• The Korean Journal of Pesticide Science
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• v.20 no.2
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• pp.104-127
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• 2016

A new analytical method has been developed to determine 320 pesticides in apple and rice. The extraction of pesticides was carried out based on QuEChERS sample extraction, and determination was performed using LC-MS/MS and GC-MS/MS. 320 pesticides were selected for experiments. 251 and 110 pesticides among them were analysed by LC-MS/MS and GC-MS/MS, respectively. 41 pesticides of them were analyzed by both GC-MS/MS and LC-MS/MS. Among pesticides analysed by LC, 242 pesticides (96% of total number) in apple and 237 pesticides (94% of total number) in rice showed recoveries in the range of 70~120% with RSD ${\leq}20%$. In case of pesticides analyzed by GC-MS/MS, 103 pesticides (94% of total number) in apple and 83 pesticides (76% of total number) in rice were successfully validated. These results indicated that LC-MS/MS and GC-MS/MS analysis with the QuEChERS sample preparation can be partly applied to multi-residue pesticides in agricultural products.

• YAKHAK HOEJI
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• v.54 no.5
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• pp.377-386
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• 2010

Single-dimensional (1-D) and two-dimensional (2-D) LC methods were utilized to separate peptides from various sources followed by MS/MS analysis. Two-dimensional ultra-high performance liquid chromatography is a useful tool for proteome analysis, providing a greater peak capacity than 1-D LC. The most popular 2-D LC approach used today for proteomic research combines strong cation exchange and reversed-phase LC. We have evaluated an alternative mode for 2-D LC of peptides using 2-D RP-RP nano UPLC Q-TOF Mass Spectrometry, employing reversed-phase columns in both separation dimensions. As control experiments, we identified 129 proteins in 1-D LC and 322 proteins in 2-D LC from E. coli extract peptides. Furthermore, we applied this method to rat primary hepatocyte and a total of 170 proteins were identified from 1-D LC, and 527 proteins were identified from all 2-D LC system. The in-depth protein profiling established by this 2-D LC MS/MS from rat primary hepatocyte could be a very useful reference for future applications in regards to drug induced liver toxicity.

• Analytical Science and Technology
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• v.20 no.5
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• pp.400-405
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• 2007

The comparative analysis of glycerin in cosmetic samples was carried out by LC/MS and $^1H$ NMR spectrometry. For the LC/MS analysis, aqueous solution was controlled in strong basic condition with sodium hydroxide, and benzoyl chloride was added to the solution for the derivatization of glycerin. The derivative was extracted using pentane and analyzed by the LC/MS. For the $^1H$ NMR analysis, sample was directly dissolved in $D_2O$ solvent without pretreatment. The quantitative analysis of glycerin was done by $^1H$ NMR ERETIC method. The analysis results of LC/MS and $^1H$ NMR showed that the calibration curves were a good linearity with $r^2=0.9991$ in the range of 0.1 to $10{\mu}g/mL$ and $r^2=1$ in the range of 25 to $500{\mu}g/mL$, respectively.

• Journal of Practical Engineering Education
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• v.14 no.2
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• pp.327-332
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• 2022

This experiment presents a precise analysis method using a mass spectrometer in the biopharmaceutical market, where utility is expanding. Among various techniques for analyzing the protein drug, somatotropin, the peptide fragments through biochemical sample preparation was analyzed by LC-MS/MS characterization. The analysis process was performed by separation analysis using nanoUPLC and MS/MS analysis using Orbitrap. In the case of somatotropin with 21 tryptic peptides, 13 of them were consistent with theoretical predictions within an average of 1 ppm error.

• Analytical Science and Technology
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• v.16 no.2
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• pp.125-133
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• 2003

In order to determine the contents of trans-resveratrol in red wine, which was mainly consumed in Korea, both LC/MS-ESI and LC/MS-APCI methods were used after solid-phase (Sep-Pak $C_{18}$-cartridges) extraction. The contents of trans-resveratrol obtained by LC/MS-ESI were detected in the range of $0.06-4.31{\mu}g/mL$. The recoveries were ranged from 88.4 to 97.9%. The values of relative standard deviation were ranged from 0.6 to 4.6% and the detection limit was $0.001{\mu}g/mL$. The contents of trans-resveratrol obtained by LC/MS-APCI were detected in the range of $0.09-4.02{\mu}g/mL$ and the detection limit was $0.005{\mu}g/mL$.

• Korean Journal of Environmental Agriculture
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• v.39 no.2
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• pp.142-169
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• 2020

BACKGROUND: A new analytical method has been developed to determine 261 pesticide residues in herbal medicines. METHODS AND RESULTS: The extraction of pesticides was carried out by modified method of the Korea Food Standards Codex sample extraction and determination was performed using GC-MS/MS and LC-MS/MS. During the pre-treatment process of the test method, Solid-liquid separation was changed to centrifugation. The method was validated by the precision and accuracy results. 261 pesticides spiked at three level 20, 50, 100 ug/kg in herbal medicines. The limit of quantification of method were 4-40 ug/kg for GC-MS/MS and 2-45 ug/kg for LC-MS/MS, respectively. Among the pesticides analysed by GC-MS/MS and LC-MS/MS, 244 pesticides (94% of total number) in chinese matrimony vine and 224 pesticides (86% of total number) in korean angelica root and 231 pesticides (89% of total number) in jujube and 214 (82% of total number) in cnidium showed recoveries in the range of 70-120% with RSD⪯20%. CONCLUSION: These results indicated that GC-MS/MS and LC-MS/MS analysis with the sample extraction in this study can be applied to multi-residue analysis of pesticides in herbal medicines.

• The Journal of Internal Korean Medicine
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• v.36 no.3
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• pp.217-227
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• 2015

Objectives: The primary aim of this study was to identify bioactive compounds in Dangnyo-hwan, a Korean herbal medicine, through instrumental analysis using LC-MS/MS and ICP, and investigate its potential use in diabetes treatment. Methods: The extract of Dangnyo-hwan has 12 medicinal herbs; these were compared with 18 marker substances selected from literature survey. Results: LC-MS/MS analysis could detect 9 of the 18 bioactive compounds: citruline, catalpol, berberine, ginsenoside Rb1, ginsenoside Rg1, oleanolic acid, β-sitosterol, mangiferin, and schizandrin. While harmful heavy metals such as As, Pb, Cd, Hg, Ni, and Cu were not present in high concentrations, Zn concentration was 4.2 mg in 100 g Dangnyo-hwan. Conclusions: Instrumental analysis such as LC-MS/MS and ICP was successfully used to identify bioactive compounds in Dangnyo-hwan. Detection of 9 bioactive substances and Zn from the herb medicine is a valuable finding, and suggests that Dangnyo-hwan is a candidate medicine for diabetes. Further investigations like in vitro assay, percent GPR 119 activity, and percent human DGAT-1 inhibition are underway.

• Korean Journal of Food Science and Technology
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• v.46 no.5
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• pp.549-555
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• 2014

The geographical origin of commercial red ginseng concentrate was studied using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The ginsenoside content of domestic and Chinese red ginseng concentrates was determined. Four types of suspected origin samples could be selected this technique. The LC-MS/MS data were statistically analyzed on the basis of canonical function analysis and principal component analysis. Domestic and Chinese samples could be discriminated via canonical function analysis using posterior probability. In addition, the mixture ratio (Korean or Chinese origin) of the unknown origin specimen could be predicted based on the relationship between the mixing concentration of red ginseng concentrates and principal component 1.

• Korean Journal of Pharmacognosy
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• v.44 no.4
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• pp.350-361
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• 2013

Asarum sieboldii has been used for treatment of fever, pain, common cold, and chronic sinusitis in Korea. In this study, we performed quantification analysis of seven major constituents including aristolochic acid I, aristolochic acid II, ${\alpha}$-asarone, ${\beta}$-asarone, elemicin, methyl eugenol, and safrole in the 70% ethanol extract of Asarum sieboldii and its solvent fractions, n-hexane, ethylacetate, n-butanol, and water ones using a ultra-performance liquid chromatography-electrospray ionization-mass spectrometer(UPLC-ESI-MS) and gas chromatography-mass spectrometer(GC-MS). Regression equations of seven components were acquired with $r^2$ values >0.99. The values of limit of detection(LOD) and quantification(LOQ) were 0.1-3.9 ng/mL and 0.3-11.7 mg/mL, respectively. The amount of the seven compounds in Asarum sieboldii were not detected -143.66 mg/g. The established LC-MS/MS and GC-MS methods will be helpful to improve quality control of Asarum sieboldii.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.46 no.2
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• pp.154-159
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• 2013

The AOAC Mouse Bioassay method (MBA) has been widely used for routine monitoring of paralytic shellfish poisoning (PSP) for more than 50 years. However, this method has low sensitivity and experiences interference from other components in the extract. Also, ethical issues have been raised against the continued use of this live-mouse assay. To establish an alternative method for PSP analysis, we attempted to develop PSP analysis conditions using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The LC-MS/MS analysis of reference material showed very reasonable accuracy, and the analysis time was just 15 min. However, the recovery rate of toxin spike samples using the LC-MS/MS analysis was 59.4-91.0%. We also attempted to remove the matrix effect using shellfish extracts, but recoveries of C1 and C2 did not improve. A comparison between the results of MBA and LC-MS/MS analysis revealed good correlations, with values of 0.8878 and 0.9211 for oyster and mussel matrices, respectively.