• Analytical Science and Technology
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• v.36 no.1
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• pp.22-31
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• 2023

As the use of e-liquid cigarettes is rapidly increasing worldwide, it multiplies the potential risk undisclosed to the health of non- and smokers. To reduce the hazard, each country has its own set of regulations for controlling e-liquids. In Korea, the narrow definition of tobacco makes it difficult and have been steadily occurring tax evasion exploiting the difference in natural and artificial nicotine. Therefore, it is very important to distinguish source of nicotine for their regulation. To find biochemical discriminant markers, this study established analysis methods based on high-performance liquid chromatography coupled with diode array detector (HPLC-DAD) and high-performance liquid chromatography coupled with triple Quadrupole mass spectrometry (HPLC-MS/MS) for nicotine enantiomers and tobacco alkaloids targeted using the difference in pathways of nicotine biosynthesis and chemical synthesis. The method was validated by experimenting linearity (R² > 0.999), recovery (80.99-108.41 %), accuracy (94.11-109.73 %) and precision (0.04-8.27 %). Then, the results for discrimination of the nicotine obtained from analysis of 65 commercial e-liquid products available in Korean market was evaluated. The method successfully applied to the e-liquids and one sample labelled 'synthetic nicotine' for tax exemption was found to contain a natural nicotine product. This method can be used to determine whether an e-liquid product uses natural or artificial nicotine and monitor non-taxable e-liquid products. The method is more scientific than the existing one, which relies only on field evidence.

• Journal of Korean Society on Water Environment
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• v.21 no.6
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• pp.549-563
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• 2005

The study was carried out to develop and standardize the analytical method of 1,4-dioxane in water. The National Institute of Environmental Research in Korea has monitored for 1,4-dioxane in water since 1998 and it has been detected in environmental water occasionally. But the environmental pollution and analytical method in water is not well known over the world. The trace analytical method at low-${\mu}/L$ level is prerequisite in order to evaluate the residue of 1,4-dioxane in water. Evaluation of the method was demonstrated by comparing and analyzing with liquid-liquid extraction, solid-phase extraction and purge & trap technique. As a result of experiment by standard solutions and raw samples, the precision and accuracy for three methods were obtained within error rate of about 10%. Therefore, three methods were standardized as official monitoring method in Korea. Also, a convenient and simple liquid-liquid extraction method for the analysis of 1,4-dioxane in water was developed by combined with gas chromatography/mass spectrometry and applied to the water samples in Korea

• Archives of Pharmacal Research
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• v.25 no.5
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• pp.664-668
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• 2002

KR-31543,(2S,3R,4S)-6-amino-4-[N-(4-chlorophenyl)-N-(2-methyl-2H-tetrazol-5-ylmethyl)amino]-3,4-dihydro-2-dimethoxymethyl-3-hydroxy-2-methyl-2H-1-benzopyran is a new neuroprotetive agent for ischemia-reperfusion damage. The in vitro and in vivo metabolism of KR-31543 in rats has been studied by LC-electrospray mass spectrometry. Rat liver microsomal incubation of KR-31543 in the presence of NADPH resulted in the formation of a metabolite M1. M1 was identified as N-(4-chlorophenyl)-N-(2-methyl-2H-tetrazol-5-ylmethyl)amine on the basis of LC-MS/MS analysis with the synthesized authentic standard. Rat CYP3A1 and 3A2 are the major CYP isozymes involved in the formation of M1.

• Journal of Pharmacopuncture
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• v.20 no.4
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• pp.274-279
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• 2017

Objective: SanYangSam and SanYangSanSam are traditional Korea-medical herbs that are grown from Panax ginseng C.A. Meyer. In our previous studies, we found that the functional compounds in SanYangSam and SanYangSanSam were different and depended on the type and the cultivation environment of ginseng. This study aimed to profile the functional constituents in SanYangSam and SanYangSanSam. Methods: To profile the functional aspects of the many compounds that have therapeutic activities in SanYangSam and SanYangSanSam extracts, we used liquid chromatography tandem mass spectrometry and quadrupole orthogonal acceleration time-of-flight mass spectrometry. Results: A total of four major compounds were detected; two of which were the natural flavonoids kaempferol and quercetin. Among others, two polyacetylene compounds, including panaxydol and panaxynol, were detected. Conclusion: In this study, we found that panaxydol, one of the polyacetylene constituents of ginseng, is a candidate anti-cancer agent in SanYangSam and SanYangSanSam pharmacopuncture. In addition, we found that the panaxydol levels in the SanYangSanSam extract were over 30 times those in the SanYangSam extract.

• Environmental Engineering Research
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• v.23 no.3
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• pp.309-315
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• 2018

Chlortetracycline (CTC) is one of the most important compounds in antibiotic production, and its distribution has been widely investigated due to health and ecological concerns. This study presents systematic approach to optimize the high-performance liquid chromatography-tandem mass spectrometry for analyzing CTC in a multiple reaction monitoring mode ($479{\rightarrow}462m/z$). One-factor-at-a-time (OFAT) test with response surface analysis (RSA) was used as optimization strategy. In OFAT tests, the fragmentor voltage, collision energy, and ratio of acetonitrile in the mobile phase were selected as major factors for RSA. The experimental conditions were determined using a composite in cube design (CCD) to maximize the peak area. As a result, the partial cubic model precisely predicted the peak area response with high statistical significance. In the model, the (solvent composition) and (collision $energy^2$) terms were statistically significant at the 0.1 ${\alpha}$-level, while the two-way interactions of the independent variables were negligible. By analyzing the model equation, the optimum conditions were derived as 114.9 V, 15.7 eV, and 70.9% for the fragmentor voltage, collision energy, and solvent composition, respectively. The RSA, coupled with the CCD, offered a comprehensive understanding of the peak area that responds to changes in experimental conditions.

• Animal Bioscience
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• v.34 no.9
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• pp.1532-1543
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• 2021

Objective: This study was aimed to establish a quantitative detection method for meat contamination based on specific polypeptides. Methods: Thermally stable peptides with good responses were screened by high resolution liquid chromatography tandem mass spectrometry. Standard curves of specific polypeptide were established by triple quadrupole mass spectrometry. Finally, the adulteration of commercial samples was detected according to the standard curve. Results: Fifteen thermally stable peptides with good responses were screened. The selected specific peptides can be detected stably in raw meat and deep processed meat with the detection limit up to 1% and have a good linear relationship with the corresponding muscle composition. Conclusion: This method can be effectively used for quantitative analysis of commercial samples.

• Safety and Health at Work
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• v.10 no.2
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• pp.196-204
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• 2019

Background: Liquid chromatography-tandem mass spectrometry (LC-MSMS) for simultaneous analysis of multiple microbial secondary metabolites (MSMs) is potentially subject to interference by matrix components. Methods: We examined potential matrix effects (MEs) in analyses of 31 MSMs using ultraperformance LC-MSMS. Twenty-one dust aliquots from three buildings (seven aliquots/building) were spiked with seven concentrations of each of the MSMs ($6.2pg/{\mu}l-900pg/{\mu}l$) and then extracted. Another set of 21 aliquots were first extracted and then, the extract was spiked with the same concentrations. We added deepoxy-deoxynivalenol (DOM) to all aliquots as a universal internal standard. Ten microliters of the extract was injected into the ultraperformance LC-MSMS. ME was calculated by subtracting the percentage of the response of analyte in spiked extract to that in neat standard from 100. Spiked extract results were used to create a matrix-matched calibration (MMC) curve for estimating MSM concentration in dust spiked before extraction. Results: Analysis of variance was used to examine effects of compound (MSM), building and concentration on response. MEs (range: 63.4%-99.97%) significantly differed by MSM (p < 0.01) and building (p < 0.05). Mean percent recoveries adjusted with DOM and the MMC method were 246.3% (SD = 226.0) and 86.3% (SD = 70.7), respectively. Conclusion: We found that dust MEs resulted in substantial underestimation in quantifying MSMs and that DOM was not an optimal universal internal standard for the adjustment but that the MMC method resulted in more accurate and precise recovery compared with DOM. More research on adjustment methods for dust MEs in the simultaneous analyses of multiple MSMs using LC-MSMS is warranted.

• Analytical Science and Technology
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• v.25 no.1
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• pp.25-32
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• 2012

Isotope dilution mass spectrometry (ID-MS) based on liquid chromatography tandem mass spectrometry (LC/MS/MS) was developed for the accurate determination of sorbic acid in tea-drink. An isotope analogue of sorbic acid, $^{13}C_2$-sorbic acid, was obtained by custom synthesis. MS was operated in the negative mode with selected reaction monitoring (SRM) mode of $[M-H]^-$ ${\rightarrow}$ $[M-CO_2H]^-$ channel at m/z 111 ${\rightarrow}$ 67 for sorbic acid and at m/z 113 ${\rightarrow}$ 68 for its isotope analogue. Chromatographic separation was accomplished with a C18 column and an isocratic mobile phase of 55% of 50 mM ammonium acetate (pH 4.5) and 45% of methanol. Homogeneous reference materials were prepared for validation of this method, including repeatability and reproducibility tests, by fortifying tea-drink with sorbic acid in our laboratory. Repeatability and reproducibility studies showed that the ID-LC/MS method is a reliable and reproducible method which provides less than 3.8% of relative standard deviation (RSD) for the analysis of sorbic acid.

• Analytical Science and Technology
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• v.17 no.3
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• pp.263-270
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• 2004

A method is described for the analysis of short-chain alkylphenol ethoxylates (APEOs), 4-octylphenol-di-ethoxylate (OP2EO) and 4-nonylphenol-di-ethoxylate (NP2EO), in drinking water or wastewater using reversed phase high-performance liquid chromatography with electrospray ionization mass spectrometry. The solvent system was water and methanol containing $10{\mu}M$ trifluoroacetic acid as an ionization solvent. We acidified 1 L of water samples to less than pH 2 with concentrated $H_2SO_4$ and loaded onto Sep-Pak $C_{18}$, and eluted with acetone. The calibration of OP2EO and NP2EO was performed for the concentration range from 20 to 500 ng/L and the correlation coefficients were 0.999 and 0.990, respectively. The limits of detection were 20 ng/L (OP2EO) and 50 ng/L (NP2EO) at a signal-to-noise ratio of 3. Accuracy and precision of this analytical method were 85.8 ~ 122.1% and 8.2 ~ 18.8%, respectively. The proposed method allowed a sensitive and rapid detection of OP2EO and NP2EO and it could be applied for monitoring of APEOs from environmental samples.

• Plant Biotechnology Reports
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• v.5 no.1
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• pp.79-88
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• 2011

Vitis vinifera cv. Koshu is a traditional grape cultivar that has been grown for centuries in Japan. The Koshu grape has pink-colored skin and Koshu wines have slight astringency. We demonstrated for the first time the characterization of hydroxycinnamic acids, flavan-3-ols, and flavonoids in Koshu grape using high-performance liquid chromatography and liquid chromatography-mass spectrometry. The gross weight of phenolic compounds excluding anthocyanins and proanthocyanidins in Koshu grape at harvest was higher than those in Sauvignon Blanc, Chardonnay, and Merlot grapes. In addition, hydroxycinnamic acid and monomeric flavonol contents in Koshu grape were also higher than those in the other grape cultivars. Transcription analysis of cinnamic acid 4-hydroxylase, p-coumarate 3-hydroxylase, caffeate methyltransferase, and flavonol synthase genes indicated high accumulation of hydroxycinnamic acids and flavonols in Koshu grape skin compared with the other cultivars. These findings obtained by chemical and molecular approaches partially explained the phenolic characteristics and the peculiar astringency of Koshu grape.