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GC-TOFMS Application: Natural Polymer Analysis by using Pyrolysis-GCxGC-MS - "Urushi" analysis with GCxGC/EI and GCxGC/PI

A Japanese lacquer film called "Urushi" is a natural polymer that has been used as a paint and adhesive for living-wares and craft-wares for approximately 8,000 years. "Urushi" has a complex structure that researchers are trying to understand using pyrolysis-gas chromatograph/mass spectrometer (Py/GC/MS) system. Recently, we developed a new gas chromatograph/high resolution time-of-flight mass spectrometer (GC/HR-TOFMS) system that can be used for comprehensive two-dimensional GC (GCxGC) measurements. Additionally, we have developed a unique combination electron ionization/photoionization (EI/PI) ion source that can be used with this GC/HR-TOFMS system. In this work, we measured "Urushi" samples using this unique Py/GCxGC/HR-TOFMS system in combination with our new combination EI/PI ion source.

Features and Applications of Newly-Developed GC-TOFMS “The AccuTOF GC”

A gas-chromatograph mass spectrometer (GC-MS) is a combined analyzer that has superior ability in analyzing organic compounds qualitatively and quantitatively. The first part, gas chromatograph, separates the compounds included in a sample (mixture), then the second part, mass spectrometer, obtains mass spectra of the compounds to carry out qualitative analysis. Quantitative analysis can be carried out as well from the peak area of the mass chromatogram of the compound. As a mass spectrometer of a GC-MS system, several types of mass spectrometers are on the market, such as magnetic field, quadrupole (QMS), ion trap (ITD), and time-of-flight (TOF). Each mass spectrometer has its own features and applications.

Visualizing fragmentation channels of polyethylene oxide with different end groups using the JMS-S3000 SpiralTOFTM with TOF–TOF option

Tandem mass spectrometry is a powerful tool for polymer characterization. It can obtain information about polymer end groups, repeating structures (linear, cyclic, or branched), and copolymerization. High-energy collision–induced dissociation (HE-CID) is a fragmentation method that is available only in tandem time-of-flight mass spectrometry (TOF–TOF). The informative fragmentation channels, which are difficult to observe with commonly used low-energy CID, are often observable in HE-CID spectra. In MSTips 270, we proposed a method to visualize this abundant structural information and enable intuitive analysis using the “Remainders of KM” (RKM) plot method. In this report, we applied the method to analyze polyethylene oxide (PEO) with different end groups.

Synthetic Polymer Structure Analysis: Poly Methal Methacrylate (PMMA)

The JMS-S3000 “SpiralTOF™” is a MALDI-TOFMS that incorporates an innovative SpiralTOF ion optics system. This system is available with a TOF-TOF option that can acquire high-energy collision-induced dissociation (CID) product ion spectra for monoisotopically selected precursor ions. In this work, we analyzed Poly Methyl Methacrylate (PMMA) shown in Fig. 1 by using the JMS-S3000 SpiralTOF with the TOF-TOF option. The resulting high-energy CID data was then processed using the Polymerix™ (Sierra Analytics, Inc., http://massspec. com/) analysis software.

Structure analysis of a polymer additive using high-energy collision–induced dissociation mass spectra acquired by SpiralTOFTM/TOF

Various kinds of additives are used in a polymer, such as an antioxidant, a light stabilizer, and an ultraviolet absorber. Because a polymer’s properties depend on the additives in the raw material, it is important to understand these additives. Matrix-assistance laser desorption/ ionization time-of-flight mass spectrometer (MALDI-TOFMS) JMS-S3000 SpiralTOF™ is widely used in polymer analysis. High-energy collision–induced dissociation (HE-CID) measurement with the TOF-TOF option is also useful in analyzing the structures of additives. SpiralTOF™ can achieve a high precursor ion selection with a revolution of 17 m. Fragmentation derived from HE-CID can be observed only due to the ions from post-source decay (PSD), these fragment ions can be eliminated by the four electrostatic sectors that constitute the spiral trajectory. In this Applications Note, we report on polymer structural analysis by compare fragmentation patterns in the product ion spectra of IRGANOX 1076 M+・ and [M+Na]+.

Structural Analysis of Tristearin

The JMS-S3000 SpiralTOF™ is a MALDI-TOF MS that uses an innovative spiral ion optical system to achieve the highest resolution currently available for a MALDI instrument. Additionally, this system can be equipped with a TOF-TOF option that can acquire high-energy collisioninduced dissociation (HE-CID) product ion spectra for monoisotopically selected precursor ions. The resulting HE-CID product ion spectra provide detailed structural information about compounds like triglycerides by means of charge-remote fragmentation (CRF).1 Tristearin is a triglyceride found in fats that consists of three stearic acid moieties (Fig. 1). In this work, we report the structural analysis of tristearin by using the HE-CID capabilities of the SpiralTOF-TOF.

Structural Analysis of Triolein

The JMS-S3000 “SpiralTOF™” is a MALDI-TOF MS that uses an innovative spiral ion optical system to achieve the highest resolution currently available for a MALDI instrument. Additionally, this system can be equipped with a TOF-TOF option that can acquire high-energy collisioninduced dissociation (HE-CID) product ion spectra for monoisotopically selected precursor ions. The resulting HE-CID product ion spectra provide detailed structural information about compounds like triglycerides by means of charge-remote fragmentation (CRF). In this work, we report the structural analysis of triolein, a triglyceride that contains 3 oleic acid moieties (Fig. 1), by using HE-CID capabilities of the SpiralTOF-TOF.

Structural Analysis of Oxidized Triolein

In previous work, we showed that the JEOL SpiralTOFTOF system’s high-energy collision-induced dissociation (HE-CID) is useful for the structural analysis of triglycerides. The resulting HE-CID mass spectra provided detailed information about the fatty acid moieties such as the positions of double bonds, branching, hydroxylation, and oxidation by means of charge-remote fragmentation (CRF). In this work, we report the structural analysis of oxidized triglycerides by HE-CID using the SpiralTOFTOF.

Structural analysis of melatonin and related compounds using JMS-S3000 SpiralTOFTM with the TOF-TOF option

The JMS-S3000 SpiralTOF™, which has a JEOL-patented spiral orbital ion optical system, has a long-flight distance of 17 m and can achieve high-mass resolution. In addition, the electrostatic sectors that constitute the ion optical system can exclude PSD ions, making it possible to acquire a mass spectrum that is less affected by background ions. These features enable accurate mass measurement even in LMW regions[1].

Structural Analysis of a High Molecular Weight Peptide

The JMS-S3000 SpiralTOF™ is a MALDI-TOF MS that uses an innovative spiral ion optics system to achieve the highest resolution currently available for a MALDI instrument. Additionally, the JMS-S3000 is available with a TOF-TOF option that acquires high-energy collision-induced dissociation (CID) product-ion spectra for monoisotopically selected precursor ions. In this work, we analyzed a high molecular weight peptide by using the JMS-S3000 SpiralTOF with the TOF-TOF option.

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