β-Carotene content is usually determined by using ultraviolet (UV)-visible spectrophotometry at 446 nm. In this study, two spectroscopic techniques, namely, Fourier transform infrared (FTIR) and near infrared (NIR) spectroscopy, have been investigated and compared to UV-visible spectrophotometry to measure the β-carotene content of crude palm oil (CPO). Calibration curves ranging from 200 to 800 ppm were prepared by extracting β-carotene from original CPO using open-column chromatography. Separate partial least squares calibration models were developed for predicting β-carotene based on the spectral region from 976 to 926 cm −1 for FTIR spectroscopy and 546 to 819 nm for NIR spectroscopy. The correlation coefficient (R 2 ) and standard error of calibration obtained were 0.972 and 25.2 for FTIR and 0.952 and 23.6 for NIR techniques, respectively. The validation set gave R 2 of 0.951 with standard error of performance (SEP) of 25.78 for FTIR technique and R 2 of 0.979 with SEP of 19.96 for NIR technique. The overall reproducibility and accuracy did not give comparable results to that of spectrophotometric method; however, the standard deviation of prediction was still within ±5% β-carotene content over the range tested. Because of their rapidness and simplicity, both FTIR and NIR techniques provide alternative means of measuring β-carotene content in CPO. In addition, these two spectroscopic techniques are environmentally friendly since no solvent is involved.Paper no. J8796 in JAOCS 76, 249-254 (February 1999).
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.
A near-infrared (NIR) spectroscopy calibration was developed for the determination of free fatty acids (FFA) in crude palm oil and its fractions based on the NIR reflectance approach. A range of FFA concentrations was prepared by hydrolyzing oil with 0.15% (w/w) lipase in an incubator at 60°C (200 rpm). Sample preparation was performed in Dutch cup, and the spectra were measured in duplicate for each sample. The optimized calibration models were constructed with multiple linear regression analysis based on C=O overtone regions from 1850-2050 nm. The best wavelength combinations were 1882, 2010, and 2040 nm. Multiple correlation coefficients squared (R 2 ) were: 0.994 for crude palm oil, 0.961 for refinedbleached-deodorized (RBD) palm olein, and 0.971 for RBD palm oil. Calibrations were validated with an independent set of 8-10 samples. R 2 of validation were 0.997, 0.943, and 0.945, respectively. The developed method was rapid, with a total analysis time of 5 min, and environmentally friendly, and its accuracy was generally good for raw-material quality control. JAOCS 75, 557-562 (1998).
A rapid direct Fourier transform infrared (FTIR) spectroscopic method using a 100 µ BaF 2 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.Paper no. J8749 in JAOCS 76, 485-490 (April 1999).
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