis of selected bands points out differences between olive oils and the other seed oils and also among varietal virgin olive oils.     

畜禽粪便热解气体的红外光谱分析

为了解畜禽粪便热解过程析出气体的主要成分以及气体析出规律,该文在30℃/min的升温速率条件下进行了猪粪、牛粪、羊粪和鸡粪的热解试验,利用傅里叶变换红外光谱（FTIR）技术对热解过程中气体产物的排放特性进行了分析。试验结果表明,畜禽粪便气体产物主要在250～500℃析出,其主要成分为H2O,CO,CO2和CH4等,其中H2O、CO和CO2的析出峰为双峰,H2O和CO2均在350℃附近形成最大析出峰,H2O约在150℃形成第1个析出峰,CO2约在710℃附近形成的第2个析出峰,CO在350℃处形成第一个析出峰,其最大析出峰形成于710℃处左右,CH4析出特性为一单峰,在530℃附近形成最大峰值。该文研究结果为热解反应器的设计和优化提供参考。     

Fourier transform infrared spectroscopy and chemometric analysis of white wine polysaccharide extracts

Monovarietal white wines from Maria Gomes and Bical Portuguese Bairrada varieties were prepared according to different maceration and pectic enzyme clarification procedures. The polysaccharide-rich extracts, obtained by wine concentration, dialysis, and lyophilization, were fractionated by graded ethanol precipitation. A wide range of fractions rich in polysaccharides were obtained. Using the spectral region between 1200 and 800 cm(-)(1) of the FTIR spectra of the wine polysaccharide dry extracts, using PCA and CCA chemometric methods, it was possible to discriminate the extracts on the basis of their polysaccharide composition. Moreover, it was possible to identify the wine-making processes involved and their influence on the wine polysaccharides. Furthermore, a calibration model using a PLS1 was proposed for the quantification of mannose in the samples obtained by precipitation with 60% ethanol aqueous solutions. This information will allow an expeditious assessment and monitoring of the polysaccharide composition and modifications that occur during the wine-making processing and evolution.     

Classification and structural analysis of live and dead Salmonella cells using Fourier transform infrared spectroscopy and principal component analysis

Fourier transform infrared spectroscopy (FT-IR) was used to detect Salmonella Typhimurium and Salmonella Enteritidis food-borne bacteria and to distinguish between live and dead cells of both serotypes. Bacteria cells were prepared in 10(8) cfu/mL concentration, and 1 mL of each bacterium was loaded individually on the ZnSe attenuated total reflection (ATR) crystal surface (45° ZnSe, 10 bounces, and 48 mm × 5 mm effective area of analysis on the crystal) and scanned for spectral data collection from 4000 to 650 cm(-1) wavenumber. Analysis of spectral signatures of Salmonella isolates was conducted using principal component analysis (PCA). Spectral data were divided into three regions such as 900-1300, 1300-1800, and 3000-2200 cm(-1) based on their spectral signatures. PCA models were developed to differentiate the serotypes and live and dead cells of each serotype. Maximum classification accuracy of 100% was obtained for serotype differentiation as well as for live and dead cells differentiation. Soft independent modeling of class analogy (SIMCA) analysis was carried out on the PCA model and applied to validation sample sets. It gave a predicted classification accuracy of 100% for both the serotypes and its live and dead cells differentiation. The Mahalanobis distance calculated in three different spectral regions showed maximum distance for the 1800-1300 cm(-1) region, followed by the 3000-2200 cm(-1) region, and then by the 1300-900 cm(-1) region. It showed that both of the serotypes have maximum differences in their nucleic acids, DNA/RNA backbone structures, protein, and amide I and amide II bands.     

Dietary supplement oil classification and detection of adulteration using Fourier transform infrared spectroscopy

Fourier transform infrared spectroscopy (FT-IR) methods and common chemometric techniques [including discriminant analysis (DA), Mahalanobis distances, and Cooman plots] were used to classify various types of dietary supplement oils (DSO) and less expensive, common food oils. Rapid FT-IR methods were then developed to detect adulteration of DSO with select common food oils. Spectra of 14 types of DSO and 5 types of common food oils were collected with an FT-IR equipped with a ZnSe attenuated total reflectance cell and a mercury cadmium telluride A detector. Classification of DSO and some common food oils was achieved successfully using FT-IR and chemometrics. Select DSO were adulterated (2-20% v/v) with the common food oils that had the closest Mahalanobis distance to them in a Cooman plot based on the DA analysis, and data were also analyzed using a partial least-squares (PLS) method. The detection limit for the adulteration of DSO was 2% v/v. Standard curves to determine the adulterant concentration in DSO were also obtained using PLS with correlation coefficients of >0.9. The approach of using FT-IR in combination with chemometric analyses was successful in classifying oils and detecting adulteration of DSO.     

Analysis of hard-to-cook red and black common beans using Fourier transform infrared spectroscopy

Extracted fractions from black and red common beans (Phaseolus vulgaris) were studied using Fourier transform infrared spectroscopy (FT-IR). Beans were stored under three conditions: control at 4 degrees C; hard-to-cook (HTC) at 29 degrees C, 65% RH for 3.5 months; and refrigerated at 2 degrees C, 79% RH for 3.5 months after a HTC period (called HTC-refrigerated). Two fractions isolated from the beans, the soluble pectin fraction (SPF) and the water insoluble residue of the cell wall (WIRCW), were analyzed using diffuse reflectance (DRIFTS) FT-IR. The soaking water and cooking water from the beans were also studied using attenuated total reflectance (ATR) FT-IR. The DRIFTS FT-IR results from the SPF and WIRCW fractions were consistent with previously published data for Carioca beans showing that in general, more phenolic compounds were associated with the SPF of HTC beans than in the control beans. Results also showed that HTC-refrigerated beans had higher concentrations of phenolic compounds than control beans in the SPF. The ATR FT-IR results for soaking and cooking waters from the HTC-refrigerated and HTC beans had higher concentrations of absorbing compounds than the control beans, indicating that they lost more constituents to the water. Additionally, results indicate that the mechanism(s) for reversibility of the HTC defect could be different than the one(s) involved in the development of the defect.     

Characterization of commercial carrageenans by Fourier transform infrared spectroscopy using single-reflection attenuated total reflection

The purity and composition of commercial carrageenans vary widely and, therefore, have to be checked prior to their use in the food industry. Infrared spectroscopy is an alternative method to the expensive and time-consuming wet chemical and NMR methods to characterize carrageenan samples. The use of an attenuated total reflection accessory coupled to a Fourier transform infrared spectrophotometer allows a direct analysis of the sample without any preparation step, which is an additional benefit for the rapid identification check of raw material at reception in an industrial environment. Using a set of calibration samples, three multivariate calibrations were developed to predict the total carrageenan content as well as the molar ratio of kappa- and iota-carrageenans. A validation with an independent set of samples confirmed the robustness of the calibrations and the accuracy of the predictions. The accuracies of the calibrations given by their respective standard errors of prediction are 5.6 g/100 g, and 6.1 mol %, and 6.6 mol %, respectively, for the total carrageenan content and the molar ratios of kappa- and iota-carrageenans. The total preparation and analysis time is <5 min per sample.     

Fourier transform infrared spectroscopic analysis of the polymethoxylated flavone content of orange oil residues

Preliminary studies have shown that orange peel polymethoxylated flavones (PMFs) exhibit beneficial biological properties in animals. These properties have increased the demands for these compounds as candidate nutraceuticals and specialty food ingredients. Orange oil residues are a likely commercial source of the PMFs, and a rapid, solvent-free method for the analysis of the PMFs in orange oil residues has been developed based on Fourier transform infrared (FTIR) spectroscopy. The intensities of the FTIR vibrations of the phenyl ring nu(C=C) stretch at 1515 cm(-1) of the PMFs can be used, relative to the intensity of the carbonyl stretch at 1733 cm(-1) of the non-PMF orange oil residue components, to measure PMF content. Excellent correlations for the ratios of the intensities of these vibrations and the total PMF content were observed irrespective of the source, viscosity, and presence of particulate material. The detection limit by this method is approximately 0.1% PMF.     

Usefulness of the frequency data of the fourier transform infrared spectra to evaluate the degree of oxidation of edible oils

The oxidation process of 13 edible oil samples with different proportions of oleic, linoleic, and linolenic acyl groups has been studied using Fourier transform infrared spectroscopy. The oxidation experiments were carried out by heating the samples in a convection oven at 70 degrees C. Duplicate spectra were recorded from a film of pure oil between two disks of KBr for each sample every day during the course of the oxidation, and frequency data of each band of the spectrum were collected automatically. Changes in the values of the frequency of most of the bands of the spectra were observed. The shiftings of the frequency value of specific bands allowed one to distinguish between the different stages of the oxidation process and to establish the oxidation degree of each oil sample. This methodology could be useful to evaluate the oxidative stability of edible oils in a simple, fast, and accurate way.     

木屑快速热裂解生物油特性及其红外光谱分析

该文以杨木木屑快速热裂解制取的生物油为原料,对其进行了理化特性研究及傅立叶变换红外光谱（FTIR）分析,同时和甜高粱茎秆残渣热裂解生物油的特性进行了比较。结果表明,木屑生物油含水率较低（25.01%）,热值较高（20.62 MJ/kg）,常温下运动黏度为3.44 mm2/s,密度、灰分含量和残炭值分别为1072 kg/m3,0.305%,12.74%,且呈明显的酸性（pH=3.07）。随着温度的升高（25～100℃）,木屑生物油运动黏度明显降低。木屑生物油的较低含水率和较高热值,使其在应用方面优于甜高粱茎秆残渣生物油。然而,从傅立叶变换红外光谱图上不同位置的吸收峰可以判断木屑生物油含有多种官能团,实际应用之前需要进一步的精制。     

缺锌玉米植株的傅立叶变换红外光谱研究

【目的】傅里叶变换红外光谱（fourier transform infrared spectroscopy, FTIR）是一种基于化合物中官能团和极性键振动的结构分析技术。本文利用傅立叶变换红外光谱仪检测缺锌和正常供锌玉米植株不同器官的组分变化,同时比较两个玉米品种植株不同部位的生物量和锌含量,以期为缺锌影响玉米生长与生理代谢的机理研究提供参考。【方法】选取农大108和郑单958两个玉米品种,利用营养液培养方式,设置缺锌和正常处理。1）当玉米出现缺锌症状后,将地上部和根系分开,测量株高和根长,烘干至恒重测干重。2）烘干至恒重的植株样品用HNO3-HClO4（3∶1）消煮,原子吸收分光光度计（型号WFX-120C,北京瑞利分析仪器公司）测定消煮液中锌浓度,计算植株中锌含量和锌积累量。3）收获玉米根系放入FAA固定液（70%酒精∶38%甲醛∶乙酸体积=90∶5∶5）中,利用扫描仪（EsponV700）扫描根系样品获取数字化图像,利用WinRHIZO根系分析软件（Regent Instruments Inc., Canada）对图像进行分析,获得根长、 根面积、 根体积等指标。4）取玉米根、 茎、 叶部分烘干样品,磨碎过0.2 mm筛,采用溴化钾压片法,利用傅立叶变换红外光谱仪（VERTEX 70,Bruker）检测不同部位的光谱特性,OPUS 6.5软件采集数据并进行基线校正。【结果】缺锌胁迫下, 植株地上部锌含量明显下降,低于临界水平（20 g/g）,生物量降低; 缺锌根系面积与体积变小,总根长变小。用缺锌与施锌植株生物量比来表征玉米对缺锌敏感性,品种农大108较郑单958对缺锌更为敏感。缺锌玉米根系和叶片FTIR谱在波数3410、 2920、 1650、 1380、 1055 cm-1附近处透过率较高,茎FTIR谱在这些波数处透过率较低,表明缺锌导致根系和叶片中碳水化合物、 脂类、 蛋白质及核酸含量下降,而在茎中有所积累。农大108植株中各组分变化受缺锌影响较大。【结论】缺锌导致玉米植株生长受抑,利用FTIR技术研究发现缺锌植株中碳水化合物、 脂类、 蛋白质及核酸组分发生变化,农大108植株中各组分变化受缺锌影响较大,品种农大108可能较郑单958对缺锌更为敏感。     

Elucidation of the thermal deterioration mechanism of bio-oil pyrolyzed from rice husk using Fourier transform infrared spectroscopy

In this study, the rationale for exploring the thermal deterioration mechanism of the bio-oil pyrolyzed from rice husk is established. This is based on identification of the unstable intermediates in the thermal deterioration process. Fourier transform infrared (FTIR) spectroscopy was used to monitor such a thermal deterioration process of bio-oil samples in thermal treatment and/or during long-term storage at ambient temperatures of 20-30 °C. Terminal olefins, as a key intermediate, so-called "signature", were identified qualitatively by using FTIR spectroscopy. A band shift observed at 880 cm(-1), which was assigned to the C-H out-of-plane deformation vibration of terminal olefins, indicates the start-up of the bio-oil thermal deterioration. A two-step pathway was proposed to describe the thermal deterioration process of bio-oil. This study suggests that the status of bio-oil could be rapidly monitored by the FTIR method.     

Discrimination of intact and injured Listeria monocytogenes by Fourier transform infrared spectroscopy and principal component analysis

Fourier transform infrared spectroscopy (FT-IR, 4000-600 cm(-)(1)) was used to discriminate between intact and sonication-injured Listeria monocytogenes ATCC 19114 and to distinguish this strain from other selected Listeria strains (L. innocua ATCC 51742, L. innocua ATCC 33090, and L. monocytogenes ATCC 7644). FT-IR vibrational overtone and combination bands from mid-IR active components of intact and injured bacterial cells produced distinctive "fingerprints" at wavenumbers between 1500 and 800 cm(-)(1). Spectral data were analyzed by principal component analysis. Clear segregations of different intact and injured strains of Listeria were observed, suggesting that FT-IR can detect biochemical differences between intact and injured bacterial cells. This technique may provide a tool for the rapid assessment of cell viability and thereby the control of foodborne pathogens.     

Monitoring of denaturation processes in aged beef loin by Fourier transform infrared microspectroscopy

We present the results of a Fourier transform infrared (FT-IR) microspectroscopic study using conventional FT-IR microscopy and FT-IR imaging to detect the denaturation process during four different heating temperatures (raw, 45, 60, and 70 degrees C) spatially resolved in bovine cryosections from longissimus dorsi muscle. FT-IR imaging, employing a focal plane array detector, which allowed the simultaneous collection of spectra at 4096 pixels, enabled the investigation of the heat-induced changes in the two major meat constituents, i.e., myofibrillar and connective tissue proteins, spatially resolved. The infrared spectra of both compounds revealed that the major spectral changes involved an increase in beta-sheet and a decrease in alpha-helical structures, which appeared to be much more pronounced for the myofibers than for the connective tissue. These conformational changes could be correlated to the denaturation of the major meat proteins, such as myosin, actin, and collagen.     

近红外光谱快速检测食用油必需脂肪酸

为了建立食用油必需脂肪酸快速检测的方法,该研究提出了基于近红外光谱技术检测食用油中α-亚麻酸和亚油酸含量的快速测定方法。对光谱信息分别采用偏最小二乘回归方法(PLS)和最小二乘支持向量机(LS-SVM)建立模型。比较了多种光谱预处理方法对模型预测能力的影响。结果表明对于亚油酸含量的预测,采用Savitzky-Golay平滑法结合多元散射校正(MSC)的光谱预处理所建立的LS-SVM模型最优。预测集的决定系数(R2)、预测均方根误差(RMSEP)和剩余预测偏差(RPD)分别达到了0.989,0.0161和9.4783。对于α-亚麻酸含量的预测,采用Savitzky-Golay平滑法结合标准正态变换(SNV)的光谱预处理所建立的LS-SVM模型最优。α-亚麻酸含量预测结果的R2、RMSEP和RPD为0.972,0.0036和6.0561,据此表明,应用近红外光谱技术能够检测食用油中α-亚麻酸和亚油酸的含量,为快速检测食用油的必需脂肪酸提供了参考。     

Discrimination of olives according to fruit quality using Fourier transform Raman spectroscopy and pattern recognition techniques

Fourier transform Raman spectroscopy combined with pattern recognition has been used to discriminate olives of different qualities. They included samples of sound olives, olives with frostbite, olives that have been collected from the ground, fermented olives, and olive samples with diseases. Milled olives were measured in a dedicated sample cup, which was rotated during spectrum acquisition. A preliminary study of the data set structure was performed using hierarchical cluster analysis and principal component analysis. Two supervised pattern recognition techniques, K-nearest neighbors and soft independent modeling of class analogy (SIMCA), were tested using a "leave-a-fourth-out" cross-validation procedure. SIMCA provided the best results, with prediction abilities of 95% for sound, 93% for frostbite, 96% for ground, and 92% for fermented olives. The olive samples with diseases (too few to define a class) were included in the validation and recognized as not belonging to any class. None of the damaged olive samples was wrongly predicted to the class of sound olives. With this approach a selection of sound olives for the production of high-quality virgin olive oil can be achieved.     

Improved method for determination of pectin degree of esterification by diffuse reflectance Fourier transform infrared spectroscopy

An improved method for the determination of pectin degree of esterification (DE) by diffuse reflectance Fourier transform infrared spectroscopy (DRIFTS) was developed. Pectin samples with a range of DE as determined by gas chromatography were used for developing a calibration curve by DRIFTS. A linear relationship between the DE of pectin standards and FTIR peak ratio for ester carboxyl peak area to total carboxyl peak area was found (R(2) = 0.97). Pectin DE of various samples was calculated from the linear fit equation developed by DRIFTS. Accuracy of the DRIFTS method was determined by comparing the DE values of four commercial pectins obtained by DRIFTS methods to the values obtained by the gas chromatography method. Greater precision was obtained for the FTIR measurement of test pectin samples when the ester peak ratio was used relative to the ester peak area.     

Investigation of the potential utility of single-bounce attenuated total reflectance Fourier transform infrared spectroscopy in the analysis of distilled liquors and wines

A new Fourier transform infrared (FTIR) spectroscopic method based on single-bounce attenuated total reflectance (SB-ATR) spectroscopy was developed for the analysis of distilled liquors and wines. For distilled liquors, a partial least-squares (PLS) calibration was developed for alcohol determination based on the SB-ATR/FTIR spectra of mixtures of ethanol and distilled water. An independent set of 12 different distilled liquor samples was predicted from the PLS calibration, and a standard deviation of the differences for accuracy (SDD(a)) between actual and predicted values of 0.142% (v/v) was obtained. The potential utility of SB-ATR/FTIR spectroscopy for the analysis of wines was initially evaluated based on a comparison with Fourier transform near-infrared (FT-NIR) spectroscopy and FTIR spectroscopy using a flow-through transmission cell. PLS calibrations for alcohol, total reducing sugars, total acidity and pH were developed using pre-analyzed wine samples (n = 28), and for SB-ATR/FTIR spectroscopy, the SDD(a) for the leave-one-out cross-validation statistics were of the order of 0.100% (v/v), 0.707 g L(-1), 0.189 g L(-1) (H2SO4), and 0.230, respectively. Overall, the SB-ATR/FTIR results were better than those obtained using FT-NIR spectroscopy and comparable to those obtained with transmission FTIR spectroscopy. A PLS calibration based on preanalyzed wine samples (n = 72) for the prediction of 11 different components and parameters in wines by SB-ATR/FTIR spectroscopy was subsequently developed and validated using an independent sample set (n = 77). Good coefficients of correlation between the reference and predicted values for the validation set were obtained for most of the components and parameters except citric acid, volatile acids, and total SO2. The results of this study demonstrate the suitability of SB-ATR/FTIR spectroscopy for the routine analysis of distilled liquors and wines.     

Using Fourier transform infrared (FT-IR) absorbance spectroscopy and multivariate analysis to study the effect of chlorine-induced bacterial injury in water

The effect of chlorine-induced bacterial injury on spectral features using Fourier transform infrared (FT-IR) absorbance spectroscopy was studied using a mixed bacterial culture of (1:1) ca. 500 CFU/mL each Escherichia coli ATCC 25922 and Pseudomonas aeruginosa ATCC 15442 in 0.9% saline. Bacterial cells were treated with 0, 0.3, or 1.0 ppm of initial free chlorine (21 degrees C, 1 h of contact time). Chlorine-injured and dead bacterial cells retained the ATR spectral properties of uninjured or live cells in the region of C-O-C stretching vibrations of polysaccharides, indicative of the cell wall peptidoglycan layer and lipopolysaccharide outer leaflet. This confirms the observations of others that extensive bacterial membrane damage is not a key factor in the inactivation of bacteria by chlorine. The bactericidal effect of chlorine caused changes in the spectral features of bacterial ester functional groups of lipids, structural proteins, and nucleic acids, with apparent denaturation reflected between 1800 and 1300 cm (-1) for injured bacterial cells. Three-dimensional principal component analysis (PCA) showed distinct segregation and clustering of chlorine-treated and untreated cells. Cells exposed to chlorine at 0.3 or 1.0 ppm could be distinguished from the untreated control 73 and 80% of the time, respectively, using soft independent modeling of class analogy (SIMCA) analysis. This study suggests that FT-IR spectroscopy may be applicable for detecting the presence of injured and viable but not culturable (VBNC) waterborne pathogens that are underestimated or not discernible using conventional microbial techniques.