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1.
Free fatty acid formation and lipid oxidation on milled rice   总被引:2,自引:0,他引:2  
Milled rice was stored at 37°C and 70% humidity and sampled regularly for 50 d. Rice surface lipid was extracted with isopropanol and analyzed for free fatty acids (FFA) and conjugated diene (CD) contents. Diffuse reflectance Fourier transform infrared (DRIFTS) spectra of the rice samples were also obtained. FFA and CD levels increased together during rice storage and exhibited three distinct phases. DRIFTS identified a decrease in intensity at 1746 cm−1 (ester, −C=O) and increases in intensity at 1731 cm−1 (aldehyde, −CO) and 1714 cm−1 (fatty acid, −C=O) during storage, which correlated well with the chemical analysis data. DRIFTS spectral data were analyzed by a partial least squares regression method to identify spectral regions that correlate strongly with measured FFA and construct prediction models. Overall, the mid-infrared region (4000–400 cm1) gave the best model (R=0.98, root mean square error of cross-validation=0.05) and also predcted the FFA content of milled rice well. The DRIFTS technique has potential for use in studying qualitative chemical changes on the milled rice surface lipids and for predicting FFA on milled rice.  相似文献   

2.
Diffuse reflectance Fourier transform infrared spectroscopy was investigated as a method for rice surface lipid determination. Long- and medium-grain rice was milled at four degrees of milling to obtain samples with various levels of residual bran, and total lipids were determined by solvent extraction. Fourier transform infrared spectra were collected between 4000 and 400 cm−1. Weighted regression analysis identified changes in surface chemical functional groups with bran removal. Groups typical of lipids increased with bran content whereas those typical of carbohydrates and protein decreased. Partial least squares (PLS) regression analysis showed a high degree of correlation between the spectra in the 4000–400 cm−1 range and extracted lipids of long-grain rice (R 2=0.96) and medium-grain rice (R 2=0.96); a high degree of correlation was also observed when long- and medium-grain rice data were combined (R 2=0.96). There was a high positive correlation between the spectra and extracted lipids in the 1300–1000 cm−1 range for the long-grain rice (R 2=0.98), medium-grain rice (R 2=0.98), and combined long-/medium-grain rice data (R 2=0.94). PLS selected spectral regions that correlated positively with functional groups of lipid/lipid oxidation products and negatively with functional groups of protein and carbohydrates.  相似文献   

3.
We introduce a visible Raman spectroscopic method for determining the free fatty acid (FFA) content of extra virgin olive oil with the aid of multivariate analysis. Oleic acid was used to increase the FFA content in extra virgin olive oil up to 0.80% in order to extend the calibration span. For calibration purposes, titration was carried out to determine the concentration of FFA for the investigated oil samples. As calibration model for the FFA content (FFA%), a partial least squares (PLS) regression was applied. The accuracy of the Raman calibration model was estimated using the root mean square error (RMSE) of calibration and validation and the correlation coefficient (R 2) between actual and predicted values. The calibration curve of actual FFA% obtained by titration versus predicted values based on Raman spectra was established for different spectral regions. The spectral window (945–1600 cm−1), which includes carotenoid bands, was found to be a useful fingerprint region being statistically significant for the prediction of the FFA%. High R 2 and small RMSE values for calibration and validation could be obtained, respectively.  相似文献   

4.
Fourier transform infrared (FTIR) spectroscopy provides a simple and rapid means of detecting lard blended with chicken, lamb, and cow body fats. The spectral bands associated with chicken, lamb, and cow body fats and their lard blends were recorded, interpreted, and identified. Qualitative differences between the spectra are proposed as a basis for differentiating between the pure animal fats and their blends. A semiquantitative approach is proposed to measure the percent of lard in blends with lamb body fat (LBF) on the basis of the frequency shift of the band in the region 3009–3000 cm−1, using the equation y=0.1616x+3002.10. The coefficient of determination (R 2) was 0.9457 with a standard error (SE) of 1.23. The percentage of lard in lard/LBF blends was also correlated to the absorbance at 1417.89 and 966.39 cm−1 by the equations y=0.0061x+0.1404 (R 2=0.9388, SE=0.018) and y=0.004x+0.1117 (R 2=0.9715, SE=0.009), respectively. For the qualitative determination of lard blended with chicken body fat (CF), the FTIR spectral bands in the frequency ranges of 3008–3000, 1418–1417, 1385–1370, and 1126–1085 cm−1 were employed. Semiquantitative determination by measurement of the absorbance at 3005.6 cm−1 is proposed, using the equation y=0.0071x+0.1301 (R 2=0.983, SE=0.012). The percentage of lard in lard/GF blends was also correlated to the absorbance at 1417.85 cm−1 (y=0.0053x+0.0821, with R 2=0.9233, SE=0.019) and at 1377.58 cm−1 (y=0.0069x+0.1327, with R 2=0.9426, SE=0.022). For blends of lard with cow body fat (CBF) bands in the range 3008–3006 cm−1 and at 1417.8 and 966 cm−1 were used for qualitative detection. The equation y=−0.005x+0.3188 with R 2=0.9831 and SE=0.0086 was obtained for semiquantitative determination at 966.22 cm−1.  相似文献   

5.
A rapid direct Fourier transform infrared (FTIR) spectroscopic method using a 100 μ BaF2 transmission cell was developed for the determination of free fatty acid (FFA) in crude palm oil (CPO) and refined-bleached-deodorized (RBD) palm olein, covering an analytical range of 3.0–6.5% and 0.07–0.6% FFA, respectively. The samples were prepared by hydrolyzing oil with enzyme in an incubator. The optimal calibration models were constructed based on partial least squares (PLS) analysis using the FTIR carboxyl region (C=O) from 1722 to 1690 cm−1. The resulting PLS calibrations were linear over the range tested. The standard errors of calibration (SEC) obtained were 0.08% FFA for CPO with correlation coefficient (R 2) of 0.992 and 0.01% FFA for RBD palm olein with R 2 of 0.994. The standard errors of performance (SEP) were 0.04% FFA for CPO with R 2 of 0.998 and 0.006% FFA for RBD palm olein with R 2 of 0.998, respectively. In terms of reproducibility (r) and accuracy (a), both FTIR and chemical methods showed comparable results. Because of its simpler and more rapid analysis, which is less than 2 min per sample, as well as the minimum use of solvents and labor, FTIR has an advantage over the wet chemical method.  相似文献   

6.
Lam HS  Proctor A  Nyalala J  Morris MD  Smith WG 《Lipids》2004,39(7):687-692
This study was conducted to develop a quantitative FTIR spectroscopy method to measure LDL lipid oxidation products and determine the effect of oxidation on LDL lipid and protein. In vitro LDL oxidation at 37°C for 1 h produced a range of conjugated diene (CD) (0.14–0.26 mM/mg protein) and carbonyl contents (0.9–3.8 μg/g protein) that were used to produce calibration sets. Spectra were collected from the calibration set and partial least squares regression was used to develop calibration models from spectral regions 4000-650, 3750-3000, 1720-1500, and 1180-935 cm−1 to predict CD and carbonyl contents. The optimal models were selected based on their standard error of prediction (SEP), and the selected models were performance-tested with an additional set of LDL spectra. The best models for CD prediction were derived from spectral regions 4000-650 and 1180-935 cm−1 with the lowest SEP of 0.013 and 0.013 mM/mg protein, respectively. The peaks at 1745 (cholesterol and TAG ester C=O stretch), 1710 (carbonyl C-O stretch), and 1621 cm−1 (peptide C=O stretch) positively correlated with LDL oxidation. FTIR and chemometrics revealed protein conformation changes during LDL oxidation and provided a simple technique that has potential for rapidly observing structural changes in human LDL during oxidation and for measuring primary and secondary oxidation products.  相似文献   

7.
The feasibility of employing a portable variable filter array (VFA) IR spectrometer equipped with a transmission flow cell to quantitatively analyze edible oils or biodiesel feedstocks for free fatty acids (FFA) was evaluated. The approach to FFA determination employed was based on a previously reported FTIR method that involves the extraction of FFAs into methanol containing the base NaHNCN, which converts the FFAs to their salts, followed by measurement of the carboxylate absorbance at ~1,573 cm−1 in the spectrum of the methanol phase. When this methodology was implemented on the low-resolution VFA-IR spectrometer, the analytical performance was comparable to that of conventional FTIR instrumentation at FFA concentrations of <1%. However, at higher FFA levels, the relatively weak pulsed IR source of the VFA-IR spectrometer was found to provide insufficient energy for accurate measurement of the carboxylate absorption superimposed on the strong methanol absorption at ~1,450 cm−1. By changing the extraction solvent to ethanol (EtOH), good spectra and calibrations could be obtained over an FFA range of 0–5%, having an overall SD of ±0.07% FFA. Based on this assessment, a VFA-IR spectrometer provides an economical instrumental means for at-line monitoring of FFA levels in crude and refined edible oils and biodiesel feedstocks, capable of analyzing ~20–30 prepared samples per hour.  相似文献   

8.
IR spectroscopy showed that the components react on the CF—binder boundary, as indicated by the differences in the intensity and position of the absorption bands of CO3 2− groups at the frequency of 1805 cm−1 and C=O and >C-O> groups at 1739 and 1241 cm−1. Thermogravimetric analysis showed that the activation energy of degradation of carbon fibre composites (CFC) increases. This indicates formation of thermostable material with a specific structure. The CFC obtained can be classified as difficultly combustible materials. __________ Translated from Khimicheskie Volokna, No. 1, pp. 37–38, January–February, 2008.  相似文献   

9.
The mandate to label food products with the content of total trans fatty acids has led to an increase in demand for sensitive and accurate methodologies for the rapid quantitation of trans fats. Unfortunately, the latest official infrared (IR) spectroscopic method lacks the required sensitivity. A more sensitive IR procedure that requires the measurement of the height of the second derivative (2D) of the trans absorption band at 966 cm−1 was recently proposed; however, a reported inconsistency at low trans levels between GC (0% of total fat) and IR (1.2% of total fat) results for a fully hydrogenated vegetable oil could not be reconciled, and triggered further investigations. For the first time, we recognize and report the presence of weak interference bands (962–956 cm−1) attributed to saturated fats in the IR spectra of trans fats; these interference bands have an adverse impact on the sensitivity and accuracy of the IR determination at low trans levels (≤0.5% of total fat). Therefore, weak spectral features observed at energies below the one expected for trans bands (966 cm−1) in test samples high in saturated fat (coconut oil and cocoa butter) must not be mistaken for trans bands.  相似文献   

10.
Decolorization of Rice Bran Oil Using Modified Kaolin   总被引:1,自引:0,他引:1  
Measurements show that kaolin from Ranong, obtained from a major deposit in southern Thailand, can be modified to produce a material that is suitable for decolorizing rice bran oil. Its sorption properties were determined after various physical and chemical modifications of this kaolin. Physical modification was achieved by grinding via a planetary ball mill (300 rpm for 1 h), and this was followed by chemical treatment using sulfuric or oxalic acids. The optimum decolorization capacity (~80%) was achieved by using 2 M sulfuric acid. With oxalic acid, the best results were obtained with 0.7 M, but these were slightly lower than those obtained with 2 M sulfuric acid. Compared to the original kaolin sample, the specific surface area of the modified clay increased from ~13 to ~244 cm2 g−1, and the total pore volume from 0.06 to 0.43 cm3 g−1. The pore size distribution curves show that most pores are in the mesoporous region with their diameters between 3.0–4.5 nm, and are suitable for adsorption of pigment molecules that are present in rice bran oil. Desorption and spectroscopic studies suggest that both electrostatic and chemical processes are involved in the interaction between pigments and active sites on the clay surface.  相似文献   

11.
Viscosity of crude rice bran oil with the wax content of 0.23–8.60 (% wt/wt) was measured using a coaxial cylindrical viscometer in the temperature range of 297–333 K. The crude oil behaved like pseudoplastic fluid obeying power law with consistency index k=2.0187×10(su−4) c0.2066 e2815/T and flow behavior index n=0.76, where c is the wax content and T is the temperature in Kelvin. Soy lecithin in the range of 1–2% did not affect the rheological properties.  相似文献   

12.
Potential N (SN) and P (SP) supplies, N and P utilization efficiencies and fertilizer recovery rates for the northern Guinea Savanna (NGS) agro-ecological zone of Nigeria were derived from data collected on farmers’ fields, and used as input in the QUantitative Evaluation of the Fertility of Tropical Soils (QUEFTS) model. The potential N supply ranged from 7 to 56 kg N ha−1, with a mean of 25 kg N ha−1, while SP ranged from 2 to 12 kg P ha−1 with a mean of 5 kg P ha−1. Both SN (CV = 42%) and SP (CV = 57%) were highly variable between farmers’ fields. Deriving potential nutrient supply from ‘a’ values gives lower estimates. The empirical equation in QUEFTS that estimates SN ( ) sufficiently predicted the SN of soils in the NGS (RMSE = 8.0 kg N ha−1 index of agreement (IOA) = 0.81). The SP equation () predicted moderately potential P supply (RMSE = 6.80 kg P ha−1, IOA = 0.54). When N or P is maximally accumulated in the plant (i.e., least efficiently utilized), the utilization efficiency was 21 kg grain kg−1 N taken up and 97 kg grain kg−1 P taken up. When these nutrients were maximally diluted in the plant (i.e., most efficiently utilized), the utilization efficiency was 70 kg grain kg−1 N taken up and 600 kg grain kg−1 P taken up. The range in N recovery fraction (NRF) of N fertilizer applied was from 0.30 to 0.57, with a mean of 0.39, while the P recovery fraction (PRF) ranged from 0.10 to 0.66 with a mean of 0.24. Although SP was moderately predicted, when QUEFTS model input parameters were adjusted for the NGS, the model sufficiently (IOA = 0.83, RMSE = 607 kg DM ha−1) estimated maize grain yield in the NGS of Nigeria. The original QUEFTS model however, gave better predictions of maize grain yield as reflected by the lower RMSE (IOA = 0.84, RMSE = 549 kg DM ha−1). Consequently, QUEFTS is a simple and efficient tool for making yield predictions in the NGS of northern Nigeria.  相似文献   

13.
A comparative study was conducted to assess the contact and fumigant toxicities of eleven monoterpenes on two important stored products insects—, Sitophilus oryzae, the rice weevil, and Tribolium castaneum, the rust red flour beetle. The monoterpenes included: camphene, (+)-camphor, (−)-carvone, 1-8-cineole, cuminaldehyde, (l)-fenchone, geraniol, (−)-limonene, (−)-linalool, (−)-menthol, and myrcene. The inhibitory effect of these compounds on acetylcholinesterase (AChE) activity also was examined to explore their possible mode(s) of toxic action. Although most of the compounds were toxic to S. oryzae and T. castaneum, their toxicity varied with insect species and with the bioassay test. In contact toxicity assays, (−)-carvone, geraniol, and cuminaldehyde showed the highest toxicity against S. oryzae with LC50 values of 28.17, 28.76, and 42.08 μg/cm2, respectively. (−)-Carvone (LC50 = 19.80 μg/cm2) was the most effective compound against T. castaneum, followed by cuminaldehyde (LC50 = 32.59 μg/cm2). In contrast, camphene, (+)-camphor, 1-8-cineole, and myrcene had weak activity against both insects (i.e., LC50 values above 500 μg/cm2). In fumigant toxicity assays, 1-8-cineole was the most effective against S. oryzae and T. castaneum (LC50 = 14.19 and 17.16 mg/l, respectively). Structure-toxicity investigations revealed that (−)-carvone—, a ketone—, had the highest contact toxicity against the both insects. 1-8-Cineole—, an ether—, was the most potent fumigant against both insects. In vitro inhibition studies of AChE from adults of S. oryzae showed that cuminaldehyde most effectively inhibited enzyme activity at the two tested concentrations (0.01 and 0.05 M) followed by 1-8-cineole, (−)-limonene, and (l)-fenchone. 1-8-Cineole was the most potent inhibitor of AChE activity from T. castaneum larvae followed by (−)-carvone and (−)-limonene. The results of the present study indicate that (−)-carvone, 1,8-cineole, cuminaldehyde, (l)-fenchone, and (−)-limonene could be effective biocontrol agents against S. oryzae and T. castaneum.  相似文献   

14.
The kinetics of the oxirane cleavage of epoxidized soybean oil (ESO) by methanol (Me) without a catalyst was studied at 50, 60, 65, 70 °C. The rate of oxirane ring opening is given by k[Ep][Me]2, where [Ep] and [Me] are the concentrations of oxiranes in ESO and methanol, respectively and k is a rate constant. From the temperature dependence of the kinetics thermodynamic parameters such as enthalpy (ΔH), entropy (ΔS), free energy of activation (ΔF) and activation energy (ΔE a) were found to be 76.08 (±1.06) kJ mol−1, −118.42 (±3.12) J mol−1 k−1, 111.39 (±2.86) kJ mol−1, and 78.56 (±1.63) kJ mol−1, respectively. The methoxylated polyols formed from the oxirane cleavage reaction , were liquid at room temperature and had three low temperature melting peaks. The results of chemical analysis via titration for residual oxiranes in the reaction system showed good agreement with IR spectroscopy especially the disappearance of epoxy groups at 825, 843 cm−1 and the emergence of hydroxy groups at the OH characteristic absorption peak from 3,100 to 3,800 cm−1.  相似文献   

15.
Estolides were produced from meadowfoam oil fatty acids, oleic, linoleic, petroselinic, andcis-5,cis-13 docosadienoic acids. Estolide reaction mixtures were quantitated by Fourier transform infrared spectroscopy and compared to the area percentages determined by high-performance liquid chromatography. The absorbance frequency of estolide carbonyl (1737 cm−1) is different than the lactone carbonyl (1790 cm−1) and the acid carbonyl (1712 cm−1). Estolide standards were obtained by wiped-film molecular-still distillations and column chromatography.  相似文献   

16.
A new procedure for determining free fatty acids (FFA) in olive oil based on spectroscopic Fourier transform infrared-attenuated total reflectance spectroscopy measurements is proposed. The range of FFA contents of samples was extended by adding oleic acid to several virgin and pure olive oils, from 0.1 to 2.1%. Calibration models were constructed using partial least-squares regression (PLSR). Two wavenumber ranges (1775–1689 cm−1 and 1480–1050 cm−1) and several pretreatments [first and second derivative; standard normal variate (SNV)] were tested. To obtain good results, splitting of the calibration range into two concentration intervals (0.1 to 0.5% and 0.5 to 2.1%) was needed. The use of SNV as a pretreatment allows one to analyze samples of different origins. The best results were those obtained in the 1775–1689 cm−1 range, using 3 PLSR components. In both concentration ranges, at a confidence interval of α = 0.05, no significant differences between the reference values and the calculated values were observed. Reliability of the calibration vs. stressed oil samples was tested, obtaining satisfactory results. The developed method was rapid, with a total analysis time of 5 min; it is environment-friendly, and it is applicable to samples of different categories (extra virgin, virgin, pure, and pomace oil).  相似文献   

17.
The curing of drying oils at 60°C has been investigated by Fourier transform infrared spectroscopy and Fourier transform Raman analysis of linseed oil and poppyseed oil. In the first step, hydroperoxides are formed (broad vibration band centered around 3425 cm−1) with concomitant conjugation and cis-trans isomerization of the double bonds (disappearance of cis bands at 3011 and 716 cm−1, appearance of trans conjugated and trans nonconjugated bands at 987 and 970 cm−1). The subsequent decomposition of hydroperoxides in the presence of oxygen leads to the formation of alcohols (nitrite band at 779 cm−1 after nitrogen monoxide treatment), aldehydes (bands at 2810 and 2717 cm−1 in gas phase), ketones (saturated and unsaturated at 1720 and 1698 cm−1, respectively), carboxylic acids (saturated and unsaturated acid fluorides identified at 1843 and 1810 cm−1 after SF4 treatment), and peresters or γ-lactones (near 1770 cm−1). A rapid decrease in the double-bond concentration is recorded when curing continues, and the formation of epoxides, characterized by a vibration band at 885 cm−1, is observed. Thermolysis experiments have suggested the proposal of a reaction of addition of peroxyl radicals on the conjugated double bonds as a probable mechanism. This mechanism explains both the rapid disappearance of conjugated double bonds and the formation of epoxides as intermediate products observed in the initial step of curing.  相似文献   

18.
Seven members of this homologous series have been studied by differential scanning calorimetry (DSC), and their melting point, enthalpy and entropy of fusion obtained. The entropy change for each additional carbon-carbon bond in the aliphatic acid chain closely observed the valueR ln 3, as expected for flexible molecules. IR spectra of crystalline glycidyl miristate, palmitate and stearate showed the typical band progression in the 1180–1350 cm−1 region and a doublet at ca. 720±10 cm−1. Glycidyl esters appeared to be free of polymorphism, since no differences in the behavior of solids crystallized from solvent or from the melt were observed either by DSC or by IR spectroscopy.  相似文献   

19.
Takashi Nakamura 《Lipids》1985,20(3):180-186
The chemical structures of lipid degradation products capable of reacting with amino acids and forming red pigments were investigated. The red pigment-forming substances (RPS's) derived from autoxidized linolenate in triglyceride of linseed oil were purified successively by gel chromatography on Sephadex LH-20, column chromatography and TLC on Silica gel 60, and HPLC on μ-Porasil. Consequently, three types of RPS's were isolated. IR spectra of RPS's were similar, except for slight differences in the fingerprint region (1300—650 cm−1). These substances included the OH group (3500 cm−1 region), conjugated aldehyde (νC=0 1688 cm−1, νC=C 1635 cm−1) and ketone (νC=0 1740 cm−1) in their molecules. RPS's were analyzed by GLC and GC-MS after derivatization with dimethylhydrazine and/or trimethylsilyl reagents, before and after the reduction with NaBH4 and/or hydrogenation with PtO2. The fragmentation patterns indicated the presence of an ethyl group in addition to the functional groups described above, and the molecular formula was estimated to be C10H14O3. Further elucidation of the structures was obtained by13C- and1H-NMR analyses, and evidence was obtained for the presence of a hydroxypentanone ring, a PG-like structure. The sequence of the protons on the ring carbons was unequivocally deduced from the double resonance experiments. All the data taken together suggested that the RPS's were the stereoisomer of 3-(2-ethyl-5-hydroxy-3-oxo) cyclopentanyl-2-propenal. Presented at the General Meeting of JSSF held in Tokyo University of Fisheries, Tokyo, April 1983.  相似文献   

20.
Crop residues are important sources of organic matter and plant nutrients and known to affect soil quality. Tillage affects residue decomposition and nutrient cycling processes. A 2 year field study was aimed to investigate the decomposition and nutrient dynamics from surface-placed and incorporated rice (Oryza sativa L.) residue on two soil types using the nylon mesh bag technique over wheat cropping cycle in rice–wheat system in northwestern India. A single-pool first-order exponential decay function showed R 2 larger than 0.9. Over the wheat growing cycle about 20% of buried rice residue and 50% of surface-placed residue remained undecomposed. Nitrogen exponential decay models were significant at P < 0.01. At wheat boot stage (1,100 growing degree days, DGD) 12 kg N ha−1 (27% of the initial N) was released from the buried residue losing 60–65% of its N at the end of decomposition cycle. Nitrogen in surface rice residue increased throughout the decomposition cycle due to microbiological immobilization. The change in P with time (DGD) was small and weakly defined by the exponential function. Nutrient dynamics of rice residue indicate that it is not a potential source of N and P for wheat over short-term. The change in K concentration was well described by exponential function (R 2 0.73–0.86). Potassium in rice residue decreased at a fast rate during the initial 20 days (400 DGD) and >80% was released by 40 days (680 DGD).  相似文献   

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