Quantitative determination of poly(vinylpyrrolidone) by continuous-flow off-line pyrolysis-GC/MS

Antić, Vesna; Antić, Mališa; Kronimus, Alexander; Oing, Katja; Schwarzbauer, Jan

doi:10.1016/j.jaap.2010.10.011

Cited by 47 publications

(29 citation statements)

References 18 publications

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“…This conclusion is directionally consistent with prior thermal studies reporting corresponding activation energies, frequency factors, and reaction orders of the two thermal reaction pathways . Antić et al previously demonstrated a methodology for the quantitation of PVP in water samples using off‐line pyrolysis and subsequent GC‐FID analysis of the NVP decomposition product . This technique was adapted for the analysis of solid lens material; the methodology was described previously .…”

Section: Resultsmentioning

confidence: 99%

“…The reaction sequence results in the formation of a highly oxygen transmissible, low bulk modulus silicone matrix with a distinct PVP phase that drives water content and surface wettability. The molecular formula of the resulting polymer matrix is [C 16 13 The material was analyzed at various cure times to confirm two-phase polymerization and achieve the targeted physical properties. Nominal lens properties include 46% water content, 70 g/mm 2 modulus, and 163 Barrer oxygen transmissibility (Dk/t).…”

Section: Dual-phase Synthesis Of Samfilcon Amentioning

confidence: 99%

“…Extracted PVP was quantified by a gas phase pyrolysis technique using high temperature APCI on an LTQ Orbitrap XL mass spectrometer (Thermo Scientific), 15 while bulk PVP content in finished lenses was quantified by an off-line tube-furnace pyrolysis technique. 16,17 In pyrolysis, heating causes polymeric PVP in the sample to decompose and revert back to its monomeric NVP form ( Figure 1). The tube furnace approach, despite its low sample throughput, overcomes sample preparation issues and limits technical concerns observed using other pyrolysis techniques.…”

Section: Quantitation Of Pvp In Lenses and Lens Extractsmentioning

confidence: 99%

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Characterization and quantitation of PVP content in a silicone hydrogel contact lens produced by dual‐phase polymerization processing

Hoteling¹,

Nichols²,

Harmon³

et al. 2017

J Biomed Mater Res

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Polyvinylpyrrolidone (PVP) has been incorporated over the years into numerous hydrogel contact lenses as both a primary matrix component and an internal wetting agent to increase lens wettability. In this study, complementary analytical techniques were used to characterize the PVP wetting agent component of senofilcon A and samfilcon A contact lenses, both in terms of chemical composition and amount present. Photo-differential scanning calorimetry (photo-DSC), gas chromatography with a flame ionization detector (GC-FID), and high-resolution/accurate mass (HR/AM) liquid chromatography-mass spectrometry (LC-MS) techniques confirmed dual phase reaction and curing of the samfilcon A silicone hydrogel material. Gel permeation chromatography (GPC) demonstrated that high molecular weight (HMW) polymer was present in isopropanol (IPA) extracts of both lenses. High-performance liquid chromatography (HPLC) effectively separated hydrophilic PVP from the hydrophobic silicone polymers present in the extracts. Collectively, atmospheric solids analysis probe mass spectrometry (ASAP MS), Fourier transform infrared (FTIR) spectroscopy, H nuclear magnetic resonance (NMR) spectroscopy, GC-FID, and LC-MS analyses of the lens extracts indicated that the majority of NVP is consumed during the second reaction phase of samfilcon A lens polymerization and exists as HMW PVP, similar to the PVP present in senofilcon A. GC-FID analysis of pyrolyzed samfilcon A and senofilcon A indicates fourfold greater PVP in samfilcon A compared with senofilcon A. © 2017 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 106B: 1064-1072, 2018.

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Section: Resultsmentioning

confidence: 99%

Section: Dual-phase Synthesis Of Samfilcon Amentioning

confidence: 99%

Section: Quantitation Of Pvp In Lenses and Lens Extractsmentioning

confidence: 99%

See 1 more Smart Citation

Characterization and quantitation of PVP content in a silicone hydrogel contact lens produced by dual‐phase polymerization processing

Hoteling¹,

Nichols²,

Harmon³

et al. 2017

J Biomed Mater Res

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“…U novijem radu Antić i saradnika razvijena je efikasna analitička metoda za kvantitativno određivanje PVP u otpadnim i rečnim vodama, bazirana na "off-line" pirolizi kuplovanoj sa GC i GC-MS [12].…”

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“…U ovom radu primenjena je "on-line" piroliza u sprezi sa GC i GC-MS, za detekciju i kvantitativno određivanje PVP u otpadnoj vodi. Poznato je i potvrđeno da se PVP može detektovati u otpadnim vodama [12], zahvaljujući veoma intenzivnoj primeni i dokazanoj stabilnosti u životnoj sredini [13]. Kvantitativno određivanje PVP je izvršeno primenom GC-FID metode, na bazi glavnog proizvoda pirolize, NVP.…”

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Quantitative determination of poly(vinylpyrrolidone) by "on-line" pyrolysis coupled to gas chromatography

Antić¹,

Antić²,

Kronimus

et al. 2012

Hem Ind

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"On-line" pyrolysis coupled with gas chromatography (GC) was performed for quantitative determination of poly(vinylpyrrolidone) (PVP) in wastewater sample. Gas chromatography-mass spectrometry (GC-MS) showed that the main product of pyrolysis of PVP, at high temperatures, is N-vinylpyrrolidone (NVP). After that, different amounts of commercial PVP were pyrolyzed in order to establish correlation between the amount of generated NVP (its GC peak area) and the initial mass of pyrolyzed PVP. GC-FID analysis was used for construction of calibration curve and for quantitative determination of PVP. Very good linear correlation was obtained between the area of NVP peak, generated during pyrolysis, and the initial mass of PVP (r2 = 0.998). Further, solutions of known concentration of PVP were prepared in destilled water ("spiked samples"). Spiked samples were preextracted with diethyl ether and n-hexane, and after that, the water-layer was evaporated and dissolved again in methanol. Analysis of pyrolysates of preextracted spiked samples showed that the "recovery" of PVP was above 96 mas%. This finding suggested that pre-extraction could be applied to reduce the concentration of organic substances that could also be pyrolyzed, and thus hinder identification and quantitative determination of PVP, without significant loss of polymer. The sample of an industrial wastewater from Pančevo, Serbia was investigated in the last part of this work. The sample was preextracted in the same way as the spiked samples and than pyrolyzed. NVP was identified by GC-MS in obtained pyrolysate, which was the evidence that PVP was present in the wastewater sample. NVP was quantified on the basis of the peak area in GC-FID chromatogram, and than the concentration of PVP in wastewater sample was calculated based on calibration curve. Concentration of PVP in industrial wastewater amounted 2.5 mg/L

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Role of Mass Spectrometry in the Elucidation of Thermal Degradation Mechanisms in Polymeric Materials

Rizzarelli¹,

Carroccio²

2015

Reactions and Mechanisms in Thermal Analysis of Advanced Materials

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Quantitative determination of poly(vinylpyrrolidone) by continuous-flow off-line pyrolysis-GC/MS

Cited by 47 publications

References 18 publications

Characterization and quantitation of PVP content in a silicone hydrogel contact lens produced by dual‐phase polymerization processing

Characterization and quantitation of PVP content in a silicone hydrogel contact lens produced by dual‐phase polymerization processing

Quantitative determination of poly(vinylpyrrolidone) by "on-line" pyrolysis coupled to gas chromatography

Role of Mass Spectrometry in the Elucidation of Thermal Degradation Mechanisms in Polymeric Materials

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