• Title/Summary/Keyword: LC/MS analysis

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Monitoring of Veterinary Drug Residues in Cultured Fishery Products in Chungcheongnam-do Province (충남지역에서 생산되는 양식수산물의 잔류 동물용의약품 모니터링)

  • Lee, Kang-Bum;Kim, Nam-Woo;Kim, Dong-Uk;Sin, Myeong-Hee;Lee, Mi-Young
    • Journal of Food Hygiene and Safety
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    • v.35 no.5
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    • pp.447-451
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    • 2020
  • For this study, we conducted a simultaneous multiresidue analysis of veterinary drugs in cultured fishery products in Chungnam Province in 2018. A total of 115 fishery product samples were obtained from fish farms and fishery production sites located in the province. In all, 29 residual veterinary drugs in the samples were analyzed using a validated liquid chromatography-tandem mass spectrometry (LC-MS/MS) method. As a result, veterinary drug residues were only detected in a small number of the 106 samples (92.2%), and the detection rate was 7.8% (9 of 115 samples). The amounts were also below maximum residual limit (MRL) for fishery products, although one sample exceeded the MRL allowed by the Ministry of Food and Drug Safety and was detected in loach. The nine residual veterinary drugs were detected in 8 samples: loach, eel, catfish, freshwater bream, flatfish, rockfish and shrimp. The detected veterinary drugs were oxolinic acid, enrofloxacin, ciprofloxacin, sulfadiazine, flumequine and oxytetracycline. The most frequently detected antibiotic was oxolinic acid, and enrofloxacin exceeded the MRL in loach sample. Residues of most veterinary drugs were either not detected or were below the MRL, and while the status of fishery products is seen as safe overall, current surveillance efforts over veterinary drugs should be continued.

Determination of radiolysis products in Tri-Octyl Amine by high performance liquid chromatography-mass spectrometer (HPLC-MS에 의한 Tri-Octyl Amine(TOA)의 방사선 분해산물 정량)

  • Yang, Han-Beom;Lee, Eil-Hee;Moon, Hyung-Sil
    • Analytical Science and Technology
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    • v.18 no.3
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    • pp.201-205
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    • 2005
  • Tri-octyl amine (TOA) is used in solvent extraction process for radioactive waste. This compound may be degraded to di-octyl amine (DOA), mono-octyl amine (MOA) by radioactive materials. Amount of TOA, DOA and MOA in TOA must be monitored because they production of these compounds means degradation of which leads to a decrease in the extraction yield. Retention behavior for TOA, DOA and MOA are studied with Phenomenex LUNA-$C_{18}$ ($4.6mm{\times}25cm$) analytical column and $CH_3OH:H_2O$ (50 mmol $CH_3COONH_4$) eluent by liquid chromatography. Optimum condition for these compounds is $CH_3OH:H_2O$ (50 mmol $CH_3COONH_4$) = 85 : 15 ratio. TOA, DOA and MOA compounds is well separated within 20 minute. Dynamic range is $30{\sim}160{\mu}g/mL$ for TOA, $5{\sim}100{\mu}g/mL$ for DOA and $0.1{\sim}5{\mu}g/mL$ for MOA, respectively. The detection limit are $0.1{\mu}g/mL$ for TOA, $1{\mu}g/mL$ for DOA (in SCAN mode) and $0.1{\mu}g/mL$ for MOA (in SIM mode) in this system with $20{\mu}L$ sample loop.

Antioxidant Activity and Nutrient Content of Ethanol and Hot-Water Extracts of Citrus unshiu Pomace (감귤박 에탄올추출물과 열수추출물의 영양성분 및 항산화 활성)

  • Song, Yeonwoo;Moon, Keun Sik;Kim Cho, Somi
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.42 no.9
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    • pp.1345-1350
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    • 2013
  • The objective of this study was to evaluate the effect of extraction methods on the antioxidant activity of Citrus unshiu pomace. For this purpose, two kinds of citrus pomace (CP)s, whole fruit CP and pulp CP, were used for preparing the extracts with hot water or 70% ethanol. It is well-known fact that whole fruit CP has more calories and carbohydrates, although moisture content is higher in pulp CP. Further, whole fruit CP extracts have higher levels of total phenolic contents compared to CP extracts. In addition, DPPH and alkyl radical scavenging activities were also higher in whole fruit CP, especially in ethanolic extracts. Our results based on liquid chromatography-mass spectrometer showed that 70% ethanolic extract of whole fruit CP has the maximum levels of nobiletin and tangeretin contents. The levels of naringin, which is known as an antioxidant flavonoid, was determined only in the 70% ethanolic extract of whole fruit CP. This result, however, is consistent with the observed DPPH and alkyl radical scavenging activities. We had also performed a gas chromatography analysis that showed all the four extracts contained the compound hydroxymethyl furfural. Significantly, this compound has been reported to have antioxidant activity. Taken together, findings of this study indicate that ethanolic extraction of whole fruit CP is a good source of antioxidant compounds and hence the same could be utilized as an important method to obtain such beneficial compounds on an industrial scale.

Evaluation of Cyantraniliprole Residues Translocated by Lettuce, Spinach and Radish (상추, 시금치 및 알타리무에 의한 Cyantraniliprole의 흡수이행 잔류량 평가)

  • Yoon, Ji Hyun;Lee, Seung Won;Lim, Da Jung;Kim, Seon Wook;Kim, In Seon
    • Korean Journal of Environmental Agriculture
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    • v.40 no.4
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    • pp.335-344
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    • 2021
  • BACKGROUND: Cyantraniliprole is a systemic diamide insecticide that has been used to control lepidopteran pests in agriculture. Cyantraniliprole has become an issue due to its potentiality of unexpectable contamination in rotational crop cultivation. Thus, studies on the evaluation of cyantraniliprole translocated from soil into rotational crops are required. METHODS AND RESULTS: Cyantraniliprole was treated at a yearly maximum application level onto bare soil under greenhouse conditions in two geographically different regions. Lettuce was transplanted and spinach and radish were sown onto the soil 30 and 60 days-plant back intervals (PBIs) after cyantraniliprole treatment. The QuEChERS method was modified and coupled with LC/MS/MS analysis to determine the residues of cyantraniliprole in soil and plant samples. The methods for sample preparation and instrumental conditions were validated to meet the criteria of Codex guidelines and were successful to determine cyantraniliprole quantitatively and qualitatively in the samples. Cyantraniliprole residues in lettuce samples were 0.01 mg/kg for PBI 60 and 0.02 mg/kg for PBI 30, respectively. The residues in spinach samples were 0.01 mg/kg for PBI 60 and 0.01~0.02 mg/kg for PBI 30, respectively. Less than limit of the quantitation (LOQ) level (0.01 mg/kg) of cyantraniliprole was observed in radish samples. The residues in the plant samples were found as the levels less than maximum residue limit (MRL) for leafy and root vegetables. CONCLUSION(S): This study suggests PBI 30~60 days for rotational cultivation of lettuce, spinach and radish in greenhouse soil treated with cyantraniliprole at a yearly maximum application level.

Uptake and Distribution of Bisphenol A and Its Metabolites in Lettuce Grown in Sandy Loam and Loam Soil

  • Cho, Il Kyu;Jeon, Yong-Bae;Oh, Young Goun;Rahman, Md. Musfiqur;Kim, Won-Il;Lee, Young-Deuk
    • Korean Journal of Environmental Agriculture
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    • v.39 no.4
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    • pp.375-383
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    • 2020
  • BACKGROUND: Bisphenol A (BPA) is a chemical widely used in polycarbonate plastics, epoxy resins. BPA is an endocrine disruptor. Residue of BPA in agricultural environments is a major concern. The objective of this study was to understand the characteristics of the uptake and distribution of BPA and its metabolites introduced into the agricultural environment to crops, and to use it as basic data for further research on reduction of BPA in agricultural products. METHODS AND RESULTS: This study established the analysis method of BPA and its metabolites in soil and crops, and estimated the intake of BPA and its metabolites from lettuce (Lactuca sativa) grown in sandy loam and loam soil, which are representative soils in Korea. The two major metabolites of BPA were 4-hydroxyacetophenone (4-HAP) and 4-hydroxybenzoic acid (4-HBA). BPA, 4-HAP and 4-HBA have been analyzed by using liquid chromatography tandem mass spectrometry (LC-MS/MS). These substances were detected in sandy loam and loam soil, indicating that certain portions of BPA were converted to 4-HAP and 4-HBA in the soil; however, it was observed that only 4-HBA migrated to lettuce through the roots into crops. CONCLUSION: The uptake residues showed the BPA and 4-HAP were not detected in lettuces grown on sandy loam (SL) and loam (L) soil treatments that were applied with of 10 ng/g, 50 ng/kg and 500 ng/g of BPA. However, the 4-HBA was detected at the level of 7 ng/g and 11 ng/g in the lettuce grown in sandy loam and loam soil that were treated with the 500 ng/g of BPA, respectively, while the 8 ng/g of 4-HBA was measured in the lettuce cultivated in the loam that was treated with 100 ng/g of BPA. This result presents that the BPA persisting in the soil of the pot was absorbed through the lettuce roots and then distributed in the lettuce leaves at the converted form of 4-HBA, what is the oxidative metabolite of BPA.

Gintonin facilitates brain delivery of donepezil, a therapeutic drug for Alzheimer disease, through lysophosphatidic acid 1/3 and vascular endothelial growth factor receptors

  • Choi, Sun-Hye;Lee, Na-Eun;Cho, Hee-Jung;Lee, Ra Mi;Rhim, Hyewhon;Kim, Hyoung-Chun;Han, Mun;Lee, Eun-Hee;Park, Juyoung;Kim, Jeong Nam;Kim, Byung Joo;Nah, Seung-Yeol
    • Journal of Ginseng Research
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    • v.45 no.2
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    • pp.264-272
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    • 2021
  • Background: Gintonin is a ginseng-derived exogenous G-protein-coupled lysophosphatidic acid (LPA) receptor ligand, which exhibits in vitro and in vivo functions against Alzheimer disease (AD) through lysophosphatidic acid 1/3 receptors. A recent study demonstrated that systemic treatment with gintonin enhances paracellular permeability of the blood-brain barrier (BBB) through the LPA1/3 receptor. However, little is known about whether gintonin can enhance brain delivery of donepezil (DPZ) (Aricept), which is a representative cognition-improving drug used in AD clinics. In the present study, we examined whether systemic administration of gintonin can stimulate brain delivery of DPZ. Methods: We administered gintonin and DPZ alone or coadministered gintonin with DPZ intravenously or orally to rats. Then we collected the cerebral spinal fluid (CSF) and serum and determined the DPZ concentration through liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis. Results: Intravenous, but not oral, coadministration of gintonin with DPZ increased the CSF concentration of DPZ in a concentration- and time-dependent manner. Gintonin-mediated enhancement of brain delivery of DPZ was blocked by Ki16425, a LPA1/3 receptor antagonist. Coadministration of vascular endothelial growth factor (VEGF) + gintonin with DPZ similarly increased CSF DPZ concentration. However, gintonin-mediated enhancement of brain delivery of DPZ was blocked by axitinip, a VEGF receptor antagonist. Mannitol, a BBB disrupting agent that increases the BBB permeability, enhanced gintonin-mediated enhancement of brain delivery of DPZ. Conclusions: We found that intravenous, but not oral, coadministration of gintonin facilitates brain delivery of DPZ from plasma via LPA1/3 and VEGF receptors. Gintonin is a potential candidate as a ginseng-derived novel agent for the brain delivery of DPZ for treatment of patients with AD.

Analysis of Chemical Components for Aerial and Underground Parts of Wild Ginseng and Evaluation of Skin Anti-aging Efficacy (야생 산삼 지상부 및 지하부의 화학성분 분석과 피부 항노화 효능 평가)

  • Seok-Seon Roh;Gwang Jin Lee;Byunghyun Kim;Bo Kyoung Hwang;Hyojin Kim;Yun Hee Chang;Jae-kun Yoou;Young-Sung Ju
    • The Korea Journal of Herbology
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    • v.38 no.5
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    • pp.85-95
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    • 2023
  • Objectives : This study was intended to reveal the chemical profiles of aerial(leaf, stem) and underground(rhizome, radix) parts of wild ginseng, and to investigate their anti-aging effects on human skin cells. Methods : Wild ginseng, estimated for over 20 years, was divided into the aerial and underground parts. Total phenolic contents of each extracts were measured using a Folin-ciocalteu method. The contents of 18 amino acids, 8 minerals and 27 ginsenosides were determined by GC-FID, ICP-MS and LC-MS, respectively. The anti-aging effects, including the radical scavenging activity, the activation of mitochondrial function on human fibroblasts, and the proliferation activity on human keratinocyte progenitor cells, for the whole plant and underground part of wild ginseng were evaluated. Results : The total phenolic acids, amino acids, and minerals in the aerial part were more than twice as high as in the underground part. Compared to the cultivated ginseng root, there were various types of ginsenosides in both parts of wild ginseng, and the total amount was more than twice as high. In particular, the aerial part significantly contained ginsenoside F1, F2, C-Mc1, and C-O, and the distinctive patterns that distinguish each parts of wild ginseng from the cultivated ginseng root were derived. The whole plant and underground part of wild ginseng exhibited significant antioxidant effect(14.3-45.6%), activation of mitochondrial membrane potential(105.5-120.1%), and cell proliferation(112.1-125.4%). Conclusions : The entire plant and underground part of wild ginseng are high value-added plants and have beneficial effects on skin anti-aging properties through its abundant metabolites.

Analysis of Nutrient Content by Digestion Phase of Legumes using an In Vitro Digestion Model (In Vitro Digestion Model을 활용한 두류 소화 단계별 영양성분 변화 분석)

  • Da Bin Lee;Kyeong A Jang;In Seon Hwang;Min Sook Kang;Mi-Kyung Seo;Haeng Ran Kim;Seon Mi Yoo
    • The Korean Journal of Food And Nutrition
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    • v.36 no.5
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    • pp.368-378
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    • 2023
  • Changes in contents of free sugars, amino acids, and fatty acids of legumes were analyzed for each phase of in vitro digestion. In addition, contents of resistant starch in raw and digested pulses were compared. Soybeans, kidney beans, cowpeas, and chickpeas were analyzed. An in vitro digestion model was used to analyze contents of nutrients using LC-MS and GC-MS. Stachyose in kidneybean, cowpea, and chickpea increased as the digestion phase progressed. In four types of legumes, raffinose slightly decreased or showed no significant difference between the Oral phase and the BBMV phase. Content of glucose, a monosaccharide, increased during the BBMV phase. During the digestion phase, levels of free amino acids and free fatty acids also increased. Content of resistant starch was reduced compared to that in the raw material. It was 0.01g/100 g food in soybean, 1.06 g/100 g food in red kidney bean, 0.77g/ 100g food in cowpea, and 0.76 g/100 g food in chickpea. It was confirmed that nutrients in the in vitro digestion model were liberated at each digestion phase with changes in the content of resistant starch. These results are expected to be used as fundamental data for obtaining bioavailability of nutrients.

Target engagement of ginsenosides in mild cognitive impairment using mass spectrometry-based drug affinity responsive target stability

  • Zhu, Zhu;Li, Ruimei;Qin, Wei;Zhang, Hantao;Cheng, Yao;Chen, Feiyan;Chen, Cuihua;Chen, Lin;Zhao, Yunan
    • Journal of Ginseng Research
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    • v.46 no.6
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    • pp.750-758
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    • 2022
  • Background: Mild cognitive impairment (MCI) is a transitional condition between normality and dementia. Ginseng is known to have effects on attenuating cognitive deficits in neurogenerative diseases. Ginsenosides are the main bioactive component of ginseng, and their protein targets have not been fully understood. Furthermore, no thorough analysis is reported in ginsenoside-related protein targets in MCI. Methods: The candidate protein targets of ginsenosides in brain tissues were identified by drug affinity responsive target stability (DARTS) coupled with label-free liquid chromatography-mass spectrometry (LC-MS) analysis. Network pharmacology approach was used to collect the therapeutic targets for MCI. Based on the above-mentioned overlapping targets, we built up a proteineprotein interaction (PPI) network in STRING database and conducted gene ontology (GO) enrichment analysis. Finally, we assessed the effects of ginseng total saponins (GTS) and different ginsenosides on mitochondrial function by measuring the activity of the mitochondrial respiratory chain complex and performing molecular docking. Results: We screened 2526 MCI-related protein targets by databases and 349 ginsenoside-related protein targets by DARTS. On the basis of these 81 overlapping genes, enrichment analysis showed the mitochondria played an important role in GTS-mediated MCI pharmacological process. Mitochondrial function analysis showed GTS, protopanaxatriol (PPT), and Rd increased the activities of complex I in a dose-dependent manner. Molecular docking also predicted the docking pockets between PPT or Rd and mitochondrial respiratory chain complex I. Conclusion: This study indicated that ginsenosides might alleviate MCI by targeting respiratory chain complex I and regulating mitochondrial function, supporting ginseng's therapeutic application in cognitive deficits.

A Study on the Safety of Powdered Agricultural Products in Incheon (분말 농산물가공품의 안전성 조사)

  • Park, Byung-Kyu;Kim, Sun-Hoi;Ye, Eun-Young;Lee, Han-Jung;Seo, Soon-Jae;Kwon, Sung-Hee;Song, Sung-Min;Joo, Kwang-Sig;Heo, Myung-Je
    • Journal of Food Hygiene and Safety
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    • v.35 no.2
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    • pp.136-145
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    • 2020
  • This study was conducted to evaluate pesticide residues and foreign metallic matter on a total of 104 powdered agricultural products in Incheon. Residue testing for 373 pesticides was conducted by GC-MS/MS, LC-MS/MS, GC-ECD, GC-NPD and HPLC-UVD. Foreign metallic matter was detected by magnetic rod. As a result pesticide testing, 7 of the 104 products were found to be within the MRL of the pesticides. The detected pesticides were chlorpyrifos, etofenprox, fenoxanil, malathion, permethrin, tebuconazole and tetraconazole. As for foreign metallic matter, 16 samples were above the allowable limits set by Korean regulations. Therefore, the inspection of residual pesticides in raw material, and the removal of foreign metallic matter will require further stringent attention for the safety of powdered agricultural products.