• Title/Summary/Keyword: LC-MS/MS method

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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.

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.

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.

A Study on the Safety of Mycotoxins in Grains and Commonly Consumed Foods (곡류 등 다소비 식품 중 곰팡이독소 안전성 조사 연구)

  • Kim, Jae-Kwan;Kim, Young-Sug;Lee, Chang-Hee;Seo, Mi Young;Jang, Mi Kyung;Ku, Eun-Jung;Park, Kwang-Hee;Yoon, Mi-Hye
    • Journal of Food Hygiene and Safety
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    • v.32 no.6
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    • pp.470-476
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    • 2017
  • The purpose of this study was to investigate and evaluate the safety of the grains, nut products, beans and oilseeds being sold in Gyeonggi province by analyzing mycotoxins. A multi-mycotoxins analysis method based on LC-MS/MS was validated and applied for the determination of eight mycotoxins, including aflatoxins ($B_1$, $B_2$, $G_1$ and $G_2$), fumonisins ($B_1$, $B_2$), zearalenone and ochratoxcin A in 134 samples. The limit of detection (LOD) and limit of quantitation (LOQ) for the eight mycotoxins ranged from 0.14 to $8.25{\mu}g/kg$ and from 1.08 to $7.21{\mu}g/kg$, respectively. Recovery rates of mycotoxins were determined in the range of 61.1 to 97.5% with RSD of 1.0~14.5% (n=3). Fumonisin $B_1$, $B_2$, zearalenone, and ochratoxin A were detected in 22 samples, indicating that 27% of grains, 12.5% of beans and 11.8% of oilseeds were contaminated. Fumonisin and zearalenone were detected simultaneously in 2 adlays and 3 sorghums. Fumonisin $B_1$ and $B_2$ were detected simultaneously in most samples whereas fumonisin $B_1$ was detected in 1 adlay, 1 millet and 1 sesame sample. The average detected amount of fumonisin was $49.3{\mu}g/kg$ and $10.1{\mu}g/kg$ for grains and oilseeds, respectively. The average detected amount of zearalenone was $1.9{\mu}g/kg$ and $1.5{\mu}g/kg$ for grains and beans, respectively. In addition, the average amount of ochratoxin A was $0.08{\mu}g/kg$ for grains. The calculated exposure amounts of fumonisin, zeralenone and ochratoxin A for grains, beans and oilseeds were below the PMTDI/PTWI.

Preparation and Antioxidant Activities In Vitro of a Designed Antioxidant Peptide from Pinctada fucata by Recombinant Escherichia coli

  • Wu, Yanyan;Ma, Yongkai;Li, Laihao;Yang, Xianqing
    • Journal of Microbiology and Biotechnology
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    • v.28 no.1
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    • pp.1-11
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    • 2018
  • An antioxidant peptide derived from Pinctada fucata meat using an Alcalase2.4L enzymatic hydrolysis method (named AOP) and identified by LC-TOF-MS has promising clinical potential for generating cosmetic products that protect skin from sunshine. To date, there have been few published studies investigating the structure-activity relationship in these peptides. To prepare antioxidant peptides better and improve their stability, the design and expression of an antioxidant peptide from Pinctada fucata (named DSAOP) was studied. The peptide contains a common precursor of an expression vector containing an ${\alpha}$-helix tandemly linked according to the BamHI restriction sites. The DNA fragments encoding DSAOP were synthesized and subcloned into the expression vector pET-30a (+), and the peptide was expressed mostly as soluble protein in recombinant Escherichia coli. Meanwhile, the DPPH radical scavenging activity, superoxide radical scavenging activity, and hydroxyl radical scavenging activity of DSAOP $IC_{50}$ values were $0.136{\pm}0.006$, $0.625{\pm}0.025$, and $0.306{\pm}0.015mg/ml$, respectively, with 2-fold higher DPPH radical scavenging activity compared with chemosynthesized AOP (p < 0.05), as well as higher superoxide radical scavenging activity compared with natural AOP (p < 0.05). This preparation method was at the international advanced level. Furthermore, pilot-scale production results showed that DSAOP was expressed successfully in fermenter cultures, which indicated that the design strategy and expression methods would be useful for obtaining substantial amounts of stable peptides at low costs. These results showed that DSAOP produced with recombinant Escherichia coli could be useful in cosmetic skin care products, health foods, and pharmaceuticals.

Isolation of Microcystin-LR and Its Potential Function of Ionophore

  • Kim, Gilhoon;Han, Seungwon;Won, Hoshik
    • Journal of the Korean Magnetic Resonance Society
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    • v.19 no.2
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    • pp.67-73
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    • 2015
  • The microcystin is a cyclic heptapeptide from metabolites of cyanobacteria in the genera mycrocystis, anabaeba as a result of eutrophication. It has been known that microcystin-LR is a potent inhibitor of the catalytic subunits of protein phosphatase-1 (PP-1) as well as powerful tumor promoter. The active site of microcystin actually has two metal ions $Fe^{2+}/Zn^{2+}$ close to the nucleophilic portion of PP-1-microcystin complex. We report the isolation and purification of this microcystin-LR from cyanobacteria (blue-green algae) obtained from Daechung Dam in Chung-cheong Do, Korea. Microcystin-LR was extracted from solid-phase extraction (SPE) sample preparation using a CN cartridge. The cyanobacteria extract was purified to obtain microcystin-LR by HPLC method and identified by LC/MS. The detail structural studies that can elucidate the possible role of monovalent and divalent metal ions in PP-1-microcystin complexation were carried out by utilizing molecular dynamics. Conformational changes in metal binding for ligands were monitored by molecular dynamic computation and potential of mean force (PMF) using the method of the free energy perturbation. The microcystin-metal binding PMF simulation results exhibit that microcystin can have very stable binding free energy of -10.95 kcal/mol by adopting the $Mg^{2+}$ ion at broad geometrical distribution of $0.5{\sim}4.5{\AA}$, and show that the $K^+$ ion can form a stable metal complex rather than other monovalent alkali metal ions.

Comparative Proteomic Analysis of Changes in the Bovine Whey Proteome during the Transition from Colostrum to Milk

  • Zhang, Le-Ying;Wang, Jia-Qi;Yang, Yong-Xin;Bu, Deng-Pan;Li, Shan-Shan;Zhou, Ling-Yun
    • Asian-Australasian Journal of Animal Sciences
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    • v.24 no.2
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    • pp.272-278
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    • 2011
  • Bovine whey protein expression patterns of colostrum are much different from that of milk. Moreover, bovine colostrum is an important source of protective, nutritional and developmental factors for the newborn. However, to our knowledge, no research has been performed to date using a comparative proteomic method on the changes in the bovine whey proteome during the transition from colostrum to milk. This study therefore separated whey protein of days 1, 3, 7 and 21 after calving using two dimension electrophoresis. Differentially expressed proteins at different collection times were identified using high-performance liquid chromatography in tandem with mass spectrometry (LC/MS) and validated by enzyme-linked immunosorbent assay (ELISA) in order to understand the developmental changes in the bovine whey proteome during the transition from colostrum to milk. The expression patterns of whey protein of days 1 and 3 post-partum were similar except that immunoglobulin G was down-regulated on day 3, and four proteins were found to be down-regulated on days 7 and 21 compared with day 1 after delivering, including immunoglobulin G, immunoglobulin M, albumin, and lactotransferrin, which are involved in immunity and molecule transport. The results of this study confirm the comparative proteomic method has the advantage over other methods such as ELISA and immunoassays in that it can simultaneously detect more differentially expressed proteins. In addition, the difference in composition of milk indicates a need for adjustment of the colostrum feeding regimen to ensure a protective immunological status for newborn calves.

Studies on the Technical Development of the Traditional Korean Golden Varnish(Hwangchil) (III) - Main Component Analysis of Korea Golden Varnishes Traditonally Refined from the Exudates of Dendropanax morbifera Lev. - (전통 황칠 도료 개발에 관한 연구(III) - 전통 황칠 도료의 주성분 분석 -)

  • Lim, Kie-Pye;Jung, Woo-Yang;Hong, Dong-Hwa
    • Journal of the Korean Wood Science and Technology
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    • v.26 no.3
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    • pp.73-80
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    • 1998
  • In order to reconstruct the traditional technology of Korean golden varnish coatings, this study was carried out to separate and determine some main coloring components of the exudates of D. morbifera and its traditionally refined golden varnishes using a process of solvent extractions, chromatographies and spectrometries. The results obtained are as follows: 1. The exudate and its traditional-refined golden varnishes appear to have a kind of natural polyacetylenes because it has some triple bond peaks in FT-IR spectrometry. 2. Some yellowing spots of the polar-solvent extrats from the exudates and refined varnishes separated on TLC appeared under natural drying condition, but those of non-polar solvent extract such as hexane did not. 3. A traditional refining method for reconstructing a Korea golden varnishes was thought to be better than solvent separation because the former had higher triple-bond peaks than the latter in FT-IR spectrometry. 4. One of main conponents in the hexane-extracts of the traditional-refined varnishes and the exudates had the same molcular weighr of 204, but the fragmentation patterns was a little different between the exudate and the refined. in LC-MS soectrometry.

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