• Mass Spectrometry Letters
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• v.9 no.3
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• pp.77-80
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• 2018

The focus of this paper is to present techniques to overcome certain difficulties in quantitative analysis with a time-of-flight mass spectrometer (TOF-MS). The method is based on conventional solid-phase extraction, followed by reversed-phase ultra high performance liquid chromatography of the extract, and mass spectrometric analysis. The target compounds included atenolol, atrazine, caffeine, carbamazepine, diclofenac, estrone, ibuprofen, naproxen, simazine, sucralose, sulfamethoxazole, and triclosan. The matrix effects caused by high concentrations of organic compounds in wastewater are especially significant in electrospray ionization mass spectroscopy. Internal-standard calibration with isotopically labeled standards corrects the results for many matrix effects, but some peculiarities were observed. The problems encountered in quantitation of carbamazepine and triclosan, due to nonlinear calibration were solved by changing the internal standard and using a narrower mass window. With simazine, the use of a quadratic calibration curve was the best solution.

• Bulletin of the Korean Chemical Society
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• v.18 no.2
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• pp.171-174
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• 1997

The initial kinetic energy of laser-ablated Zn cation has been investigated via time-of-flight mass spectrometry. The flight times of the ions have been measured with a high voltage pulse on the extract electrode in the mass spectrometer, which has been delayed from the laser pulse. The time-of-flight equation including the initial kinetic energy term of the ion has been derived for the mass spectrometer. The optimum value of the initial kinetic energy has been extracted by fitting the measured flight times into the time-of-flight equation. The initial kinetic energy of the ions generated by Nd:YAG laser (532 nm) at the power density of 5 × 107 W/cm2 has been determined to be 22-44 kJ/mol.

• Bulletin of the Korean Chemical Society
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• v.31 no.10
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• pp.2791-2796
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• 2010

In the present study, we constructed a membrane inlet assembly for selective permeation of volatile airborne organic compounds for subsequent analysis by time-of-flight mass spectrometry. The time-dependent diffusion of analytes through a $75\;{\mu}m$ thick polydimethylsiloxane membrane was measured by monitoring the ion signal after a step change in the sample concentration. The results fit well to a non-steady-state permeation equation. The diffusion coefficient, response time, and sensitivity were determined experimentally for a range of polar (halogenated) and nonpolar (aromatic) compounds. We found that the response times for several volatile organic compounds were greatly influenced by the alkyl chain length as well as the size of the substituted halogen atoms. The detection limits for benzene, ethylbenzene, and 2-propanol were 0.2 ppm, 0.1 ppm, and 3.0 ppm by volume, respectively, with a linear dynamic range greater than three orders of magnitude. These results indicate that the membrane inlet/time-of-flight mass spectrometry technique will be useful for a wide range of applications, particularly for in situ environmental monitoring.

• Bulletin of the Korean Chemical Society
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• v.25 no.1
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• pp.101-105
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• 2004

The laser ablation/ionization time-of-flight mass spectrometry is applied to the isotopic analysis of solid samples using a home-made instrument. The technique is convenient for solid sample analysis due to the onestep process of vaporization and ionization of the samples. The analyzed samples were lead, cadmium, molybdenum, and ytterbium. To optimize the analytical conditions of the technique, several parameters, such as laser energy, laser wavelength, size of the laser beam on the samples surface, and high voltages applied on the ion source electrodes were varied. Low energy of laser light was necessary to obtain the optimal mass resolution of spectra. The 532 nm light generated mass spectra with the higher signal-to-noise ratio compared with the 355 nm light. The best mass resolution obtained in the present study is ~1,500 for the ytterbium.

• Mass Spectrometry Letters
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• v.15 no.1
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• pp.26-39
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• 2024

Gold nanostructures (Au NSs) are useful and interesting matrices for mass spectrometric analysis of various biomolecules based on organic matrix-free laser desorption/ionization time-of-flight mass spectrometry (LDI-TOF-MS). Au NSs provide high efficiency and versatility in LDI-TOF-MS analysis based on their well-established synthesis and surface functionalization, large surface area, high laser absorption capacity, and photothermal conversion efficiency. Therefore, Au NSs based LDI-TOF-MS can be a facile, functional, and efficient analytical method for important small biomolecules owing to its simple preparation, rapid analysis, salt-tolerance, signal reproducibility, and quantitative analysis. This review chronologically summarizes the important advance of Au NSs-based LDI-TOF-MS platforms in terms of in-depth mechanism, signal enhancement, quantitative analysis, and disease diagnosis.

• Analytical Science and Technology
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• v.8 no.4
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• pp.715-722
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• 1995

The structural characterization for series of polyesters has been done by time-of-flight secondary ion mass spectrometry (TOF-SIMS). Polymer fragments and intact oligomers composed of large numbers of repeat units have been investigated. Transesterification of polyesters in trifluoroacetic acid (TFA) and chlorodifluoroacetic acid (CFA) was monitored and reaction products were identified using TOF-SIMS. The shapes and intensities of clusters in transesterification spectra show good agreement with the theoretical isotope pattern. TOF-SIMS spectra were used to obtain information about the progress of the transesterification reaction.

• Mass Spectrometry Letters
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• v.12 no.1
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• pp.26-30
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• 2021

The impurity concentration is a crucial parameter for semiconductor thin films. Evaluating the impurity distribution in silicon thin film is another challenge. In this study, we have investigated the doping concentration of boron in silicon thin film using time of flight secondary ion mass spectrometry in dynamic mode of operation. Boron doped silicon film was grown on i) p-type silicon wafer and ii) borosilicate glass using hot wire chemical vapor deposition technique for possible applications in optoelectronic devices. Using well-tuned SIMS measurement recipe, we have detected the boron counts 101~104 along with the silicon matrix element. The secondary ion beam sputtering area, sputtering duration and mass analyser analysing duration were used as key variables for the tuning of the recipe. The quantitative analysis of counts to concentration conversion was done following standard relative sensitivity factor. The concentration of boron in silicon was determined 1017~1021 atoms/㎤. The technique will be useful for evaluating distributions of various dopants (arsenic, phosphorous, bismuth etc.) in silicon thin film efficiently.

• Proceedings of the SCSK Conference
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• 2003.09b
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• pp.480-507
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• 2003

A rapid and efficient method for analyzing the nonionic surfactants and silicone polymers, which control the shape and characteristics of cosmetic products and give influence on product quality, has been developed using Matrix-Assisted Laser Desorption Ionization Time of Flight Mass Spectrometry (MALDI- TOF IMS). The MALDI-TOF/MS could easily and effectively determine the molecular weight distribution and monomer units of nonionic surfactants. As a result, creating a library of mass spectrum data of surfactants used in cosmetic products using MALDI-TOF/MS and analyzing surfactants extracted from the products may become a useful method for detailed structural characterization of the surfactants. Furthermore, the MALDI-TOF/MS analysis was effective in obtaining the spectrum of silicone polymers from which the molecular weight distribution could be determined. The repetition units and structural data could also be obtained through molecular mass peaks. Additionally, the monomer ratio and terminal groups as properties of silicone copolymers could be determined

• Food Science of Animal Resources
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• v.44 no.3
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• pp.651-661
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• 2024

Chicken broth has a taste of umami, and the stewing time has an important effect on the quality of chicken broth, but there are fewer studies on the control of the stewing time. Based on this, the study was conducted to analyze the effects of different stewing times on the sensory, small molecular metabolites, free fatty acids, and volatile flavor compounds contents in chicken broths by liquid chromatography-quadrupole/time-of-flight mass spectrometry, gas chromatography-mass spectrometry, headspace solid-phase microextraction, and gas chromatography-mass spectrometry. Eighty-nine small molecular metabolites, 15 free fatty acids, and 86 volatile flavor compounds were detected. Palmitic and stearic acids were the more abundant fatty acids, and aldehydes were the main volatile flavor compounds. The study found that chicken broth had the best sensory evaluation, the highest content of taste components, and the richest content of volatile flavor components when the stewing time was 2.5 h. This study investigated the effect of stewing time on the quality of chicken broth to provide scientific and theoretical guidance for developing and utilizing local chicken.

• Mass Spectrometry Letters
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• v.5 no.1
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• pp.24-29
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• 2014

An advanced and reliable high performance liquid chromatography (HPLC)/ultraviolet detector (UV)/ion-trap time-of-flight (IT-TOF) mass spectrometry was developed for the simultaneous quantification of 19 marker compounds in Bang-poong-tong-sung-san (BPTS), a traditional oriental prescription. Various parameters affecting HPLC separation and IT-TOF detection were investigated, and optimized conditions were identified. The separation was achieved on a Capcell PAK C18 column ($1.5mm{\times}250mm$, $5{\mu}m$ particle size) using a gradient elution of acetonitrile and water containing 0.1% formic acid at a flow rate of 0.1 mL/min. The column temperature was maintained at $40^{\circ}C$ and the injection volume was $2{\mu}L$. IT-TOF system was equipped with an electrospray ion source (ESI) operating in positive or negative ion mode. The optimized electrospray ionization parameters were as follows: ion spray voltage, +4.5 kV (positive ion mode), or -3.5 kV (negative ion mode); drying gas ($N_2$), 1.5 L/min; heat block temperature, $200^{\circ}C$. Automatic $MS^n$ (n = 1~3) analyses were carried out to obtain structural information of analytes. Elemental compositions and their mass errors were calculated based on their accurate masses obtained from a formula predictor software. The marker compounds in BPTS were identified by comparisons between $MS^n$ spectra from standards and those from extracts. Moreover, the libraries of $MS^2$ and $MS^3$ spectra and accurate masses of parent and fragment ions for marker compounds were constructed. The developed method was successfully applied to the BPTS extracts and identified 17 out of 19 marker compounds in the BPTS extracts.