• Safety and Health at Work
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• 제10권2호
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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.

• 한국대기환경학회지
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• 제33권1호
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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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• 한국환경농학회 2009년도 정기총회 및 국제심포지엄
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• pp.519-527
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• 2009

• 한국식품위생안전성학회지
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• 제37권1호
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• pp.1-8
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• 2022

본 연구는 2021년 2월부터 7월까지 잡곡 106건을 수거하여 잔류농약 실태조사를 하였다. 대형, 중소형 및 온라인 유통매장을 중심으로 국내 잡곡 40건과 수입 잡곡 66건을 수거하였고, GC/MSMS, GC/ECD, GC/NPD, LC/MSMS, UPLC/PDA, HPLC/FLD를 이용하여 다종농약 다성분분석법으로 잔류농약 341종을 분석하였다. 잔류농약이 검출된 잡곡은 대형유통매장 1건, 중소형 유통매장 2건, 온라인 유통매장 5건으로 총 8건(7.5%)이었고, 5건(4.7%)에서는 농약잔류허용기준을 초과하였다. 이들 잡곡에서는 MGK-264, chlorpyrifos, thiamethoxam, malathion, piperonyl butoxide, pirimiphos-methyl 등 6종의 농약 성분이 검출되었다. 검출된 잡곡은 강낭콩(1건), 녹두(6건), 수수(1건)이다. 검출된 잡곡 중 농약잔류허용기준을 초과한 품목은 수입 녹두(5건)로 미얀마산이었고, 초과한 농약 성분은 thiamethoxam이었다.

• 한국식품위생안전성학회지
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• 제36권5호
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• pp.392-399
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• 2021

본 연구는 2020년 1월부터 10월까지 향신식물 114건을 수거하여 잔류농약 실태조사를 실시하였다. GC-MSMS, GC-ECD, GC-NPD, LC-MSMS, LC-PDA, LC-CAS를 이용하여 다종농약 다성분분석법으로 잔류농약 341종을 분석하였다. 조사 결과 36건의 검출이 있었으며 검출률은 31.6%이었다. 이 중 7건은 농약 잔류허용기준을 초과하였으며 부적합률은 6.1%이었다. 농약 잔류허용기준을 초과한 품목은 고수(2건), 민트(2건), 바질(1건), 로즈마리(1건), 서양자초(1건)이었다. 잔류농약 341종을 분석한 결과 22종의 농약 성분이 52회 검출되었고 농약 잔류허용기준을 초과한 성분은 8종이었다. 농약 잔류허용기준을 초과한 성분은 etofenprox, flufenoxuron, fluquinconazole, iprodione, lufenuron, paclobutrazol, phenthoate, spiromesifen 이었다.

• Mass Spectrometry Letters
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• 제13권4호
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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.

• 한국식품위생안전성학회지
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• 제37권4호
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• pp.260-270
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• 2022

본 연구에서는 경기도내 유통매장 및 온라인에서 유통 중인 과일류 18품목과 박과과채류 2품목 114건의 시료를 구입하였다. 과피와 과육을 분리한 후 GC-NPD, GC-ECD, GC-MSMS, LC-MSMS를 이용하여 341종 잔류농약 분석을 진행했다. 과일 전체(과피+과육)를 분석했을 때 48건의 시료에서 검출이 되었고 부적합은 없었으며 0.0025-0.1663 mg/kg의 검출범위를 나타냈다. 과피에서는 85건에서 0.0026-4.7185 mg/kg의 검출범위를 보이며 분리 전과 비교했을 때 높은 검출량을 보였다. 과육에서는 8건의 검출이 있었으며 검출범위는 0.0021-0.0993 mg/kg 로 나타났다. 대부분의 과피에서 농산물의 잔류허용기준 이하의 농약이 검출되었고 키위 과피에서 기준 0.05 mg/kg인 deltamethrin이 0.1020 mg/kg의 검출량을 보였다. 잔류허용기준은 과일 전체에 대한 기준이기 때문에 섭취에 부적합한 것은 아니지만 더욱 안전하고 건강한 과피 섭취를 위해 세척 후 과일 그대로를 섭취할 것을 권장하며 과피와 과육에 대한 지속적인 모니터링이 필요한 것으로 보여진다.

• 대한화장품학회지
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• 제34권3호
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• pp.157-165
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• 2008

이전 연구에서 저자들은 나문재 추출물의 항산화 작용과 추출물 함유 크림의 유화 안정성에 대한 결과를 보고한 바 있다[1,2]. 본 연구에서는 thin layer chromatography(TLC), high performance liquid chromatography (HPLC)와 liquid chromatography/Electrospray Tandem mass spectrometry (LC/ESI/MS/MS), $^1H$-NMR을 이용하여 나문재 추출물에 대한 성분 분석을 수행하였다. 나문재 추출물 중 ethyl acetate분획의 TLC는 5개의 띠($SA1{\sim}SA5$)로 분리되었다. Ethyl acetate 분획의 당 제거반응 후 얻어진 aglycone 분획에 대한 HPLC 크로마토그램은 2개의 피이크(SAA 2 및 SAA 1)를 나타냈고, 각각 그 용리 순서는 quercetin, kaempferol이었으며 조성비는 quercetin 16.88%, kaempferol 83.12%로 kaempferol의 함량이 큰 것으로 나타났다. 또한 LC/ESI-MS/MS를 통해서 SA 2는 kaempferol-3-O-gluco-side로 SA 3는 quercetin-e-O-glucoside, SA 4는 kaempferol-3-O-rutinoside, SA 5는 quercetin-3-O-rutinoside로 확인되었다. LC/ESI-MS/MS의 스펙트럼에서 SAA 1은 탈양성자화된 aglycone 분획에 상용하는 분자이온 $[M-H]^$-(m/z285) 피이크를 나타냈으며, $^1$v 분석을 실시한 결과 [${\delta}$ 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')]에서 피이크들이 나타났다. 따라서 SAA 1은 kaempferol임이 확인되었다. SAA 2는 aglycone 분획에 상응하는 분자이온 $[M-H]^-$ (m/z 301)을 생성하였고, $^1H$-NMR 스펙트럼은 [${\delta}$ 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')]에서 피이크들을 나타냈고, 따라서 SAA 2는 quercetin으로 확인되었다. 결론적으로, 이미 보고된 나문재 추출물의 항산화 작용 그리고 안정성 실험과 더불어 나문재 추출물의 성분분석은 새로운 기능성 화장품원료로서 응용이 가능함을 시사한다.

• 한국대기환경학회지
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• 제34권5호
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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.