• Title/Summary/Keyword: LC-MS-MS

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Method Development and Validation for Analysis of Isopyrazam Residues in Agricultural Products (농산물 중 살균제 Isopyrazam의 개별 잔류분석법 확립)

  • Kim, Ji-Yoon;Kim, Ja-Young;Ham, Hun-Ju;Do, Jung-Ah;Oh, Jae-Ho;Lee, Young-Deuk;Hur, Jang-Hyun
    • The Korean Journal of Pesticide Science
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    • v.17 no.2
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    • pp.84-93
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    • 2013
  • Validated analytical methods for isopyrazam are meager or lacking. In the present study, a single residual analytical method was developed for isopyrazam in selected commodities. Isopyrazam was analyzed in brown rice, soybean, green pepper, mandarin, cucumber, and Korean melon. We tried different solvents and methods through extraction, partition and purification steps to obtain best analytical results. For isopyrazam samples were extracted with acetonitrile, concentrated and partitioned with n-hexane, clean-up using florisil with n-hexane/ethylacetate (70/30) and analyzed with HPLC/UVD. The limit of quantitation (LOQ) for isopyrazam was 1.0 ng (S/N > 10) and method LOQ (MLOQ) was 0.04 mg $kg^{-1}$. Recovery ranged through 81.0~105.3% (syn-isomer) and 80.8~105.6% (anti-isomer) at fortification level of 0.04 (MLOQ), 0.4 (10 ${\times}$ MLOQ), and 2.0 (50 ${\times}$ MLOQ). The coefficient of variation (CV) for isopyrazam was less than 10% regardless of sample types. These results were further confirmed with LC/MS, respectively. The proposed method is highly reproducible and sensitive and is suitable for routine analysis.

Protective Effects of Flavonoids from the Boehmeria quelpaertense against H2O2-Induced Cytotoxicity in H9c2 Cardiomyoblast Cells (H9c2 심근세포에서 제주모시풀(Boehmeria quelpaertense)로부터 분리된 flavonoids의 H2O2로 유도된 독성 보호 효과)

  • Woo, Kyeong-Wan;Sim, Mi-Ok;Bak, Ho;Jung, Ho Kyung;An, Byeongkwan;Ham, Seong-Ho;Park, Jong Hyuk;Cho, Hyun-Woo
    • Korean Journal of Plant Resources
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    • v.31 no.1
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    • pp.1-9
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    • 2018
  • As a part of an infrastructure project on medicinal herb-based remedies, we conducted a phytohemical investigation of the 100% MeOH extract from the aerial part of Boehmeria quelpaertense; our findings resulted in the isolation of flavonoids (1-2), isoquercitrin (1) and hyperoside (2). The identification and structural elucidation of these compounds were based on $^1H$-, $^{13}C-NMR$, and LC ESI IT-TOF MS data. All the compounds isolated from this plant were reported for the first time. In this study, we examined the antioxidant activity of the 1 and 2 on the hydrogen peroxide ($H_2O_2$)-induced oxidative stress in a Rat Cardiomyoblast cell line (H9c2). The pretreatment of the flavonoids showed that it protects against $H_2O_2$-mediated cell death in the H9c2 cell line. Also, it decreases the intracellular reactive oxygen species (ROS) levels by the flavonoids in the $H_2O_2$-treated H9c2 cell line. These results showed that the 1 and 2 are a source of antioxidants. As a result, they might be helpful in preventing the progress of various oxidative stress mediated diseases, including myocardial infarction.

The Compositions and Contents of Flavonol Glycosides in Onion (Allium cepa L.) Germplasm (양파(Allium cepa L.) 유전자원의 Flavonol 배당체 조성 및 함량)

  • Lee, Jung-Ro;Lee, Min-Ki;Kim, Heon-Woong;Lee, Sung-Hyeon;Lee, Young-Min;Jang, Hwan-Hee;Hwang, Kyung-A;Gwag, Jae-Gyun;Ko, Ho-Cheol;Kim, Jung-Bong;Cho, Jin-Woong
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.59 no.3
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    • pp.385-389
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    • 2014
  • Flavonols as a major kind of plant secondary metabolites are known for health-promoting compounds in onions (Allium cepa L.). The objectives of this study are to determine profiles of flavonol glycosides in different 75 onion accessions. A total of five flavonols (quercetin 3,4'-diglucoside, Q34'diG; quercetin 3-glucoside, Q3G; quercetin 4'-glucoside, Q4'G; isorhamnetin 4'-glucoside, I4'G; quercetin, Q) were identified from onion accessions. In positive ion mode using LC-ESI-MS, individual flavonols were confirmed from one and two glycosylation binding with aglycone such as quercetin and isorhamnetin. Total flavonol contents were distributed in white onion (range of 0.18-6.47 mg/g DW) and purple onion accessions (range of 2.39-6.47 mg/g), respectively. The mean of flavonol contents in purple onion (4.41 mg/g) showed 1.4-fold higher than white onion (3.23 mg/g). The Q34'diG and Q4'G were considered as the major compounds of flavonol glycosides in onion accessions.

Comparison of Different Solid-Phase Extraction Methods for the Analysis of Heterocyclic Amines from Pan-Fried Pork Meat (가열 조리된 돼지고기의 Heterocyclic Amines 분석을 위한 Solid-phase 추출 방법의 비교)

  • Lee, Jae-Hwan;Back, Yu-Mi;Lee, Kwang-Geun;Shin, Han-Seung
    • Food Science of Animal Resources
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    • v.28 no.5
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    • pp.637-644
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    • 2008
  • Four different extraction and purification methods were evaluated to determine the heterocyclic amines (HCAs) in fried pork patties. Pork patties were cooked in the teflon-coated electric frying pan at $230^{\circ}C$ for 8 min per side. HCAs in the fried pork patties were extracted and purified using four different solid-phase extraction (SPE) methods and quantitated by LC-MS (API-ESI). Recovery of four different extraction and purification methods was evaluated by comparing the HCAs amounts quantified by the standard addition method. Validation of extraction and purification methods for fried pork patties was determined to establish accurate sample preparation. The recoveries of HCAs from different SPE methods were calculated. The recovery yields were 15.7-68.7% (Polar amine group) and 25.0-74.7% (less-polar amine group) in method A. Method D provided recovery yields ranging from 14.1% to 68.7% in polar amine groups and from 3.0% to 72.3% in less-polar amine groups, respectively. Modified procedures of Method A and D were the most suitable extraction and purification method for HCAs analysis from fried pork patties.

Biosensor System for the Detection of Agrichemicals and Its Applications (농약 검출을 위한 바이오센서 시스템 연구 및 그 응용)

  • Park, Tae-Jung;Yang, Min-Ho;Lee, Sang-Yup;Kim, Soo-Hyun
    • KSBB Journal
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    • v.24 no.3
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    • pp.227-238
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    • 2009
  • In the recent years, some organic toxic chemicals were used for obtaining high-yield productivity in agriculture. The undegraded pesticides may remain in the agricultural foods through atmosphere, water, and soil and cause public health problems to environmental resources and human beings even at very low concentrations. Small amounts of pesticides can affect a central nervous system, resulting in immunogenic diseases, infertility problems, respiratory diseases and born marrow diseases, which can lead even to death. Monitoring of the environmental pesticide is one of the important issues for the human well-being. Several kinds of biosensors have been successfully applied to the detection of agrichemical toxicity. Also, few platforms for biocide detection have been definitely developed for the degradation and reaction of pesticides. Biochip and electrochemistry experiments involve immobilizing a receptor molecule on a solid substrate surface, and monitoring its interaction with an analyze in a sample solution. Furthermore, nanotechnology can be applied to make high-throughput analyses that are smaller, faster and sensitive than conventional assays. Some nanomaterials or nanofabricated surfaces can be coupled to biomolecules and used in antibody-based assays and enzymatic methods for pesticide residues. The operation procedure has become more convenient as it does not require labeling procedure. In this paper, we review the recent advances in agrichemical defection research and also describe the label-free biosensor for pesticides using various useful detection methods.

Identification of Standard Compound of Ja-ha-guh Pharmacopuncture and Validation of Analytic Methods (자하거 약침의 지표물질 선정 및 분석법 벨리데이션)

  • Park, Sang-won;Lee, Jae-woong;Lee, Jin-ho;Ha, In-Hyuk;Byun, Jang-hoon;Jung, Bum-hwan;Jung, Hwa-jin;Lee, In-hee;Kim, Min-Jeong;Kim, Eun-Jee
    • Journal of Korean Medicine Rehabilitation
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    • v.26 no.1
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    • pp.33-40
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    • 2016
  • Objectives Despite the increasing use of Ja-ha-guh (Hominis-placenta ) pharmacopuncture in rehabilitative medicine field, its standard compound has yet to be investigated. The purpose of this study is to provide standardization for future studies and increase satisfaction of patients by utilizing standard pharmacopuncture. Methods Alanine and leucine were selected as potential standard compounds. LC/MS was used to devise an analytic method. This analytic method was subject to validation. According to validation guideline of Korea Food and Drug Administration, the specificity, linearity, precision, range, quantitative limits, detection limits and accuracy were measured. With this analysis, 3 lots of Ja-ha-guh pharmacopuncture were analyzed. Results Because the specificity, linearity, precision, range, quantitative limits, detection limits and accuracy meet criteria of the guideline, the analytic method was validated. It was found that Ja-ha-guh pharmacopuncture contained $211.02{\pm}7.28ug/ml$ of alanine and $372.03{\pm}7.58ug/ml$ of leucine. Conclusions Both alanine and leucine appear to be suitable standard compounds. These results are likely to contribute to further standardization of Ja-ha-guh for medical use.

Antimicrobial Activity of Pseudomonas aeruginosa BCNU 1204 and Its Active Compound (Pseudomonas aeruginosa BCNU 1204의 항균활성과 활성 물질)

  • Shin, Hwa Jin;Joo, Woo Hong
    • Journal of Life Science
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    • v.29 no.1
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    • pp.84-89
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    • 2019
  • Previous screening of novel antibacterial agents revealed that some bacterial isolates exhibited antibiotic activity against both gram-positive and gram-negative bacteria and that they showed antibacterial activity, even against methicillin-resistant Staphylococcus aureus (MRSA). Among these isolates, one bacterial strain, BCNU 1204, was identified as Pseudomonas aeruginosa using phenetic and phylogenetic analysis, based on 16S ribosomal RNA gene sequences. The maximum productivities of antimicrobial substances of BCNU 1204 were obtained after being cultured at $35^{\circ}C$ and pH 7.0 for 4 d in King's medium B (KMB). Dichloromethane (DCM) and ethylacetate (EA) extracts of P. aeruginosa BCNU 1204 exhibited strong antimicrobial activity, particularly against gram-positive bacteria. The EA extracts exhibited broad-spectrum activity against antibiotic resistant strains. Fraction 5-2, was obtained by recycling preparative liquid chromatography (LC) and preparative thin-layer chromatography (TLC) and was identified as phenazine-1-carboxylic acid belonging to phenazines using gas chromatography and mass spectrometry (GC/MS). Its minimum inhibitory concentration (MIC) values were $25{\mu}g/ml$, $50{\mu}g/ml$, ${\geq}25{\mu}g/ml$, and ${\geq}50{\mu}g/ml$ for MRSA CCARM 3089, 3090, 3091, and 3095 strains, respectively. P. aeruginosa BCNU 1204 may be a potential resource for the development of anti-MRSA antibiotics. Additional research is required to identify the active substance from P. aeruginosa BCNU 1204.

Effect of Fermented Soybean on the Proliferation and Growth in HaCaT and Fibroblast Cell (대두 발효물이 인간 유래 피부세포의 증식 및 성장에 미치는 영향)

  • Kim, Eun-Joo;Han, Myung-Ryun;Lee, So-Young;Kim, Ae-Jung
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.22 no.2
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    • pp.326-335
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    • 2021
  • This study was undertaken to determine the effect of fermented soybean extract and its fractions on skin cell proliferation and growth. The extract was procured by the pepsin and Lactobacillus rhamnosus fermentation of soybean. LC-MS analysis was performed subsequent to soybean fermentation, and cell viability was measured by the WST-1 assay. Cell proliferation was observed to increase after exposing cells to the fermented soybean extract and its fractions at all concentrations tested (0~2,000 ㎍/mL). In particular, compared to the normal control group and 120 % proliferation of the EGF (epidermal growth factor) positive control group, 160~180 % cell proliferation was achieved at 800 ㎍/ml, indicating the excellent potential as an application material for skin aging inhibition and skin cell regeneration. In addition, we also examined the effects of fermented soybean extract and its fractions on wound healing ability, in HaCaT cells and fibroblasts. Our results indicate excellent cell migration abilities after treatment with fermented soybean extract and its fractions, as compared to the control treatment. Similar cell migration abilities were observed in the positive control group (EGF). Taken together, our results indicate that fermented soybean extract and its fractions (F4 and F5) exert amelioratory effects as a natural material for skin.

A Study on the Use of Human Antibacterial Peptide LL-37-derived FK-13 as a Cosmetic Preservative (인간 항균펩타이드인 LL-37 유래의 FK-13의 화장품보존제로 활용에 대한 연구)

  • Yun, Hyo-Suk;Choe, Yong-Joon;Yang, Jae-Chan;Min, Hye-Jung
    • Journal of the Korean Applied Science and Technology
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    • v.38 no.6
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    • pp.1568-1576
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    • 2021
  • Here, we conducted the study on the possibility of using FK-13, a short analog of human-derived antibacterial peptide LL-37, as a cosmetic preservative to discover a natural cosmetic preservative that is safe for human body. For the purpose, FK-13 composed of 13 amino acids was synthesized by solid-phase peptide synthesis, and purified using reversed phase-high performance liquid chromatography (RP-HPLC). The purity and molecular weight were confirmed by liquid chromatography-mass spectrometry (LC-MS) analysis. FK-13 showed high antimicrobial activity on the three gram-positive bacteria (Staphylococcus aureus, Bacillus subtilis, and Staphylococcus epidermidis), the three gram-negative bacteria (Escherichia coli, Salmonella typhimurium, and Pseudomonas aeruginosa), and also even the fungus Candida glabrata. FK-13 had a broad spectrum of antibacterial activity, showing a suitability as a cosmetic preservative. In addition, FK-13 showed high thermostability and higher antibacterial activity in a comparative test with existing natural herbal cosmetic and chemical preservatives. Therefore, as FK-13 is a safe material and has high antibacterial activity at a low concentration, it is likely to be applied as a peptide natural cosmetic preservative that can replace existing chemical preservatives.

Polyphenol Profiling and Comparison of Extraction Solvents on Useful Component Content and Antioxidant Activity of Rhododendron micranthum Shoot (꼬리진달래 신초의 폴리페놀 프로파일링과 추출용매에 따른 유용성분 함량 및 항산화 활성 비교)

  • Jungmok Kang;Yong-Woo Park;Eun-Suk Jung;Daeho Choi
    • Korean Journal of Plant Resources
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    • v.37 no.2
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    • pp.110-119
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    • 2024
  • This study was conducted to provide information on the possibility of using Rhododendron micranthum as resource plant. Through polyphenol profiling of R. micranthum shoot extract, useful components were selected and the content of useful components and antioxidant activity by extraction solvent were compared. As a result, 37 polyphenol compounds were identified in R. micranthum shoot extract through LC-ESI-MS analysis. Contents by extraction solvent were compared of chlorogenic acid, astragalin, myricetin, and afzelin. Chlorogenic acid was highest at 6.57±0.12 mg/g in the ethanol extract, astragalin was 2.29±0.02 mg/g in the ethanol extract, myricetin was 4.77±0.06 and 4.52±0.27 mg/g in the methanol, ethanol extracts, and afzelin was highest at 0.10±0.01 mg/g in the methanol extract. Total polyphenol content of the R. micranthum shoot extract according to the extraction solvent was highest in the ethanol extract at 80.01±2.36 mg/g, and total flavonoid content was also highest in the ethanol extract at 78.08±3.44 mg/g. The IC50 value of DPPH radical scavenging activity according to the extraction solvent of R. micranthum shoot was lowest in methanol extract at 943.57±10.68 mg/L, and the IC50 value of ABTS radical scavenging activity was also lowest in methanol extract at 641.60±7.58 mg/L.