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1.
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   

2.
A near infrared (NIR) spectroscopic method was developed to measure peroxide value (PV) in crude palm oil (CPO). Calibration standards were prepared by oxidizing CPO in a fermentor at 90°C. A partial least squares (PLS) calibration model for predicting PV was developed based on the NIR spectral region from 1350 to 1480 nm with reference to single-point baseline at 1514 nm. The optimization of calibration factors was guided by the predicted residual error sum of squares test. The standard error of calibration obtained was 0.156 over the analytical range of 2.17–10.28 PV and the correlation coefficient (R 2) was 0.994. The method was validated with an independent set of samples which was prepared in the same manner on a different day. A linear relationship between the American Oil Chemists’ Society and the NIR methods was obtained with R 2 of 0.996 and standard error of performance of 0.17. This study has demonstrated that the prediction of PV in the NIR region is possible. The method developed is rapid, with total analysis time less than 2 min, is environmentally friendly, and its accuracy is generally good for quality control of CPO.  相似文献   

3.
Fourier transform infrared (FTIR) spectra of palm oil samples between 2900 and 2800 cm−1 and 1800 and 1600 cm−1 were used to compare different multivariate calibration techniques for quantitative determination of their thiobarbituric acid-reactive substance (TBARS) content. Fifty spectra (in duplicate) of palm oil with TBARS values between 0 and 0.25 were used to calibrate models based on partial least squares (PLS) and principal components regression (PCR) analyses with different baselines. The methods were compared for the number of factors, coefficients of determination (R 2), and accuracy of estimation. The standard errors of prediction (SEP) were calculated to compare their predictive ability. The calibrated models generated three to eight factors, R 2 of 0.9414 to 0.9803, standard error of estimation (SEE) of 0.0063 to 0.0680, and SEP of 1.20 to 6.67.  相似文献   

4.
A simple, rapid, and direct Fourier transform infrared (FTIR) spectroscopic method was developed for the determination of moisture content of crude palm oil (CPO). The calibration set was prepared by adding double-distilled water to dried CPO in ratios (w/w) between 0 and 13% moisture. A partial least squares (PLS) regression technique was employed to construct a calibration model followed by cross-validation step. The accuracy of this method was comparable to the accuracy of the American Oil Chemists' Society's vacuum oven method, which is used for determination of moisture and volatile matter, with mean difference (MDa) of 0.0105, a coefficient of determination (R 2) and a standard error of calibration (SEC) of 0.9781 and 0.91, respectively. It is also comparable to the accuracy of the International Union of Pure and Applied Chemistry's distillation method with MDa, R 2, and SEC of 0.0695, 0.9701, and 0.65, respectively. The study showed that midband FTIR spectroscopy combined with the PLS regression calibration technique is rapid and accurate for determination of moisture content of CPO samples with a total analysis time of less than 2 min and less than 2 mL of sample.  相似文献   

5.
A method was developed to determine the total phospholipid content in vegetable oil by Fourier transform infrared spectroscopy (FTIR). Calibration curves of I-α-phosphatidylcholine (PC), I-α-phosphatidylethanolamine (PE), and I-α-phosphatidylinositol (PI) in hexane were generated at different concentrations. The optimal phospholipid absorption bands between 1200–970 cm−1 were identified and used for quantitative determination. High R 2≥0.968 were observed between band areas and phospholipid standard concentrations. Phospholipids from crude soybean oil were obtained by water degumming, and purification was performed on a silicic acid column. The phospholipid contents of purified phospholipid extract, degummed and crude soybean oil determined from calibration equations were >90, 0.0113, and 1.77%, respectively. High correlations of determination (R 2≥0.933) were observed between the FTIR method and thin-layer chromatography-imaging densitometry method for the determination of phospholipid content. FTIR was found to be a useful analytical tool for simple and rapid quantitative determination of phospholipids in vegetable oil.  相似文献   

6.
To verify the feasibility of the determination of the Si?H content (HC) of hydrogen silicone oil (HS‐oil) with Fourier transform near infrared (FT‐NIR) spectroscopy and attenuated total reflectance (ATR)–Fourier transform infrared (FTIR) spectroscopy combined with the partial least squares regression (PLS‐R) model, HS‐oil samples were synthesized from concentrated hydrosilicone oil (HC = 1.4 wt %), octamethylcyclotetrasiloxane, and hexamethyldisiloxane or prepared by the dilution of concentrated hydrosilicone oil with octamethylcyclotetrasiloxane. The FT‐NIR PLS‐R model (8695–4000 cm?1, two principal components) was developed from the FT‐NIR spectral data, and the coefficient of determination for cross‐validation (R2) and the coefficient of determination for external validation (r2) were 0.992 and 0.995, respectively. The ATR–FTIR PLS‐R model (2302–2040 cm?1, one principal component) was developed from the ATR–FTIR spectral data; it produced an R2 of 0.995 and an r2 of 0.996. This study demonstrated that the combination of FT‐NIR and ATR–FTIR spectroscopy with the PLS‐R model were successfully used to determine the HC of the HS‐oil. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40694.  相似文献   

7.
Trans fat poses serious health risks to consumers. In order to meet the FDA labeling requirements for trans fatty acids, development of fast, accurate, easy-to-use analytical methods for oils, fats and related products is desirable. Fourier transform infrared spectroscopy (FTIR) is a well-established analytical technique for quantifying trans fats, and the development of handheld FTIR units over the past decade presents new application opportunities. Our objective was to evaluate the performance of a handheld FTIR sensor for measuring trans fat content between 0.1 and 20% trans (w/w) in edible saturated and unsaturated oils. Calibration models were built by measuring height of the band at 966 cm−1 and by partial least squares regression (PLSR) using benchtop FTIR as a reference method. Predictive accuracy of the models was validated with an independent test set of commercial edible oils. Calibration models developed using PLSR and linear regression of band heights gave correlation coefficients R 2 > 0.98. Multivariate analysis for the handheld unit gave standard error of prediction (SEP) of approximately 1%, comparable to values obtained with benchtop systems. This study demonstrates that handheld FTIR spectroscopy coupled with chemometrics is a suitable method for quantitation of trans fat content.  相似文献   

8.
It is difficult to remove β-carotene from oils with alumina-column chromatography, because β-carotene is even less-polar than triacylglycerols (TAGs) are. The objective of this study was to obtain butter oil TAGs free from β-carotene and antioxidants via sequential treatments with activated carbon (AC) adsorption and alumina column chromatography. The AC used was prepared from waste apricots. The effects of AC dosages, temperatures and time courses on β-carotene adsorption were studied. The Langmuir and Freundlich isotherms were used to describe the adsorption of β-carotene onto AC, and it was found to be more consistent with the Freundlich isotherm with a higher R 2 value (0.9784). Adsorption kinetics of β-carotene was analyzed by pseudo-first order and pseudo-second order models. The pseudo-second order model was found to explain the kinetics of β-carotene adsorption more effectively (R 2 = 0.9882). The highest β-carotene reduction was achieved (from 31.9 to 1.84 mg/kg) at an AC dosage of 10 wt%, temperature of 50 °C, and adsorption time of 240 min. A considerable amount of α-tocopherol was also adsorbed during the AC treatment. Remaining portions of α-tocopherol were completely removed with alumina adsorption chromatography. The method described may be used for purification of vegetable oil TAGs, which will be used as model compounds in model oxidation studies.  相似文献   

9.
A new method was developed to determine the gossypol content in cottonseed oil using FTIR spectroscopy with a NaCl transmission cell. The wavelengths used were selected by spiking clean cottonseed oil to gossypol concentrations of 0–5% and noting the regions of maximal absorbance. Transmittance values from the wavelength regions 3600–2520 and 1900–800 cm−1 and a partial least squares (PLS) method were used to derive FTIR spectroscopic calibration models for crude cottonseed, semirefined cottonseed, and gossypol-spiked cottonseed oils. The coefficients of determination (R 2) for the models were computed by comparing the results from the FTIR spectroscopy against those obtained by AOCS method Ba 8-78. The R 2 were 0.9511, 0.9116, and 0.9363 for crude cottonseed, semirefined cottonseed, and gossypol-spiked cottonseed oils, respectively. The SE of calibration were 0.042, 0.009, and 0.060, respectively. The calibration models were cross-validated within the same set of oil samples. The SD of the difference for repeatability and accuracy of the FTIR method were better than those for the chemical method. With its speed (ca. 2 min) and ease of data manipulation, FTIR spectroscopy is a useful alternative to standard wet chemical methods for rapid and routine determination of gossypol in process and/or quality control for cottonseed oil.  相似文献   

10.
A new, rapid, and direct method was developed for the determination of moisture content in biodiesel produced from various types of oils using Fourier transform infrared (FTIR) spectroscopy with an attenuated total reflectance (ATR) element. Samples of biodiesels used in this study were produced using sludge palm oil (SPO). The calibration set was prepared by spiking double-distilled water into dried biodiesel samples in ratios (w/w) between 0 and 10% moisture. Absorbance values from the wavelength regions 3,700–3,075 and 1,700–1,500 cm−1, and the partial least square (PLS) regression method were used to derive a FTIR spectroscopic calibration model for moisture content in biodiesel samples. The coefficient of determinations (R 2) for the models was computed by comparing the results obtained from FTIR spectroscopy against the values of the moisture concentrations (%) determined using the American Oil Chemists’ Society (AOCS) oven method Ca 2d-25. Same comparison was done using International Union of Pure and Applied Chemistry (IUPAC) distillation method 2.602. R 2 was 0.9793 and 0.9700 using AOCS and IUPAC methods, respectively. The standard error (SE) of calibration was 1.84. The calibration model was cross validated within the same set of samples, and the standard deviation (SD) of the difference for repeatability (SDDr) and accuracy (SDDa) of the FTIR method was determined. With its speed and ease of data manipulation, FTIR spectroscopy is a useful alternative method to other methods for rapid and routine determination of moisture content in biodiesel for quality control.  相似文献   

11.
To verify the feasibility of the determination of the Si? H content (HC) of hydrogen silicone oil (HS‐oil) with Fourier transform near infrared (FT‐NIR) spectroscopy and attenuated total reflectance (ATR)–Fourier transform infrared (FTIR) spectroscopy combined with the partial least squares regression (PLS‐R) model, HS‐oil samples were synthesized from concentrated hydrosilicone oil (HC = 1.4 wt %), octamethylcyclotetrasiloxane, and hexamethyldisiloxane or prepared by the dilution of concentrated hydrosilicone oil with octamethylcyclotetrasiloxane. The FT‐NIR PLS‐R model (8695–4000 cm?1, two principal components) was developed from the FT‐NIR spectral data, and the coefficient of determination for cross‐validation (R2) and the coefficient of determination for external validation (r2) were 0.992 and 0.995, respectively. The ATR–FTIR PLS‐R model (2302–2040 cm?1, one principal component) was developed from the ATR–FTIR spectral data; it produced an R2 of 0.995 and an r2 of 0.996. This study demonstrated that the combination of FT‐NIR and ATR–FTIR spectroscopy with the PLS‐R model were successfully used to determine the HC of the HS‐oil. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40694.  相似文献   

12.
A new analytical method was developed for the determination of aflatoxins in groundnut and groundnut cakes by Fourier transform infrared (FTIR) spectroscopy using horizontal attenuated total reflectance technique. Groundnut and groundnut cake samples were used in this study. The wave-lengths were selected for the four types of aflatoxins—B1, B2, G1, and G2—and the standards prepared for earch by spiking some clean sample with the aflatoxins in concentrations of 0–1200 parts per billion. A partial least square regression was used to derive the calibration models for each toxin. The coefficients of determination (R 2) of the calibration model were computed for the FTIR spectroscopy predicted values vs. actual values of aflatoxins in parts per billion. The R 2 was found to be 0.9911, 0.9859, 0.9986, and 0.9789 for aflatoxins B1, B2, G1 and G2, respectively. Standard errors of calibration for groundnut samples were found to be 1.80, 2.03, 1.42, and 2.05 for aflatoxins B1, B2, G1, and G2, respectively. Calibration models were validated with an independent set of samples. The R 2 of validation models were computed. The SD of the difference for repeatability of the FTIR method was found to be better than that of the chemical method. Based on the results obtained, FTIR spectroscopy can be a useful instrumental method for determining aflatoxins in oilseeds and oilseed cakes. With its speed and ease of data manipulation by computer software, it is a possible alternative to the standard wet chemical methods for a rapid and accurate routine determination of aflatoxin levels in food and feed.  相似文献   

13.
A rapid method for the quantitative determination of iodine value (IV) of palm oil products by FTIR transmission spectroscopy is described. A calibration standard was developed by blending palm stearin and superolein in specific ratios that covered a range of 27.9 to 65.3 IV units. The spectra of these standards was measured in the range between 3050 and 2984 cm−1, corresponding to the absorption band of=C-H cis stretching vibration. A partial least squares calibration model for the prediction of IV was developed to quantify the IV of palm oil products. A validation approach was used to optimize the calibration with a correlation coefficient of R 2=0.9995 and a standard error of prediction of 0.151. This study concludes that the FTIR transmission approach can be used to determine the IV of palm oil products with a total analysis time per sample of less than 2 min for liquid samples.  相似文献   

14.
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   

15.
Quantitative procedures employing liquid-chromatography/particle beam mass spectrometry (LC/PB-MS) and gas chromatography-mass spectrometry (GC-MS) were applied to the determination of the endogenous and 13C-labeled β-carotene, lutein, and retinol in plasma of a subject who consumed kale (Brassica oleracea) that had been grown in a 13CO2-enriched atmosphere. All compounds were analyzed in the negative chemical ionization (NCI) mode using methane as the moderating reagent gas. β-Carotene and lutein were analyzed using LC/PB-MS applying reversed-phase high-performance liquid chromatography (HPLC) separation procedures to resolve the analytes. The concentrations of the β-carotene isotopomers in the plasma over a several-week period were determined using 2H8-β-carotene as an internal standard. The total plasma concentrations of all trans-lutein were quantified by HPLC analysis with a photodiode array detector using β-apo-8′-carotenal as an internal standard, and the ratio of the 13C∶12C isotopomers of lutein was determined by PB-MS. The retinol isotopomers were collected from individual HPLC fractions of the plasma extract and then analyzed as the trimethylsilyl ethers by GC-MS in the NCI mode. The 13C-and 12C-retinol isotopomers were quantified using 2H4-retinol as an internal standard. These methods demonstrate the application of highly sensitive procedures empolying NCI MS for the quantitative determination of carotenoids and vitamin A for the purpose of conducting metabolism studies of phytonutrients.  相似文献   

16.
Application of FTIR spectroscopy in determining sesamol in sesame seed oil   总被引:2,自引:0,他引:2  
A new analytical method was developed for determining sesamol in sesame seed oil by FTIR spectroscopy. Sesamol was also spiked at 0 to 1000 mg/kg in freshly refined, bleached, and deodorized palm olein (RBDPOo) and groundnut (peanut) oil. FTIR spectra were recorded using a transmission (NaCl) cell accessory at room temperature, and the partial least squares regression statistical method was used to derive calibration models for each oil. The standard errors of calibration were 6.07, 5.88, and 4.24 mg/100 g for sesame, RBDPOo, and groundnut oils, with coefficients of determination (R 2) of 0.9947, 0.9940, and 0.9662, respectively. The calibration models were validated by the “leave-one-out” cross-validation method, and the R 2 of validation, the standard errors of prediction, and SD of the differences for repeatability and accuracy were computed. Our results support the premise that FTIR spectroscopy is an efficient and accurate method for determining minor components such as sesamol in edible oils.  相似文献   

17.
Rapid Fourier transform infrared (FTIR) spectroscopy combined with attenuated total reflectance (ATR) was applied for quantitative analysis of virgin coconut oil (VCO) in binary mixtures with olive oil (OO) and palm oil (PO). The spectral bands correlated with VCO, OO, PO; blends of VCO and OO; VCO and PO were scanned, interpreted, and identified. Two multivariate calibration methods, partial least square (PLS) and principal component regression (PCR), were used to construct the calibration models that correlate between actual and FTIR-predicted values of VCO contents in the mixtures at the FTIR spectral frequencies of 1,120–1,105 and 965–960 cm−1. The calibration models obtained were cross validated using the “leave one out” method. PLS at these frequencies showed the best calibration model, in terms of the highest coefficient of determination (R 2) and the lowest of root mean standard error of calibration (RMSEC) with R 2 = 0.9992 and RMSEC = 0.756, respectively, for VCO in mixture with OO. Meanwhile, the R 2 and RMSEC values obtained for VCO in mixture with PO were 0.9996 and 0.494, respectively. In general, FTIR spectroscopy serves as a suitable technique for determination of VCO in mixture with the other oils.  相似文献   

18.
The effects of 0, 1.0 × 10”−5, 2.5 × 10−5, and 5.0 × 10−5 M β-apo-8'-carotenal, β-carotene, and canthaxanthin on the photooxidation of soybean oil in methylene chloride containing 3.3 × 10−9 M chlorophyll b were studied by measuring peroxide values and conjugated diene content. β-Apo-8'-carotenal, β-carotene, and canthaxanthin contain 10,11, and 13 conjugated double bonds, respectively. The peroxide values and conjugated diene contents of oils containing the carotenoids were significantly lower (P<0.05) than those of control oil containing no carotenoid. As the number of conjugated double bonds of the carotenoids increased, the peroxide values of soybean oils decreased significantly (P<0.05). The quenching mechanisms and kinetics of the carotenoids in the photosensitized oxidation of soybean oil were studied by measuring peroxide values. The steady-state kinetics study showed that carotenoids quenched singlet oxygen to reduce chlorophyll-sensitized photooxidation of soybean oil. The singlet-oxygen quenching rate constants ofβ- apo-8'-carotenal, β-carotene, and canthaxanthin were 3.06 × 109, 4.60 × 109, and 1.12 × 1010 M−1sec−1, respectively.  相似文献   

19.
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   

20.
Palm carotene was successfully concentrated from crude palm oil (CPO) by an adsorption process using a synthetic adsorbent followed by solvent extraction. Evaluation of feed CPO and CPO which underwent the carotene extraction process was conducted. The quality of CPO after the extraction process was slightly deteriorated in terms of free fatty acid, moisture content, impurities, peroxide value, anisidine value, discriminant function, and deterioration of bleachability index. However, the CPO still can be refined to produce refined, bleached, deodorized palm oil that meets the Palm Oil Refiners Association of Malaysia specifications. No extra cost was incurred by refining this CPO as the dosage of bleaching earth used was very similar to the refining of standard CPO. The triglyceride carbon number and fatty acid composition of CPO after going through the carotene extraction process were almost the same as CPO data. The major components of the carotene fraction were similar to CPO, which contains mainly α- and β-carotene. The carotene could be stored for at least 3 mon.  相似文献   

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