• 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.

• Journal of Korean Society for Atmospheric Environment
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• v.33 no.1
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• pp.54-63
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• 2017

Atmospheric nitrogen containing organic compounds(e.g. amino acids) has attracted considerable attention from the viewpoint of the oceanic biogeochemical cycle of nitrogen as well as the long range transfer. However, only a few measurements of organic nitrogen compounds have been conducted due to analytical difficulties. In this study, total of nine amino acids such as Glutamic acid, Histidine, Arginine, Tyrosine, Cystine, Valine, Methionine, Phenylalanine, Lysine have been analytically determined by Liquid Chromatography - Mass Spectrometry Mass Spectrometry (LC-MSMS). As results, Fragmentor Voltage (FV), Precursor Ion, Collision Energy, Product Ion related to individual amino acid compounds are shown. Based on the operational conditions, Lysine, Glutamine Acid, Tyrosine were analyzed during the China Oriented Smog Period. High concentrations of Lysine, Glutamine Acid, and Tyrosine are discussed with organic carbon (OC), elemental carbon (EC), and water soluble ions. The results can provide to understand the sources with aging process related to amino acids influenced by the long-range transport from the Yellow Sea area.

• 한국환경농학회:학술대회논문집
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• 2009.07a
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• pp.519-527
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• 2009

• Journal of Food Hygiene and Safety
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• v.37 no.1
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• pp.1-8
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• 2022

In this study, the pesticide residues in 106 commercial cereal grains were monitored from February to July 2021. For the investigation, 40 domestic and 66 imported products from large, small-to-medium sized offline and online distribution channels, were collected and analyzed by using the multiresidue method for 341 pesticides on GC/ECD, GC/NPD, GC/MSMS, UPLC/PDA, HPLC/FLD, LC/MSMS. Pesticides were detected in total of 8 samples (7.5%), of which one was from big box retailers, two from small and medium-sized distribution stores, and five from online shopping mall. Five (4.7%) samples were found to have pesticide residues greater than the maximum residue limits (MRLs). The detected pesticides in kidney beans (1 case), mung beans (6 cases), and sorghum (1 case), were MGK-264, chlorpyrifos, thiamethoxam, malathion, piperonyl butoxide, and pirimiphos-methyl. Specifically, an excessive amount of thiamethoxam was found from the imported mung bean (5 cases).

• Journal of Food Hygiene and Safety
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• v.36 no.5
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• pp.392-399
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• 2021

This study was conducted to research the status of pesticide residues in a total of 114 herbs and spices obtained from January to October 2020. 341 pesticide residues were analyzed by the multi class pesticide multiresidue methods using GC-MSMS, GC-ECD, GC-NPD, LC-MSMS, LC-PDA, and LC-CAS. As a result of analysis, 36 pesticide residues were found, and detection rate was 31.6%. Of them, seven samples were detected over Maximum Residue Limits (MRLs) and the unsuitable level in pesticide was 6.1%. The herbs and spices exceeding MRLs include coriander (2 times), mint (2 times), basil (once), rosemary (once), and boraye (once). According to an analysis of 341 pesticide residues, 22 pesticides were detected 52 times and 8 pesticides were found to exceed the MRLs. The pesticides exceeding MRLs were ingredients such as etofenprox, flufenoxuron, fluquinconazole, iprodione, lufenuron, paclobutrazol, phenthoate, and spiromesifen.

• Mass Spectrometry Letters
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• v.13 no.4
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• pp.158-165
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• 2022

Many therapeutic class drugs such as beta-blocker, corticosteroids, NSAIDs, etc are prohibited substances in the horse racing industry. Liquid chromatography-tandem mass spectrometry (LC-MS/MS) technology makes it possible to isolate drugs from interference, enables various drug analyses in complex biological samples due to its sensitive sensitivity, and has been successfully applied to doping control. In this paper, we describe a rapid and sensitive method based on solid-phase extraction (SPE) using solid phase cartridge and LC-MS/MS to screen for different class's 35 drug targets in equine plasma. Plasma samples were pretreated by SPE with the NEXUS cartridge consisted non-polar carbon resin and minimum buffer solvent. Chromatographic separation of the analytes was performed on ACQUITY HSS C18 column (2.1 × 150 mm, 1.8 ㎛). The elution gradient was conducted with 5 mM ammonium formate (pH 3.0) in distilled water and 0.1% formic acid in acetonitrile at a flow rate of 0.25 mL/min. The selected reaction monitoring (SRM) mode was used for drug screening with multiple transitions in the positive ionization mode. The specificity, limit of detection, recovery, and stability was evaluated for validation. The method was found to be sensitive and reproducible for drug screening. The method was applied to plasma sample analysis for the proficiency test from the Association of Racing Chemist.

• Journal of Food Hygiene and Safety
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• v.37 no.4
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• pp.260-270
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• 2022

In this study, we tested for pesticide residues in 114 samples representing 20 different types of fruit circulating in Gyeonggido. A total of 341 pesticides were identified via a multi-residue method using GC-NPD, GC-ECD, GC-MSMS, and LC-MSMS. In whole fruit, pesticides were detected in 48 cases, with a concentration range of 0.0025-0.1663 mg/kg. In the peels, pesticides were detected in 85 cases, with a concentration range of 0.0026-4.7185 mg/kg and a higher average concentration than was found in whole fruit. In the pulp, pesticides were detected in 8 cases, with a concentration range of 0.0021-0.0993 mg/kg. In most of the peels, pesticides were detected below MRL. In the kiwi peel, deltamethrin (with an MRL of 0.05 mg/kg) was detected at 0.1020 mg/kg. Since MRLs are applied to whole fruit, these levels are not unsuitable for ingestion. However, washing is recommended before ingestion to promote healthier and safer inclusion of the peel in the diet. Continuous monitoring of the peel and pulp is indicated.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.34 no.3
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• pp.157-165
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• 2008

In the previous study, the anti-oxidant activity of oxtract/fraction of Sueada aspparagoides(SA) and the stability test for the cream containing SA extract were investigated respectively[1,2]. In this study, the components of SA extract were analyzed by TLC, HPLC, and LC/ESI-MS/MS, $^1H$-NMR. TLC chromatogram of ethyl acetate fraction of SA extract revealed 5 bands $(SA1{\sim}SA5)$. HPLC chromatogram of aglycone fractions obtained from deglycoylation reaction of ethyl acetate fraction showed 2 bands (SAA 2 and SAA 1), which were identified as quercetin (composition ratio, 16.88%) and kaempferol (83.12%) in the order of elution time. Among 5 bands of TLC chromatogram, 4 bands $(SA2{\sim}SA5)$ also were Identified as kaempferol-3-O-glucoside (SA 2), quercetin-3-O-glucoside (SA3), kaempferol-3-O-rutinoside (SA 4), quercetin-3-O-rutinoside (SA 5) by LC/ESI-MS/MSMS/MS. respectively. The spectrum generated for SAA 1 by LC/ESI-MS/MS in the negative ion mode also gave the ion corresponding to the deprotonated aglycone $[M-H]^-$ (285m/z), the $^1H$-NMR spectrum contained signals [${\delta}$ 6.19 (1H, d, J=1.8Hz, H-6), ${\delta}$ 6.44 (1H, d, J=1.8Hz, H-8), ${\delta}$ 6.92 (2H, d, J=9.0Hz, H-3', 5'), ${\delta}$ 8.04 (2H, d, J=9.0Hz, H-2', 6', thus SAA 1 was identified as kaempferol. SAA 2 yielded the deprotonated agycone ion $[M-H]^-$ (301m/z), $^1H$-NMR spectrum showed signals [${\delta}$ 6.20 (1H, d, J=2.0Hz, H-6), ${\delta}$ 6.42 (1H, d, J=2.0Hz, H-8), ${\delta}$ 6.90 (1H, d, J=8.6Hz, H-5'), ${\delta}$ 7.55 (1H, dd, J=8.6, 2.2Hz, H-6'), ${\delta}$ 7.69 (1H, d, J=2.2Hz, H-2', thus SAA 2 was Identified as quercetin. In conclusion, with the anti-oxidant activity and the stability test reported previously, component analysis of SA extracts could be applicable to new cosmeceuticals.

• Journal of Korean Society for Atmospheric Environment
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• v.34 no.5
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• pp.639-650
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• 2018

Identification of the major sources contributing to PM is of importance in order to understand their quantitative contributions to atmosphere. In the viewpoint of the meat cooking in Korea, only a few analyses of organic molecular markers have been conducted due to analytical difficulties. In this study, ten different parts of meat (i.e., blade shoulder, belly, and arm shoulder of pork; ribeye roll, top blade muscle, and short plate of beef; leg quarter, breast, and wing of chicken; duck; mackerel) were pyrolyzed to generate the cooked PM using an electronic heating plate. Generated PM were collected by the pyrolysis sampling system to identify total carbon (TC) using a carbon analyzer and cholesterol using a Liquid chromatography tandem-mass spectrometry (LC-MSMS) based on fragmentor voltage (FV), precursor ion, collision energy, product ion. In addition, oxydative potential (OP) analysis using dithiothreitol (DTT) method were discussed to investigate the toxicity relates. Highly correlated pairwise scatterplots between the cholesterol and TC indicate that oxydative potential was highly associated with different parts of meat. This study provides insight into the meat cooking components of PM, which could be drivers of the oxidative potential relates.