Abstract
An FTIR spectrometer coupled to an autosampler and attendant methodologies for high-volume automated quantitative analysis of free fatty acids (FFA) or moisture in edible oils are described. Samples are prepared by adding 20 g of oil to a 50 ml screw-capped vial, to which is added either a methanol/NaHNCN solution or dry acetonitrile in a I:I (w/v) ratio for FFA or H2O analysis, respectively. After capping with Mylar-lined septum caps, the vials are loaded into an autosampler tray, which is then agitated vigorously to extract the constituent of interest from the oil into the oil-immiscible solvent, and are then left to stand for ∼ 10 min to allow for phase separation. The upper solvent layer in each vial is aspirated successively into the IR cell, with the Mylar seal allowing facile autosampler needle penetration into the vials. The spectra of the sample extraction solvents serve as spectral backgrounds in addition to being used in monitoring cell path length and verifying cell loading. FFA and H2O analyses are carried out using 100 and 500 μm CaF2 cells, respectively. For FFA analysis, quantification is achieved using the ν (COO) band at 1573 cm−1, while moisture is determined using water absorption bands at 3629 or 1631 cm−1, depending on the moisture range of the samples. Calibration procedures and data are presented. The spectrometer and autosampler are controlled using proprietary Universal Method Platform for InfraRed Evaluation software, which provides a simple user interface and automates the spectral analysis; the output data can also be sent to a Laboratory Information Management System. Validation and performance data obtained with this automated system demonstrate that it is capable of analyzing >60 samples/h, a rate commensurate with the throughput required by commercial contract or high-volume process control laboratories.
| Original language | English |
|---|---|
| Pages (from-to) | 23-29 |
| Number of pages | 7 |
| Journal | Journal of laboratory automation |
| Volume | 11 |
| Issue number | 1 |
| DOIs | |
| Publication status | Published - 2006 |
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Keywords
- automation
- edible oils
- free fatty acids
- FTIR
- water
ASJC Scopus subject areas
- Computer Science Applications
- Medical Laboratory Technology
Cite this
Automated FTIR Analysis of Free Fatty Acids or Moisture in Edible Oils. / al-Alawi, Ahmed; Van de Voort, Frederick R.; Sedman, Jacqueline; Ghetler, Andrew.
In: Journal of laboratory automation, Vol. 11, No. 1, 2006, p. 23-29.Research output: Contribution to journal › Article
}
TY - JOUR
T1 - Automated FTIR Analysis of Free Fatty Acids or Moisture in Edible Oils
AU - al-Alawi, Ahmed
AU - Van de Voort, Frederick R.
AU - Sedman, Jacqueline
AU - Ghetler, Andrew
PY - 2006
Y1 - 2006
N2 - An FTIR spectrometer coupled to an autosampler and attendant methodologies for high-volume automated quantitative analysis of free fatty acids (FFA) or moisture in edible oils are described. Samples are prepared by adding 20 g of oil to a 50 ml screw-capped vial, to which is added either a methanol/NaHNCN solution or dry acetonitrile in a I:I (w/v) ratio for FFA or H2O analysis, respectively. After capping with Mylar-lined septum caps, the vials are loaded into an autosampler tray, which is then agitated vigorously to extract the constituent of interest from the oil into the oil-immiscible solvent, and are then left to stand for ∼ 10 min to allow for phase separation. The upper solvent layer in each vial is aspirated successively into the IR cell, with the Mylar seal allowing facile autosampler needle penetration into the vials. The spectra of the sample extraction solvents serve as spectral backgrounds in addition to being used in monitoring cell path length and verifying cell loading. FFA and H2O analyses are carried out using 100 and 500 μm CaF2 cells, respectively. For FFA analysis, quantification is achieved using the ν (COO) band at 1573 cm−1, while moisture is determined using water absorption bands at 3629 or 1631 cm−1, depending on the moisture range of the samples. Calibration procedures and data are presented. The spectrometer and autosampler are controlled using proprietary Universal Method Platform for InfraRed Evaluation software, which provides a simple user interface and automates the spectral analysis; the output data can also be sent to a Laboratory Information Management System. Validation and performance data obtained with this automated system demonstrate that it is capable of analyzing >60 samples/h, a rate commensurate with the throughput required by commercial contract or high-volume process control laboratories.
AB - An FTIR spectrometer coupled to an autosampler and attendant methodologies for high-volume automated quantitative analysis of free fatty acids (FFA) or moisture in edible oils are described. Samples are prepared by adding 20 g of oil to a 50 ml screw-capped vial, to which is added either a methanol/NaHNCN solution or dry acetonitrile in a I:I (w/v) ratio for FFA or H2O analysis, respectively. After capping with Mylar-lined septum caps, the vials are loaded into an autosampler tray, which is then agitated vigorously to extract the constituent of interest from the oil into the oil-immiscible solvent, and are then left to stand for ∼ 10 min to allow for phase separation. The upper solvent layer in each vial is aspirated successively into the IR cell, with the Mylar seal allowing facile autosampler needle penetration into the vials. The spectra of the sample extraction solvents serve as spectral backgrounds in addition to being used in monitoring cell path length and verifying cell loading. FFA and H2O analyses are carried out using 100 and 500 μm CaF2 cells, respectively. For FFA analysis, quantification is achieved using the ν (COO) band at 1573 cm−1, while moisture is determined using water absorption bands at 3629 or 1631 cm−1, depending on the moisture range of the samples. Calibration procedures and data are presented. The spectrometer and autosampler are controlled using proprietary Universal Method Platform for InfraRed Evaluation software, which provides a simple user interface and automates the spectral analysis; the output data can also be sent to a Laboratory Information Management System. Validation and performance data obtained with this automated system demonstrate that it is capable of analyzing >60 samples/h, a rate commensurate with the throughput required by commercial contract or high-volume process control laboratories.
KW - automation
KW - edible oils
KW - free fatty acids
KW - FTIR
KW - water
UR - http://www.scopus.com/inward/record.url?scp=32544447024&partnerID=8YFLogxK
UR - http://www.scopus.com/inward/citedby.url?scp=32544447024&partnerID=8YFLogxK
U2 - 10.1016/j.jala.2005.11.002
DO - 10.1016/j.jala.2005.11.002
M3 - Article
VL - 11
SP - 23
EP - 29
JO - JALA - Journal of the Association for Laboratory Automation
JF - JALA - Journal of the Association for Laboratory Automation
SN - 1535-5535
IS - 1
ER -