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The simultaneous LC/MS analyses of hexachlorobenzene (HCB) and pentachlorophenol (PCP), two dioxin precursors were studied by both atmospheric pressure chemical ionization (APCI) and atmospheric pressure photoionization mass spectrometry (APPI/MS). The optimum LC/MS conditions of the simultaneous analysis were determined for these two compounds with different polarity. Ionization by APPI was found to be more effective than by APCI, and is thus a better ionization method for analysis of the two compounds. Using LC/APPI/MS we can achieve the simultaneous analysis of HCB and PCP at ppb levels.

The effects of an on-line ion suppressor device on alkali metal ion adduct formations of the model compound tacrolimus were investigated. The base peak ion in the positive ion ESI-MS spectrum of tacrolimus was a sodium ion adduct, [M+Na]+. On the other hand, an ammonium ion adduct, [M+NH4]+, was the base peak ion in the full-scan mass spectrum of tacrolimus with a cation-exchange suppressor resin, and both [M+Na]+ and [M+K]+ were eliminated. These results indicate that the combination of an on-line ion suppressor with ESI-MS is a simple and effective technique that eliminates undesirable alkali metal ion adduct formations in the positive-ion mode.

The applicability of matrix-free surface-assisted laser desorption/ionization mass spectrometry using porous silicon (DIOS-MS) and TiO2 nanoparticles (TiO2-SALDI-MS) was examined by analyzing an antioxidant added to insoluble polypropylene (PP) materials. The optimized solvent extraction, which involved freezing and crushing the PP, results in a good recovery, 89±4 and 97±8% for 0.5 wt% of the added antioxidant, tetrakis[methylene3-(3,5-di-t-butyl-4-hydroxyphenyl)propionate]methane (commercial name; Irganox1010) in laboratory-produced and commercial PP composites, respectively. The positive ion measurements in DIOS and TiO2-SALDI-MS yielded sodium adduct ions without any interference from other signals. Using an internal standard with a similar structure, a good calibration curve linearity was established in the Irganox1010 concentration range of 0.01-2.0 mg/mL in PP, which was sufficient for monitoring the plastic additives. However, TiO2-SALDI-MS was superior to DIOS-MS in terms of mass resolution and easiness of sample preparation. A solvent extraction method followed by TiO2-SALDI-MS appears to be a anticipated method for the analysis of additives in insoluble plastics.

identifier:https://dspace.jaist.ac.jp/dspace/handle/10119/10611

This paper reports a study on the formation mechanism of nanoparticles (NPs) composed of bismuth, antimony and tellurium for thermoelectric materials using a modified polyol synthetic route. Our one-pot synthesis technique has proven highly versatile in creating a wide range of different anisotropic NPs such as nanowires (NWs), nanodiscs (NDs), nanoribbons and nanospines (NDs studded on NWs) simply by modifying the capping species or elemental precursor feeding ratio used in the synthesis. However, an independent control of morphology and composition is still hugely challenging and the facile synthesis of (Bi,Sb)_2Te_3 solid solution NPs is not a trivial task, reflecting the complex nature of this multicomponent system. To achieve this goal, it is imperative to understand the formation mechanism based on a systematic investigation of mono- and binary elemental NP systems. Our study clearly shows the different actions of oleylamine (OAM) and decanethiol (DT) capping ligands in our synthesis reaction. In the case of DT capping system, Te NDs are first formed, and then, Bi and Sb are separately incorporated into the Te ND structure via catalytic decomposition of Bi-DT and Sb-DT complexes on the Te ND surfaces. Therefore, the resulting NPs are phase segregated into Te, Bi_2Te_3 and Sb_2Te_3. On the other hand, in the case of the OAM capping system, Te NWs and Bi-Sb solid solution NPs are formed separately, and then, parts of Te NWs are transformed into (Bi,Sb)_2Te_3 phase via oriented attachment of Bi-Sb NPs and Te NWs. These findings are crucially important towards the one-pot synthesis of uniform (Bi,Sb)_2Te_3 nanobuilding blocks with controllable characteristics for highly efficient thermoelectric materials., identifier:https://dspace.jaist.ac.jp/dspace/handle/10119/10737

We analysed the bioactive compounds in Panax ginseng C.A. Meyer by using nanoparticle-assisted laser desorption/ionisation (nano-PALDI) mass spectrometry (MS). To this end, we prepared manganese oxide nanoparticles (d = 5.4 nm) and developed a nano-PALDI MS method to analyse the standard ginsenosides and identify these ginsenosides in an extract of P. ginseng. The nanoparticles served as an ionisation-assisting reagent in MS. The mass spectra did not show any background interference in the low-m/z range. Our pilot study showed that the nanoparticles could ionise the standard ginsenosides and also respective lipid and ginsenosides in the extract without the aid of chemical and liquid matrices used in conventional MS methods. Analysis of the post-source decay spectra obtained using nano-PALDI MS will yield information regarding the chemical structure of the analyte., identifier:https://dspace.jaist.ac.jp/dspace/handle/10119/9049

The applicability of matrix-free surface-assisted laser desorption/ionization mass spectrometry using porous silicon (DIOS-MS) and TiO2 nanoparticles (TiO2-SALDI-MS) was examined by analyzing an antioxidant added to insoluble polypropylene (PP) materials. The optimized solvent extraction, which involved freezing and crushing the PP, results in a good recovery, 89±4 and 97±8% for 0.5 wt% of the added antioxidant, tetrakis[methylene3-(3,5-di-t-butyl-4-hydroxyphenyl)propionate]methane (commercial name; Irganox1010) in laboratory-produced and commercial PP composites, respectively. The positive ion measurements in DIOS and TiO2-SALDI-MS yielded sodium adduct ions without any interference from other signals. Using an internal standard with a similar structure, a good calibration curve linearity was established in the Irganox1010 concentration range of 0.01-2.0 mg/mL in PP, which was sufficient for monitoring the plastic additives. However, TiO2-SALDI-MS was superior to DIOS-MS in terms of mass resolution and easiness of sample preparation. A solvent extraction method followed by TiO2-SALDI-MS appears to be a anticipated method for the analysis of additives in insoluble plastics.