Composition and distribution of NSO compounds in two different shales at the early maturity stage characterized by negative ion electrospray ionization coupled with Fourier transform ion cyclotron resonance mass spectrometry

Gas chromatography/mass spectrometry （GC/MS） can only analyze volatile molecular compounds, and it has limitations when applied to determine the complex components of crude oils and hydrocarbon source rocks. Based on Fourier transform ion cyclotron resonance mass spectrometry （FT-ICR-MS） and GC/MS analyses, the molecular compositions of NSO compounds in extracts from the Permian Dalong Formation, Sichuan Basin and the Permian Lucaogou Formation, Junggar Basin in China were compared. Analyses of types of heteroatoms present （S~, $2, $3, OS, OS2, 02S, NS, and NOS compounds） suggest that marine shales from the Dalong Formation are mainly composed of carboxylic acids （02 com- pounds） with a high abundance of fatty acids, indicating a marine phytoplankton organic source. However, lacustrine shales from the Lucaogou Formation are dominated by pyrrolic compounds （N1 compounds） with abundant dibenzocar- bazole. It suggests that the organic source materials may be derived from lower aquatic organisms and lacustrine algae. Overall, FT-ICR-MS has potential for applications in analyses and determination of depositional environments and organic sources in petroleum geology.

Advanced molecular-fingerprinting analysis of dissolved organic sulfur by electrospray ionization-Fourier transform ion cyclotron resonance mass spectrometry using optimal spray solvent

Molecular level characterization of dissolved organic sulfur(DOS)by electrospray ionizationFourier transform ion cyclotron resonance mass spectrometry(ESI-FTICR MS)is necessary for further understanding of the role of DOS in the environment.Here,ESI spray solvent,a key parameter for ion production during ESI process,was investigated for its effect on the molecular characterization of DOS by ESI-FTICR MS.100%MeOH as spray solvent was found for the first time to remarkably enhance the ionization efficiency of the majority of CHOS-molecules in NOM,which facilitated a total of 1473 CHOS-molecular formulas with one sulfur atom to be detected.The number of CHOS-molecular formulas obtained using 100%MeOH as spray solvent increased notably over 740 in comparison with those using 50%MeOH aqueous solution(731)or 50%ACN aqueous solution(653).Moreover,due to the enhancement of ionization efficiency of DOS during ESI processes,the tandem mass spectra of the NOM CHOS-molecules could be easily obtained using 100%MeOH as spray solvent,which were hardly obtained using 50%MeOH aqueous solution as spray solvent.The results of the tandem mass spectra suggested the first discovery of organosulfates or sulfonic acids in Suwannee River NOM sample.A simple method based on 100%MeOH as ESI spray solvent for advanced molecular characterization of DOS by ESI-FTICR MS was proposed and applied,and the results revealed more molecular information of DOS in sea DOM samples.

Combination of Solid-Phase Micro-Extraction and Direct Analysis in Real Time-Fourier Transform Ion Cyclotron Resonance Mass Spectrometry for Sensitive and Rapid Analysis of 15 Phthalate Plasticizers in Beverages

A method for rapid identification and quantification of phthalate plasticizers in beverages was developed.A number of 15 phthalate plasticizers which covered all the phthalates concerned in the US Consumer Product Safety Improvement Act(CPSIA),European Union legislations and Chinese national standards(GB)were analyzed.By a combined solid-phase micro-extraction(SPME)and direct analysis in real time mass spectrometry(DART-MS)approach,phthalates at sub-ng•mL^(−1)levels can be qualitatively and quantitatively analyzed in a short time.The use of ultrahigh-resolving power and the accurate mass measurement capacity naturally provided by Fourier transform ion cyclotron resonance mass spectrometry(FT-ICR-MS)minimizes the matrix interferences and thus enables the evaluation of phthalates in a complex matrix without extensive sample handlings or preparations.The limits of quantification(LOQs)were estimated to be at 0.3-5.0 ng•mL^(−1),lower than the Maximum Residue Limit(MRL)regulated by the European Union legislations(2007/19/EC)in foods,beverages,food packaging and toys(0.3-30 ng•mL^(−1)).This rapid and easy-to-use SPME-DART-FT-ICR-MS method provided a relatively high-throughput and powerful analytical approach for quick testing and screening phthalates in beverages and water samples to ensure food safety.

Studies on Fragmentation of Peptide by Nano-electrospray Ionization Fourier Transform Ion Cyclotron Resonance Multi-stage Tandem Mass Spectrometry

The sequence analysis of peptides was performed by nano-electrospray ionization Fourier transform ion cyclotron resonance tandem mass spectrometry（Nano-ESI-FT-ICR-MSn） and several peptides were chosen as examples. With the aid of the collision induced dissociation（CID）, FT-ICR provides not only precise mass/charge ratio, but also structure information of the selected peptides. The fragment ions were identified according to the observed molecular weights and peptide sequence was determined successfully. So Nano-ESI-FT-ICR-MSn is a useful tool for identification of the amino acid sequence of peptides with high confidence. Besides, a pathway for the dehydration of y ions without amino acids containing carboxylic acid under sustained off-resonance irradiation collision-induced dissociation（SORI-CID） condition was proposed.

Measurement of niobium reaction rate for material surveillance tests in fast reactors

A highly accurate and precise technique for measurement of the 93 Nb(n,n’)93m Nb reaction rate was established for the material surveillance tests,etc.in fast reactors.The self-absorption effect on the measurement of the characteristic X-rays emitted by 93m Nb was decreased by the dissolution and evaporation to dryness of niobium dosimeter.A highly precise count of the number of 93 Nb atoms was obtained by measuring the niobium solution concentration using inductively coupled plasma mass spectrometry.X-rays of 93m Nb were measured accurately by means of comparing the X-ray intensity of irradiated niobium solution with that of the solution in which stable 93 Nb was added.The difference between both intensities indicates the effect of 182 Ta,which is generated from an impurity tantalum,and the intensity of X-rays from 93m Nb was evaluated.Measurement error of the 93 Nb(n,n’)93m Nb reaction rate was reduced to be less than 4%,which was equivalent to the other reaction rate errors of dosimeters used for Joyo dosimetry.In addition,an advanced technique using Resonance Ionization Mass Spectrometry was proposed for the precise measurement of 93m Nb yield,and 93m Nb will be resonance-ionized selectively by discriminating the hyperfine splitting of the atomic energy levels between 93 Nb and 93m Nb at high resolution.