Multiple headspace solid-phase microextraction of 2-cyclopentyl-cyclopentanone in polyamide 6.6: possibilities and limitations in the headspace analysis of solid hydrogen-bonding matrices

Gröning, Mikael; Hakkarainen, Minna

doi:10.1016/j.chroma.2004.08.112

Cited by 34 publications

(7 citation statements)

References 39 publications

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“…This is true for many solid samples. Examples for such samples that have already been analyzed by MHS-SPME are soil, polyamide, cork stoppers, rosemary extract, sausages, tomatoes, mushrooms, , spices, and ink on paper . The following paragraphs give a detailed picture on the method itself as well as on its development.…”

Section: Introductionmentioning

confidence: 99%

Quantification of Volatiles from Technical Lignins by Multiple Headspace Sampling-Solid-Phase Microextraction-Gas Chromatography-Mass Spectrometry

Guggenberger

Potthast

Rosenau

et al. 2019

ACS Sustainable Chem. Eng.

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Industrial lignins comprise a mixture of substances, including volatile, low-molecular weight compounds. In material applications of lignins, these volatiles contribute to the malodor of the finished product. We developed a method based on solid-phase microextraction-gas chromatography-mass spectrometry (SPME-GC-MS) to assay qualitatively and quantitatively the volatiles emitted from lignin samples. Substances were identified by mass spectra and retention indices, while quantitation was achieved by multiple headspace sampling (MHS). Guaiacol and dimethyl disulfide were calibrated as representative compounds for the most prominent substance classes. The method was validated and gave good recovery, ranging from 89 to 123% for dimethyl disulfide and 90 to 105% for guaiacol, a measurement range of several dozen nanogram to a few micrograms, which can be extended by adjusting the sample amount, and limits of detection of 86 ng for dimethyl disulfide and 25 ng for guaiacol. Sample preparation is limited to weighing of the sample into a headspace vial and requires no consumables or auxiliaries. The entire analytical workflow was automatized, including the necessary data evaluation, which combines the outcome of repeated analyses of the same sample. The concentrations of guaiacol in four representative lignin samples ranged from 0.4 to 1200 ppm, while dimethyl disulfide was detected only in a single sample.

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Section: Introductionmentioning

confidence: 99%

Quantification of Volatiles from Technical Lignins by Multiple Headspace Sampling-Solid-Phase Microextraction-Gas Chromatography-Mass Spectrometry

Guggenberger

Potthast

Rosenau

et al. 2019

ACS Sustainable Chem. Eng.

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“…13 Other potential migrants from PP based packaging are, for example, UV and hindered amine light stabilizers (HALS). 14,15 Common instruments often used for the analysis and detection/identification of migrants from polymers are high-performance liquid chromatography (HPLC) 2,12,16,17 or liquid chro-matographyÀmass spectrometry (LC-MS) 15,20 for semivolatiles and gas chromatographyÀmass spectrometry (GC-MS) 18,19 for volatile substances. The separation of low molecular weight substances from water prior to GC-MS analysis can be achieved by solid phase microextraction (SPME) using multiple headspace extraction (MHE).…”

Section: ' Introductionmentioning

confidence: 99%

Microwave Heating Causes Rapid Degradation of Antioxidants in Polypropylene Packaging, Leading to Greatly Increased Specific Migration to Food Simulants As Shown by ESI-MS and GC-MS

Alin

Hakkarainen

2011

J. Agric. Food Chem.

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100

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Microwave heating of commercial microwavable polypropylene packaging in contact with fatty food simulants caused significant antioxidant degradation and increased specific migration as shown by electrospray ionization-mass spectrometry (ESI-MS) and gas chromatography-mass spectrometry (GC-MS). Degradation of the antioxidants Irgafos 168 and Irganox 1010 was not detected during conventional heating of polypropylene packaging at the same temperature. The migration into aqueous food simulants was primarily restricted by the water solubility of the migrants. Using isooctane as fatty food simulant caused significant swelling and greatly enhanced overall migration values compared to the other fatty food simulant, 99.9% ethanol, or the aqueous food simulants 10% ethanol, 3% acetic acid, or water. ESI-MS spectra clearly reflected the overall migration values, and the number and amount of compounds detected decreased as the hydrophilicity of the food simulant increased. ESI-MS was shown to be an excellent tool for the analysis of semivolatile migrants and a good complement to GC-MS analysis of volatile migrants.

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“…Compounds containing C-13 labeled atoms, aside from cyclopentanone {17}, shown in Tables 1 and 2, originated from the 1,6-hexanediamine portion of the nylon 6.6 backbone; cyclopentanone {17} was expected to form from the adipic acid portion of nylon 6.6 [17,20,31,32] and was also the only compound with an identifiable C-13 label for aged C-13 labeled adipic acid (Scheme 1b). Five compounds containing five-carbon atoms-1-pentene {5}, cyclopentene {8}, 2-pentanone {12}, tetrahydropyran {13}, and pyridine {14}-did not exhibit a significant change in the relative amount of unlabeled to labeled species as aging time increased (Table 2).…”

Section: Degradation Products Containing C-13 Isotopic Labelsmentioning

confidence: 99%

Characterization of Volatile Nylon 6.6 Thermal-Oxidative Degradation Products by Selective Isotopic Labeling and Cryo-GC/MS

Smith

White

et al. 2012

J. Am. Soc. Mass Spectrom.

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Aged materials, such as polymers, can exhibit modifications to their chemical structure and physical properties, which may render the material ineffective for its intended purpose. Isotopic labeling was used to characterize low-molecular weight volatile thermal-oxidative degradation products of nylon 6.6 in an effort to better understand and predict changes in the aged polymer. Headspace gas from aged (up to 243 d at 138°C) nylon 6.6 monomers (adipic acid and 1,6-hexanediamine) and polymer were preconcentrated, separated, and detected using cryofocusing gas chromatography mass spectrometry (cryo-GC/MS). Observations regarding the relative concentrations observed in each chromatographic peak with respect to aging time were used in conjunction with mass spectra for samples aged under ambient air to determine the presence and identity of 18 degradation products. A comparison of the National Institute of Standards and Technology (NIST) library, unlabeled, and isotopically labeled mass spectra (C-13 or N-15) and expected fragmentation pathways of each degradation product were used to identify the location of isotopically labeled atoms within the product's chemical structure, which can later be used to determine the exact origin of the species. In addition, observations for unlabeled nylon 6.6 aged in an O-18 enriched atmosphere were used to determine if the source of oxygen in the applicable degradation products was from the gaseous environment or the polymer. Approximations for relative isotopic ratios of unlabeled to labeled products are reported, where appropriate.

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Multiple headspace solid-phase microextraction of 2-cyclopentyl-cyclopentanone in polyamide 6.6: possibilities and limitations in the headspace analysis of solid hydrogen-bonding matrices

Cited by 34 publications

References 39 publications

Quantification of Volatiles from Technical Lignins by Multiple Headspace Sampling-Solid-Phase Microextraction-Gas Chromatography-Mass Spectrometry

Quantification of Volatiles from Technical Lignins by Multiple Headspace Sampling-Solid-Phase Microextraction-Gas Chromatography-Mass Spectrometry

Microwave Heating Causes Rapid Degradation of Antioxidants in Polypropylene Packaging, Leading to Greatly Increased Specific Migration to Food Simulants As Shown by ESI-MS and GC-MS

Characterization of Volatile Nylon 6.6 Thermal-Oxidative Degradation Products by Selective Isotopic Labeling and Cryo-GC/MS

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