• Title/Summary/Keyword: C18

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Development and Validation of an Analytical Method for Quinoxyfen in Agricultural Products using QuEChERS and LC-MS/MS (QuEChERS법 및 LC-MS/MS를 이용한 농산물 중 살균제 Quinoxyfen의 잔류시험법 개발 및 검증)

  • Cho, Sung Min;Do, Jung-Ah;Lee, Han Sol;Park, Ji-Su;Shin, Hye-Sun;Jang, Dong Eun;Choi, Young-Nae;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.140-147
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    • 2019
  • An analytical method was developed for the determination of quinoxyfen in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with 1% acetic acid in acetonitrile and water was removed by liquid-liquid partitioning with $MgSO_4$ (anhydrous magnesium sulfate) and sodium acetate. Dispersive solid-phase extraction (d-SPE) cleanup was carried out using $MgSO_4$, PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed by using LC-MS/MS in positive mode with MRM (multiple reaction monitoring). The matrix-matched calibration curves were constructed using six levels ($0.001-0.25{\mu}g/mL$) and the coefficient of determination ($R^2$) was above 0.99. Recovery results at three concentrations (LOQ, 10 LOQ, and 50 LOQ, n=5) were in the range of 73.5-86.7% with RSDs (relative standard deviations) of less than 8.9%. For inter-laboratory validation, the average recovery was 77.2-95.4% and the CV (coefficient of variation) was below 14.5%. All results were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for quinoxyfen determination in agricultural commodities. This study could be useful for the safe management of quinoxyfen residues in agricultural products.

Development of Analytical Method for Ergot Alkaloids in Foods Using Liquid Chromatoraphy-Tandem Mass Spectrometry (LC-MS/MS를 이용한 식품 중 맥각 알칼로이드 시험법 개발)

  • Chun, So Young;Chong, Euna;Lee, Bomnae;Kwon, Jin-Wook;Park, Hye Young;Kim, Sheenhee;Gang, Giljin
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.158-169
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    • 2019
  • Ergot alkaloids are mycotoxin produced by fungi of the Claviceps genus, mainly by Claviceps purpurea in EU. Recently obtained informations indicates necessity for control the ergot in imported grains. Recent occurrence data of ergot alkaloids from EU countries indicate the necessities of management and control these toxins from the imported grains like rye, wheat, oat etc. The aim of this study is to optimize the liquid chromatography-tandem mass spectrometry method for determination of ergot alkaloids (ergometrine, ergosine, ergotamine, ergocornine, ergocryptine, ergocristine and their epimers (-inines) from grain and grain-based food. The test method was optimized by extracting the sample with acetonitrile containing 2 mM ammonium carbonate, purification with Mycosep cartridge, and instrumental analysis by LC-MS/MS using Syncronis C18 column. The standard calibration curves showed linearity with correlation coefficents; $R^2$ >0.99. Mean recoveries ranged from 72.0 to 111.3% at three different fortified levels (20, 50, and $100{\mu}g/kg$). The correlation coefficient expressed as precision was within the range of 1.9-12.9%. The limit or quantifications (LOQ) ranged from 0.012 to $0.058{\mu}g/kg$. The developed analytical method met the criteria of AOAC Int. and CAC validation parameters like accuracy and sensitivity. As a result, it was confirmed that the test method developed in this study is suitable for the simultaneous analysis of six species of ergot alkaloid from grains and grain products.

Determination and Validation of an Analytical Method for Dichlobentiazox in Agricultural Products with LC-MS/MS (LC-MS/MS를 이용한 농산물 중 Dichlobentiazox 시험법 개발 및 검증)

  • Gu, Sun Young;Lee, Han Sol;Park, Ji-Su;Lee, Su Jung;Shin, Hye-Sun;Kang, Sung Eun;Chung, Yun Mi;Choi, Ha Na;Yoon, Sang Soon;Jung, Young-Hyun;Yoon, Hae Jung
    • Korean Journal of Environmental Agriculture
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    • v.40 no.2
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    • pp.108-117
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    • 2021
  • BACKGROUND: Dichlobentiazox is a newly registered pesticide in Korea as a triazole fungicide and requires establishment of an official analysis method for the safety management. Therefore, the aim of this study was to determine the residual analysis method of dichlobentiazox for the five representative agricultural products. METHODS AND RESULTS: Three QuEChERS methods were applied to establish the extraction method, and the EN method was finally selected through the recovery test. In addition, various adsorbent agents were applied to establish the clean-up method. As a result, it was found that the recovery of the tested pesticide was reduced when using the d-SPE method with PSA and GCB, but C18 showed an excellent recovery. Therefore this method was established as the final analysis method. For the analysis, LC-MS/MS was used with consideration of the selectivity and sensitivity of the target pesticide and was operated in MRM mode. The results of the recovery test using the established analysis method and inter laboratory validation showed a valid range of 70-120%, with standard deviation and coefficient of variation of less than 3.0% and 11.6%, respectively. CONCLUSION: Dichlobentiazox could be analyzed with a modified QuEChERS method, and the method determined would be widely available to ensure the safety of residual pesticides in Korea.

Study on Characteristic of Pyropia Dentata Three Cultivar in Haenam Aquafarm, Jellanam-do (전남 해남에서 잇바디돌김 3종의 양식 특성 연구)

  • Han, M.K.;Jeong, D.S.;Kim, C.W.;Choi, S.J.
    • Journal of Practical Agriculture & Fisheries Research
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    • v.23 no.2
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    • pp.43-50
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    • 2021
  • Growth tests on the Yuldo, Supum1 and Supum2 cultivars of Pyropia dentata were performed at the Eoran and Imha aquafarm, Haenam in Jeollanamdo, from October to December in 2017. The mean water temperature ranged from 5.4 to 26.4 ℃. In Eoran aquafarm (flating raft method), dissolved total nitrogen (DTN), dissolved total phosphorus (DTP), total nitrogen (TN), total phosphorus (TP) and chemical oxygen demand (COD) ranged from 0.091 to 0.181 mg/L, 0.007 to 0.019 mg/L, 0.114 to 0.187 mg/L, 0.008 to 0.033 mg/L and 0.200 to1.000 mg/L, respectively. In Imha aquafarm (fixed pold method), DTN, DTP, TN, TP and COD ranged from 0.118 to 0.276 mg/L, 0.005 to 0.024 mg/L, 0.155 to 0.305 mg/L, 0.009 to 0.042 mg/L and 0.300 to1.400 mg/L, respectively. In order to investigate the number of conchospores attached on the Pyropia net, which was cut into about 4cm long. The mean number of conchospores of Yuldo, Supum1 and Supum2 cultivars were 39.5, 26.5, 72.5, respectively. Young thalli were harvested two times at Eoran aquafarm, and three times at Imha aquafarm. In eoran aquafarm, the mean thallus length of Yuldo, Supum1 and Supum2 cultivars were 49.9, 46.0, 42.0 cm on October and 163, 126.0, 263.0 cm on November, respectively. The mean thallus width of Yuldo, Supum1 and Supum2 cultivars were 5.8, 4.6, 11.5 cm on October and 20.9, 11.5, 14.0 cm on November, respectively. In Imha aquafarm, the mean thallus length of Yuldo, Supum1 and Supum2 cultivars were 119.0, 60.9, 71.0 cm on October, 196.0, 132.0, 262.0 cm on November and 187.0, 281.0, 296.0 cm on December, respectively. The mean thallus width of Yuldo, Supum1 and Supum2 cultivars were 4.2, 3.4, 3.1 cm on October, 8.9, 6.2, 6.6 cm on November and 11.7, 11.6, 9.4 cm on December, respectively. In eoran aquafarm, contents of moisture, crude ash, crude lipid, crude protein and carbohydrate of three cultivars ranged from 11.64 to 20.15, 19.54 to 21.19, 0.00 to 0.18, 29.78 to 37.81, 29.16 to 29.71, respectively. In Imha aquafarm, contents of moisture, crude ash, crude lipid, crude protein and carbohydrate of three cultivars ranged from 8.43 to 9.15, 11.42 to 17.49, 0.00 to 0.00, 31.90 to 37.54, 36.30 to 42.24, respectively.

Characterization of Myostatin Gene Variants in Jeju Horses (제주마에서 Myostatin 유전자 변이 특성 구명)

  • Choi, Jae-Young;Shin, Kwang-Yun;Lee, Jongan;Shin, Sang-Min;Kang, Yong-Jun;Shin, Moon-Cheol;Cho, In-Cheol;Yang, Byoung-Chul;Kim, Nam-Young
    • Journal of Life Science
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    • v.31 no.12
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    • pp.1088-1093
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    • 2021
  • Jeju horse (Equus ferus caballus) is a Korean horse breed that has been native to Jeju Island for a long time. Jeju horses are used as racehorses, and their racing ability is a major economic trait. The role of the myostatin (MSTN) gene in skeletal muscle mass has been studied in various mammals, and mutations in the MSTN gene are known to affect the racing ability and stamina of thoroughbreds. In this study, we compared the frequency of mutations in the MSTN gene in several horse breeds, including 1,433 Jeju horses. Among the mutations (ECA18 g.66493737C>T) in the MSTN gene, the long-distance aptitude genotype (TT) was found to have a frequency of 0.826 in Jeju horses, which was higher than that in Halla horses (0.285) and thoroughbreds (0.252). The genotypes and arrival records of Jeju horses were compared according to various distances (400 m, 800 m, 900 m, 1,000 m, 1,110 m, and 1,200 m). According to the results, the CT type showed a faster-reaching record than the TT type in races of less than 1,000 m. However, almost identical results were confirmed in races over 1,110 m. This study suggests that the MSTN mutation in Jeju horses may be related to race distance aptitude. In future research, the data in this study can be used for developing markers related to race distance aptitude and racing abilities in Jeju horses.

Improvement of an Analytical Method for Methoprene in Livestock Products using LC-MS/MS (LC-MS/MS를 이용한 축산물 중 살충제 메토프렌의 잔류분석법 개선)

  • Park, Eun-Ji;Kim, Nam Young;Park, So-Ra;Lee, Jung Mi;Jung, Yong Hyun;Yoon, Hae Jung
    • Journal of Food Hygiene and Safety
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    • v.37 no.3
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    • pp.136-142
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    • 2022
  • The research aims to develop a rapid and easy analytical method for methoprene using liquid chromatography-tandem mass spectrometry (LC-MS/MS). A simple, highly sensitive, and specific analytical method for the determination of methoprene in livestock products (beef, pork, chicken, milk, eggs, and fat) was developed. Methoprene was effectively extracted with 1% acetic acid in acetonitrile and acetone (1:1), followed by the addition of anhydrous magnesium sulfate (MgSO4) and anhydrous sodium acetate. Subsequently, the lipids in the livestock sample were extracted by freezing them at -20℃. The extracts were cleaned using MgSO4, primary secondary amine (PSA), and octadecyl (C18), which were then centrifuged to separate the supernatant. Nitrogen gas was used to evaporate the supernatant, which was then dissolved in methanol. The matrix-matched calibration curves were constructed using 8 levels (1, 2.5, 5, 10, 25, 50, 100, 150 ng/mL) and the coefficient of determination (R2) was above 0.9964. Average recoveries spiked at three levels (0.01, 0.1, and 0.5 mg/kg), and ranged from 79.5-105.1%, with relative standard deviations (RSDs) smaller than 14.2%, as required by the Codex guideline (CODEX CAC/GL 40). This study could be useful for residue safety management in livestock products.

Cell Migration and Wound Healing Activities of Recombinant Thymosin β-4 Expressed in Escherichia coli (재조합 Thymosin β-4의 세포이동능과 상처치유능)

  • Hong, Kyo-Chang;Choi, Yung Hyun;Kim, Gun-Do;Cha, Hee-Jae;Jeon, Sung-Jong;Nam, Soo-Wan
    • Journal of Life Science
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    • v.32 no.2
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    • pp.135-141
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    • 2022
  • Thymosin β-4 (TB4) is a small peptide composed of 43 amino acids. To obtain sufficient biologically active mouse TB4 economically, we cloned and overexpressed this gene in an Escherichia coli system. With the isopropyl β-D-1-thiogalactopyranoside induction of the E. coli transformant, TB4 fusion protein with intein- and chitin-binding domain was successfully expressed in the soluble fraction within the E. coli cell. The TB4-intein - chitin-binding domain fusion protein was purified from the soluble fraction of E. coli cell lysate. The affinity chromatography with chitin beads and dithiothreitol-mediated intein self-cleavage reaction releases the TB4 peptide into the stripping solution. Sodium dodecyl sulphate - polyacrylamide gel electrophoresis and Western blot analyses were used to confirm that the recombinant TB4 peptide was produced with the expected size of 5 kDa. We found that the recombinant TB4 stimulated cell migration in the transwell plate chamber assay. After 18 hr of the treatment of the recombinant TB4 with 1 ng/ml concentration, the migration of the HT1080 cell was increased by 20% compared with that of the chemically synthesized TB4. The recombinant TB4 was also observed to promote the healing of a wound area in C57BL/6 mice by as high as 35% compared with that of the chemically synthesized TB4. These results suggest that the recombinant TB4 has better biological activity for cell migration and wound healing than that of the chemically synthesized TB4 peptide.

Effect of Soil Temperatures on Seedling Emergence in Direct Seeding on Dry Paddy (벼 건답직파에서 파종기 지온이 출아에 미치는 영향)

  • Soh, Chang-Ho;Yun, Jin-Il;Rho, Yeong-Deok;Kim, Moo-Sung;Kwon, Shin-Han
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.40 no.5
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    • pp.580-586
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    • 1995
  • Soil temperatures at depths of 1~5cm are important to the germination and emergence of dry seeded-rice. An automated weather station was used to monitor the hourly weather parameters at Experiment Farm, Kyung Hee University from April 21 to May 30 in 1994. The data was analyzed to figure out the 24-hour temporal changes in air 1.5m above ground and soil temperatures under ground of 0, 2.5, 5, 10 and 20cm. The fluctuations of soil temperature were greatest at the soil surface and decreased with increasing depth. Mean soil temperatures at depth of 2.5cm were about 3$^{\circ}C$ higher than mean air temperatures during the observation period. Although mean soil temperatures at depth of 2.5cm during 10 or 15 days after April 21, May 1 and May 11 showed almost same temperatures, the distribution patterns of temperature regime were different from each other. Rice cultivars, Hwasung, Seohae, Nampung, IR60 and CR155, were seeded at depth of 2.5cm on April 21, May 1 and May 11, respectively. The periods of seedling emergence(PSE) varied in accordance with cultivars and seeding dates. PSE was correlated with accumulated daily mean air temperatures and accumulated hours classified by temperature regimes.

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LC-MS/MS analysis and anti-inflammatory effects of crude extract from Coptidis Rhizoma (황련 추출물의 LC-MS/MS 분석 및 항염증 효과)

  • Min-Jung, Kim;Ye-Jin, Yang;Kwang-Youn, Kim;Hun Hwan, Kim;Jae Dong, Son;Ju-Hye, Yang;Dong bin, Lee;Woo Hyun, Kim;Hu-Jang, Lee;Seon Been, Bak;Kwang-Il, Park
    • Herbal Formula Science
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    • v.31 no.1
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    • pp.1-10
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    • 2023
  • Objectives : The main aim of this study was to examine the LC-MS/MS used to identify phenolic compounds of CRE(Coptidis Rhizoma 70% EtOH Extract). Also, we investigated antioxidative activities and Anti-inflammatory activities. Methods : LC-MS/MS Analysis HPLC and LC-MS/MS were performed on a 1260 series HPLC system (Agilent Technologies, Inc., California, USA) and 3200 QTrap tandem mass system (Sciex LLC) operated in positive ion mode (spray voltage set at -4.5 kV). The solvent used was DW and Acetonitrile containing 0.1% formic acid, a gradient system was used at a flow rate of 0.5 mL/min for analysis, and a Prontosil C18 column (length, 250 mm; inner diameter, 4.6 mm; particle size, 5 ㎛; Phenomenex Co., Ltd., California, USA, Biochoff Chromatography) was used. The solvent conditions used in the mobile phases were 0-10 min at 10-15% B, 10-20 min at 20% B, 20-30 min at 25%, 30-40 min at 40%, 40-50 min at 70%, 50-60 min at 95%, and 60-70 min at 95%. The analysis was performed at a wavelength of 284 nm and a temperature of 35℃. The cell viability was measured using a 3-(4,5-dimethyethiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay and 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging activity. We examined the effects of CRE on the lipopolysaccharide (LPS)-induced production of nitric oxide (NO) in a RAW 264.7 cells Results : The chemical analysis CRE by Liquid chromatography-tandem mass spectrometry (LC-MS/MS) confirmed that Rosmarinic acid, Ferrulic acid, 3-O-feruloylquinic acid, and 5-O-feruloylquinic acid as phenolic components. DPPH radical scavenging activity was the inhibitory activity of CRE showed at 200 ㎍/mL a statistically significant level. MTT assay demonstrated that the CRE did not have a cytotoxic effect in RAW 264.7 and LPS-induced RAW264.7 cells. Also, CRE reduced NO production in RAW 264.7 cells stimulated with LPS. Conclusions : Based on these findings, The chemical analysis 4 major components CRE such as Rosmarinic acid, Ferrulic acid, 3-O-feruloylquinic acid, and 5-O-feruloylquinic acid. Moreover, we confirmed that CRE has effects antioxidant and anti-inflammatory. The results demonstrate that CRE can be used as an antioxidant and a powerful chemopreventive ingredient against inflammatory diseases.

Effects of Gibberellic Acid and Abscisic Acid on Proteolysis of Senescing Leaves from Rice Seedlings (노화 수도유묘엽의 단백질분해에 미치는 GA$_3$과 ABA의 영향)

  • Kang, S. M;Kang, N. J;Cho, J. L;Kim, Z. H;Kwon, Y. W
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.38 no.4
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    • pp.350-359
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    • 1993
  • The effect of gibberellic acid ($GA_3) and abscisic acid (ABA) on KCl-enhanced proteolysis of senescing leaves of rice(Oryza sativa L. cv. Chilsung) was studied. Emphasis was given to their effects on KCI-enhanced efflux of amino acids and proteinase activity. When treated singly, $GA_3 affected leaf proteolysis little, while ABA increased proteolysis, the rate of amino acid efflux, and ribulose -1,5 -bisphosphate carboxylase / oxygenase (Rubisco)-degrading endoproteinase activity. An additive increase in all three parameters mentioned above was observed when leaves were treated with ABA and KCl. No such an additive effect was found when $GA_3 was treated with KCl. Both $GA_3 and ABA helped to alleviate the KCI-suppressed activity of Rubisco-degrading exoproteinases. The additive increase in proteolysis of rice leaves in the presence of both ABA and KCl could thus be ascribed to a further increase in the efflux of protein hydrolyzates and Rubisco-degrading endoproteinase activity. An increase in proteolysis was accompanied by a decrease in water absorption, and the combined treatment of ABA with KCl resulted in a further reduction of water absorption.

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