• Title/Summary/Keyword: LCMS/MS

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Persistence Study of Thiamethoxam and Its Metabolite in Kiwifruit for Establishment of Import Tolerance

  • Il Kyu Cho;Gyeong Hwan Lee;Woo Young Cho;Yun-Su Jeong;Danbi Kim;Kil Yong Kim;Gi-Woo Hyoung;Chul Hong Kim
    • Korean Journal of Environmental Agriculture
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    • v.41 no.4
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    • pp.355-364
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    • 2022
  • BACKGROUND: Pre-harvest interval and decline pattern of thiamethoxam were determined in kiwifruit using liquid chromatography-tandem mass spectrometry (LCMS/MS). The study was carried out to propose import tolerance using OECD maximum residue limit (MRL) calculator for the export promotion of kiwifruit to Taiwan. METHODS AND RESULTS: The thiamethoxam residue in kiwifruit was determined by using the LC-TriQ-MS/MS with the analytical process to set up the import tolerance under greenhouse conditions for Taiwan. Excellent linearity was observed for all of the analytes with a determination coefficient (R2)≥0.99. The limit of quantification was determined to be 0.01 mg/kg for both thiamethoxam and clothianidin in kiwifruit. Linearity was determined from the co-efficient of determinants (R2) obtained from the seven-point calibration curve. The standard calibration curve showed as follows; 1) Site 1 (Gimje): y = 944,406X + 1,583 (R2=0.9995), 2) Site 2 (Goheung): y = 1,356,205X + 934 (R2=0.9983), and 3) Site 3 (Jangheung): y = 1,239,937X - 3,090 (R2=0.9908). The residue of thiamethoxam in the kiwifruit for three decline trials showed the range of 0.35 to 0.56 mg/kg in site 1 (Gimje), 0.24 to 0.55 mg/kg in site 2 (Goheung), and 0.28 to 0.42 mg/kg in site 3 (Jangheung), respectively. However, clothianidin was not detected in all of the treatments. The maximum residual amounts (decline) in the samples, sprayed according to the safe-use standard for thiamethoxam 10% WG in kiwifruit (30 days before harvest, 3 sprays every 7 days) were 0.56 mg/kg in site 1, 0.55 mg/kg in site 2, and 0.42 mg/kg in site 3, respectively. CONCLUSION(S): The import tolerance (IT) of thiamethoxam for kiwifruit may be proposed to be 0.9 mg/kg by using the OECD MRL calculator.

Proteomic Analysis of Global Changes in Protein Expression During Exposure of Gamma Radiation in Bacillus sp. HKG 112 Isolated from Saline Soil

  • Gupta, Anil Kumar;Pathak, Rajiv;Singh, Bharat;Gautam, Hemlata;Kumar, Ram;Kumar, Raj;Arora, Rajesh;Gautam, Hemant K.
    • Journal of Microbiology and Biotechnology
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    • v.21 no.6
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    • pp.574-581
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    • 2011
  • A Gram-positive bacterium was isolated from the saline soils of Jangpura (U.P.), India, and showed high-level of radiation-resistant property and survived upto 12.5 kGy dose of gamma radiation. The 16S rDNA sequence of this strain was examined, identified as Bacillus sp. strain HKG 112, and was submitted to the NCBI GenBank (Accession No. GQ925432). The mechanism of radiation resistance and gene level expression were examined by proteomic analysis of whole-cell extract. Two proteins, 38 kDa and 86.5 kDa excised from SDS-PAGE, which showed more significant changes after radiation exposure, were identified by MALDI-TOF as being flagellin and S-layer protein, respectively. Twenty selected 2-DE protein spots from the crude extracts of Bacillus sp. HKG 112, excised from 2- DE, were identified by liquid chromatography mass spectrometry (LC-MS) out of which 16 spots showed significant changes after radiation exposure and might be responsible for the radiation resistance property. Our results suggest that the different responses of some genes under radiation for the expression of radiation-dependent proteins could contribute to a physiological advantage and would be a significant initial step towards a fullsystem understanding of the radiation stress protection mechanisms of bacteria in different environments.

A Safety Survey of Pesticide Residues in Fruit Products Circulated in Chungcheongnam-do Province, Korea (충남도내 유통 과일류의 잔류농약 안전성 조사)

  • Lee, Kang-Bum;Kim, Nam-Woo;Song, Nak-Soo;Lee, Jung-Ho;Jung, Sang-Mi;Shin, Myoung-Hee;Choi, Seon-Sil;Kim, Ji-Hee;Sung, Si-Youl
    • Journal of Food Hygiene and Safety
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    • v.34 no.5
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    • pp.421-430
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    • 2019
  • In this study, 195 pesticide residues in fruit samples (n=150) at local markets in Chungcheongnam-do Chungnam, Korea were monitored using a multi-residue method combined with GC-MS/MS and LCMS/MS. Among 150 fruit samples, 40 types of pesticides were detected in 63 samples and the detection rate was 42.0%. However, the amounts were below the maximum residue limit (MRL). Detection rates for pesticides in each thpe of fruit were as follows ; citrus fruits (55.2%), pome fruits (41.3%), berries (38.7%) and stone fruits (36.0%). Although the sample size was small (n=2), pesticide residues were not detected in tropical fruits. Occurrences of detection of pesticide residues in apple showed the highest level, and mainly, insecticides were detected most frequently. The most commonly detected pesticides residues were bifenthrin (21), pyraclostrobin (17), novaluron (13), boscalid (10), chlorfenapyr (9), trifloxystrobin (9), furathiocarb (9), acetamiprid (8) and chlorpyrifos (8). Five types of residual pesticides (bifenthrin, chlorfenapyr, deltamethrin, fenpropathrin and fenvalerate) were detected in quince, and out of these five, fenpropathrin exceeded the MRL based on the Positive List System (PLS). These results suggested that pesticide residues in fruit samples should be continuously monitored, although residue levels in 63 other fruit samples were evaluated as being within a safe level.

Antimalarial Activity and Phytochemical Profile of Ethanolic and Aqueous Extracts of Bidara Laut (Strychnos ligustrina Blum) Wood

  • MANURUNG, Harisyah;SARI, Rita Kartika;SYAFII, Wasrin;CAHYANINGSIH, Umi;EKASARI, Wiwied
    • Journal of the Korean Wood Science and Technology
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    • v.47 no.5
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    • pp.587-596
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    • 2019
  • This study aimed to determine the antimalarial effect of the Strychnos ligustrina (SLW) wood extracts and to analyze its phytochemicals. The SLW powder samples were macerated with 100% ethanol (E100), 75% ethanol (E75), 50% ethanol (E50), 25% ethanol (E25), and aqueous (A100). The extracts were analyzed by LCMS/MS, and its in-vitro antimalarial activity was tested with Plasmodium falciparum. The results showed that the extract yields of E100, E75, E50, E25, and A100 were 4.3, 5.2, 5.3, 4.7, and 3.6%, respectively. The antimalarial activities of the A100, E25, E50, and E75 extracts were classified as active with $IC_{50}$ values of 38.6, 42.6, 42.9, and $43.7{\mu}g/mL$, respectively. But, the antimalarial activity of the E100 extract was classified as slightly active with $IC_{50}$ values of $87.4{\mu}g/mL$. The dominant compounds contained in the extracts of A100, E25, E50, E75, and E100 was the alkaloid compound, namely brucine with relative concentrations of 24.96, 24.55, 21.33, 11.79, and 11.62%, respectively.

Biological Activities and the Metabolite Analysis of Camptotheca acuminata Dence.

  • Cho, Jwa Yeong;Park, Mi Jin;Ryu, Da Hye;Kang, Young-Hwa
    • Proceedings of the Plant Resources Society of Korea Conference
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    • 2018.04a
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    • pp.14-14
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    • 2018
  • This Camptotheca acuminata Decne. (CA), belonging to Nyssaceae, is a deciduous tree. and has been used as Traditional Chinese medicine since ancient times. The CA produces camptothecin a natural indole alkaloid, and reported to have anti-cancer effects. But the studies on biological activities of CA leaves are insufficient. Therefore, this study confirmed various biological activities such as antioxidant, antidiabetic, anticancer, antiinflammatory and metabolism analysis by HPLC-MS/MS of CA leaves. The $RC_{50}$ values of DPPH radical scavenging activity of ethyl acetate fraction, n-Butanol fraction, methanol extraction, water fraction and n-Hexane fraction were $12.23{\pm}0.01$, $15.93{\pm}0.42$, $55.12{\pm}0.45$, $56.29{\pm}4.15$ and $427.29{\pm}6.13ug/mL$, respectively. The $IC_{50}$ values of ${\alpha}$-glucosidase inhibitory activity of ethyl acetate fraction, n-Butanol fraction, methanol extraction, n-Hexane fraction and water fraction were $24.29{\pm}0.14$, $47.86{\pm}0.45$, $54.23{\pm}1.21$ $466.76{\pm}2.21$ and $623.91{\pm}9.67ug/mL$, respectively. The nitric oxide release activity of n-Hexane fraction, methanol extraction, ethyl acetate fraction, water fraction and n-Butanol fraction were $31.49{\pm}5.74$, $29.79{\pm}0.71$, $26.89{\pm}0.71$, $8.24{\pm}5.83$ and $7.75{\pm}4.08%$ at 25 ug/mL, respectively. The anti-cancer activity of n-Hexane fraction, methanol extraction, ethyl acetate fraction, water fraction and n-Butanol fraction were $31.49{\pm}5.74$, $29.79{\pm}0.71$, $26.89{\pm}0.71$, $8.24{\pm}5.83$ and $7.75{\pm}4.08%$ at 25 ug/mL, respectively. The ethyl acetate fraction activities showed higher biological activities than other fractions. Thus, Additional studies were conducted using ethyl acetate fraction. Metabolite analysis was performed using a LCMS-8040 triple quadrupole mass spectrometer. As a result, Five compounds (1-5) were identified in the ethyl acetate fraction of the CA leave. The identification of these compounds was generated by the analysis of fragmentation methods of the negative and positive ion modes. Five compounds were identified as gallic acid (1), chlorogenic acid (2), isoquercetin (3), astragalin (4) and camptothecin (5). These results suggest that the CA leave can be used for functional materials.

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Comparison of the bioactive compounds and anti-inflammatory effects found in different flower colors from Abeliophyllum distichum Nakai (미선나무 꽃 색에 따른 생리활성 화합물 및 항염증 활성 비교)

  • Jang, Tae-Won;Choi, Ji-Soo;Han, So-Yeon;Park, Hye-Jeong;Lee, Da-Yoon;Min, Young-Sil;Park, Jae-Ho
    • Journal of Applied Biological Chemistry
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    • v.65 no.3
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    • pp.203-213
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    • 2022
  • Abeliophyllum distichum (A. distichum, Korean endemic plant) is one genus and one species in the Oleaceae family. According to the color variation of petals and calyx, A. distichum is classified as A. distichum (white flower), A. distichum for. lilacinum (pink flowers), A. distichum for. eburneum (ivory flowers), and Okhwang 1 (golden flowers). In previous studies, bioactivities (antioxidant, anti-inflammatory, and anti-cancer) of A. distichum have been reported. We conducted a comparison of the differences in bioactive compounds and the anti-inflammatory effects on macrophages among four flowers of A. distichum (FAD). The identification and quantification of glycosides were analyzed by HPLC/PDA and LCMS. These results were shown FAD has rutin, hirsutrin, and acteoside. Antioxidant activity of FAD significantly decreased reactive oxygen species. In addition, FAD reduced the expression of pro-inflammatory mediators (nitric oxide, iNOS, and COX-2) in lipopolysaccharide-induced RAW 264.7 cells. For further study, we investigated the regulation of nuclear factor kappa B (NF-κB) and mitogen-activated protein kinase (MAPK) signaling pathways. In conclusion, FAD may exert anti-inflammatory effects by suppressing inflammatory mediators via regulations of NF-κB and MAPK signaling pathways. Therefore, these findings suggest that FAD is a potential resource as a preventative or therapeutic agent for inflammation.