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  • Comprehensive thin layer chromatography×gas chromatography using headspace sampling modulation-A case study on fatty acid composition analysis.

Comprehensive thin layer chromatography×gas chromatography using headspace sampling modulation-A case study on fatty acid composition analysis.

Journal of chromatography. A (2015-06-24)
Mitja Križman, Alenka Pušar
ABSTRACT

The recently developed comprehensive TLC×GC technique using headspace sampling is presented. The main advantage of this approach, as demonstrated in lipid analysis, is the possibility to include a transesterification step of glycerides into fatty acid methyl ester derivatives (FAME) because no particular constraints in terms of operational time between TLC and GC are present. Besides being a relatively low-cost solution, TLC×GC by means of headspace sampling provides many benefits in terms of flexibility of separation conditions and modulation sampling width. The technique provides over two orders of magnitude of linear range with TLC sample loads of about 1mg with good reproducibility and accuracy, as demonstrated by multiple headspace extraction (MHE) tests. The technique is a viable alternative to the established but more expensive HPLC×GC technique. The useful range of TLC×GC in terms of analyte volatility can be further extended with a future development of devices based on thermal desorption.

MATERIALS
Product Number
Brand
Product Description

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Diethyl ether, suitable for residue analysis, JIS 5000
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Methanol, SAJ special grade
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Methanol, suitable for HPLC
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Chloroform, suitable for HPLC
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Diethyl ether, JIS 300, ≥99.5%, suitable for residue analysis
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Sulfuric acid, SAJ first grade, ≥95.0%
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Sulfuric acid solution, 0.05 M
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Acetic acid, SAJ first grade, ≥99.0%
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Sulfuric acid solution, 5 mM
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Acetic acid, ≥99.7%
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Acetic acid, ≥99.7%
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Diisopropyl ether, JIS special grade, ≥99.0%
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Acetic acid, JIS special grade, ≥99.7%
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Acetic acid, 99.5-100.0%
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Chloroform, SAJ super special grade, ≥99.0%
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Methanol, SAJ first grade, ≥99.5%
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Chloroform, SAJ first grade, ≥99.0%, contains 0.4-0.8% ethanol
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Methanol, JIS 300, ≥99.8%, suitable for residue analysis
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Acetic acid solution, 1 N, 1 M
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Methanol, JIS special grade, ≥99.8%
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Diethyl ether, SAJ first grade, ≥99.0%
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Sulfuric acid solution, 0.025 M
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Chloroform, JIS 300, ≥99.0%
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Sulfuric acid solution, 0.5 M
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Sulfuric acid solution, 1.5 M
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Diethyl ether, ≥99.5%
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Chloroform, JIS special grade, ≥99.0%
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Acetic acid, ≥99.7%, suitable for amino acid analysis
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Diethyl ether, JIS special grade, ≥99.5%
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Sulfuric acid solution, 0.01 M