• Title/Summary/Keyword: solid phase method

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Analysis of Pesticide Residues in Rice Straw for Livestock Feed (사료용 볏짚 중 잔류농약 분석)

  • Gil, Geun-Hwan;Kim, Jin-Bae;Kim, Chan-Sub;Son, Gyeong-Ae;Gwon, Hye-Yeong;Park, Jea-Eup;Lee, Kyu-Seung
    • The Korean Journal of Pesticide Science
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    • v.16 no.4
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    • pp.273-281
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    • 2012
  • This study was conducted for the establishment of the analytical method of pesticide residues in rice straw for 9 pesticides; etofenprox, tricyclazole, diazinon, edifenphos, propiconazole, carbaryl, carbofuran, 3-hydroxy carbofuran and 3-keto carbofuran and for the monitoring of these pesticides in rice straw for livestock feed in Korea. These pesticides were classified into 4 groups according to analytical instrument condition. Group 1 (HPLC-UVD1) included tricyclazole and etofenprox while group 2 (HPLC-UVD2) included propiconazole and edifenphos. Group 3 (HPLC-FLD) included carbaryl, carbofuran, 3-hydroxy carbofuran and 3-keto carbofuran. Group 4 (GC-NPD) included Diazinon. The dried rice straw samples were extracted with acetone and purified by liquid-liquid partition and solid phase extraction (SPE): Combination of Florisil SPE and amino-propyl SPE was used for group 1 and group 2, amino-propyl SPE for group 3, and Florisil SPE was for group 4. Recovery was in the ranged 70~110% and the limits of quantitation (LOQ) were lower than the half of maximum residue limits. Therefore this method was proved to be efficient for monitoring of these pesticides residue in rice straw. A total of 18 rice straw samples from 6 provinces in Korea in 2010 were analyzed using established method and, only 3-keto carbofuran was detected in one sample at concentration of 0.04 mg/kg.

Development and Validation of an Analytical Method for Fenpropimorph in Agricultural Products Using QuEChERS and LC-MS/MS (QuEChERS법과 LC-MS/MS를 이용한 농산물 중 Fenpropimorph 시험법 개발 및 검증)

  • Lee, Han Sol;Do, Jung-Ah;Park, Ji-Su;Cho, Sung Min;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.115-123
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    • 2019
  • An analytical method was developed for the determination of fenpropimorph, a morpholine fungicide, in hulled rice, potato, soybean, mandarin and green pepper using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) sample preparation and LC-MS/MS (liquid chromatography-tandem mass spectrometry). The QuEChERS extraction was performed with acetonitrile followed by addition of anhydrous magnesium sulfate and sodium chloride. After centrifugation, d-SPE (dispersive solid phase extraction) cleanup was conducted using anhydrous magnesium sulfate, primary secondary amine sorbents and graphitized carbon black. The matrix-matched calibration curves were constructed using seven concentration levels, from 0.0025 to 0.25 mg/kg, and their correlation coefficient ($R^2$) of five agricultural products were higher than 0.9899. The limits of detection (LOD) and quantification (LOQ) were 0.001 and 0.0025 mg/kg, respectively, and the limits of quantification for the analytical method were 0.01 mg/kg. Average recoveries spiked at three levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n=5) and were in the range of 90.9~110.5% with associated relative standard deviation values less than 5.7%. As a result of the inter-laboratory validation, the average recoveries between the two laboratories were 88.6~101.4% and the coefficient of variation was also below 15%. All optimized results were satisfied the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. This study could serve as a reference for safety management relative to fenpropimorph residues in imported and domestic agricultural products.

tans-Resveratrol Content of Varieties and Growth Period in Peanut (땅콩 품종 및 생육기별 trans-Resveratrol 함량)

  • Lee, Mi-Ja;Cheong, Young-Keun;Kim, Hyung-Soon;Park, Ki-Hun;Doo, Hong-Soo;Suh, Duck-Yong
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.48 no.6
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    • pp.429-433
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    • 2003
  • trans-Resveratrol(3,5,4'-trihydroxystilbene) is phenolic compound present in grapes, wines, and peanuts, has been reported to have health benefits including anticarcinogenic effects, protection against cardiovascular diseases and reduced cancer risk. A simple method for the quantitative extraction of trans-resveratrol from peanut has been developed. Optimal conditions for extraction were investigated. Type of solvent, time, and temperature assayed influenced trans-resveratrol yield. Adequate extraction condition was decided to ethanol/water (80:20v/v) maintained at $25^{\circ}C$ for 45 min. After extraction, the protocol consists of sample preparation using a $\textrm{C}_{18}$ solid-phase extraction (SPE) cartridge after concentrate with rotary evaporator and quantified by reversed phase HPLC using a $\textrm{C}_{18}$ column at 308 nm. Analytical methods for measuring trans-resveratrol in peanut were adapted to isolate, identify, and quantify trans-resveratrol in 11 peanut varieties by HPLC (high-performance liquid chromatography) with UV detector, The 11 peanut varieties content ranged from 0.018 to 1.125 $\mu\textrm{g}/\textrm{g}$ with an average of 0.289 $\mu\textrm{g}/\textrm{g}$. The contents were higher in the seeds with than without testa, regardless of varieties. The trans-resveratrol content was Higher in 110, 130 days after sowing than that of other period.

A Study on the Fixed Forms and Adsorption of Phosphorus in Citrus Orchard Soil Derived from Volcanic Ash (제주도(濟州道) 감귤원(柑橘園) 토양(土壤)의 인산형태(燐酸形態) 및 흡착(吸着)에 관(關)한 연구(硏究))

  • Kim, Hyeong-Ok
    • Applied Biological Chemistry
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    • v.17 no.3
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    • pp.219-234
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    • 1974
  • A series of experiments was conducted to study the behavior of the phosphorus added to the soils having the high phorphorus fixing capacity derived from volcanic ash in Cheju Island. Soil samples were taken from different depths of 0-10, 10-30, and 30-50cm in six citrus orchards where heavy application of phosphate fertilizer has been practised. Various forms of phosphorus were determined and phosphorus adsorption experiments were performed. The results obtained can be summarized as follows: 1. The content of inorganic phosphorus fractions determined by the method of Chang and Jackson was: water soluble P

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Soil Characteristic of Plow and Compaction Layer in Fluvio-marine Deposit Paddy Soil (하해혼성 충적층 논토양 작토층과 경반층의 토양특성)

  • Yang, Chang-Hyu;Kim, Taek-Kyum;Ryu, Jin-Hee;Kim, Jae-Duk;Jung, Kwang-Yong
    • Korean Journal of Soil Science and Fertilizer
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    • v.42 no.5
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    • pp.364-370
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    • 2009
  • This study was conducted to survey, analyze on the compaction layer and the plow layer at Jeonbug and Jisan series paddy soil, which is the representative soil in fluvio-marine and local alluvium, respectively. The depths of surface soil were 12.6 and 12.7 cm in Jeonbug and Jisan series, respectively. A plowing depth was 10.5 cm. The properties of compaction layer in two soil series were as follows. The hardness were $14.7kg\;cm^{-2}(25.3mm)$ and $8.7kg\;cm^{-2}(22.1mm)$ in Jeonbug and Jisan series, respectively. The thickness were 22.3 cm and 17.8 cm in Jeonbug and Jisan series, respectively. The depth of soil compaction, which means depth from surface, were 15 and 20 cm in Jeonbug and Jisan series, respectively. The relationship between the hardness of compaction layer and the depth of surface soil showed negative correlation, however relationship between the hardness and the thickness of compaction layer showed positive correlation. Soil temperature was lower in compaction layer than in plow layer. This temperature differences between compaction layer and plow layer were from 1.0 to $2.5^{\circ}C$ in Jeonbug series and from 0.7 to 2.1 in Jisan series. The soil physical properties of compaction layer were higher in bulk density and solid phase and lower in porosity and gaseous phase than those of plow layer in all soil series. The soil chemical properties of compaction layer were higher in pH, content of available silicate, exchangeable calcium and magnesium but lower in total nitrogen, content of organic matter and available phosphate than those of plow layer in all soil series. Cation exchangeable capacity and content of exchangeable potassium were similar between compaction layer and plow layer in Jeonbug series, however, in Jisan series these were lower in compaction layer than in plow layer. Elution amount of inorganic nitrogen were lower in compaction layer than in plow layer in all soil series. The content of soluble Fe and Mn were plenty in compaction layer compared with plow layer and these tendency was apparent in Jeonbug series. The water depth decrease were fast until the latter part of June, and were slow as $1{\sim}3mm\;day^{-1}$ for July and August, and were fast again from september. Rice roots distributions as each soil series and tillage method were 25 cm at rotary plowing in Jeonbug series, 30 cm at deep plowing in Jeonbug series, and 20 cm at tillage in Jisan series. Dry weight per m2 at heading stage were much in order of deep plowing in Jeonbug series, rotary plowing in Jeonbug series, and tillage in Jisan series.

Improvement of an Simultaneous Determination for Clenbuterol and Ractopamine in Livestock Products using LC-MS/MS (LC-MS/MS를 이용한 축산물 중 clenbuterol과 ractopamine의 동시 분석법 개선)

  • Cho, Yoon-Jae;Chae, Young-Sik;Kim, Jae-Young;Kim, Hyung-Soo;Kang, Ilhyun;Do, Jung-Ah;Oh, Jae-Ho;Kwon, Kisung;Chang, Moon-Ik
    • Korean Journal of Food Science and Technology
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    • v.45 no.1
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    • pp.25-33
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    • 2013
  • Clenbuterol and ractopamine, which are ${\beta}$-agonists, have been misused as a growth promoting agent in meat producing animals. Clenbuterol was banned for veterinary drug in Korea because of its problems regarding safety. Due to their adverse effects, such as cardiovascular and central nervous diseases on human health proper control and monitoring should be conducted. The existing analytical method of clenbuterol and ractopamine in the Food code was improved through our present study. The bovine muscle samples were subjected to enzymatic hydrolysis, extracted with ethyl acetate and defatted by hexane-methanol partitioning. A molecular imprinted polymer (MIP) solid phase extraction cartridge was used for clean-up and LC-MS/MS was operated in positive multiple reaction monitoring (MRM). Clenbuterol-$d_9$ and ractopamine-$d_3$ were used as an internal standard. The renewed method was validated according to the CODEX guideline. The limits of quantitation for clenbuterol and ractopamine were 0.2 and 0.5 ${\mu}g/kg$, respectively. The mean recoveries ranged in 104.2-113.5% for clenbuterol and in 107.6-118.1% for ractopamine. The improved method was able to save both time and expenses.

A study of relationship between stomach cancer and selenoproteins in Korean human blood serum (한국인 혈청에서의 셀레노 단백질과 위암과의 상관관계 연구)

  • Park, Myungsun;Pak, Yong-Nam
    • Analytical Science and Technology
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    • v.28 no.6
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    • pp.417-424
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    • 2015
  • In this study, the relationship between selenoprotein concentrations in blood and stomach cancer have been searched for Korean. The concentration of each selenoprotein in blood serum was analyzed and the correlation between the concentration and stomach cancer was studied to find a potential for using Selenium as a biomarker. In concentration determination, a simple calibration curve method was used with the monitoring of m/z 78 without the use of solid phase extraction. This is a lot more simple than the method using SPE with post column isotope dilution. The result obtained from the analysis of CRM BCR-637, 72.20±3.35 ng·g−1, showed similar value of reference value (81±7 ng·g−1). The total concentration of Se for the controlled group, cardiovascular patients group, was 105.70±21.20 ng·g−1. This value was the same as normal healthy person reported earlier. Each selenoprotein concentration of GPx, SelP and SeAlb was 26.12±7.84, 65.15±14.50, 14.43±6.99 ng·g−1, respectively. The distribution of each selenoprotein was 24.7%, 61.6%, and 13.7%, which was similar to the normal person. The result of stomach cancer patients, the total concentration of Se was 76.11±28.12 ng·g−1 and each concentration of GPx, SelP and SeAlb was 15.41±9.01, 50.83±17.91, and 9.87±5.21 ng·g−1, respectively. The total and each selenoprotein concentration level showed significant decrease for the stomach cancer patients. The level of decrease was 41.0% for GPx, 22.0% for SelP, and 31.6% for SeAlb. However, the distribution of each selenoprotein was not much different. Either total Selenium or each selenoprotein could be used as a possible index for the diagnosis of cancer. However, in age group study, it is shown that young age group (30's-40's) did not show much difference.

Determination of homogentisic acid in human plasma by GC-MS for diagnosis of alkaptonuria (GC-MS를 이용한 혈장 중 호모겐티식산의 분석;알캅톤뇨증의 진단)

  • Thapa, Maheshwor;Yu, Jundong;Lee, Wonjae;Islam, Fokhrul;Yoon, Hye-Ran
    • Analytical Science and Technology
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    • v.28 no.5
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    • pp.323-330
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    • 2015
  • Alkaptonuria, a rare inherited metabolic disease, is characterized by a lack of homogentisate dioxygenase and accumulation of homogentisic acid (HGA), leading to homogentisic aciduria, arthritis, and ochronosis. In this study, a rapid analytical method, without an expensive and tedious solid phase extraction step, was developed to quantify HGA in plasma using GC-MS. HGA-spiked pooled plasma samples were subjected to liquid-liquid extraction (LLE) with ethyl acetate, followed by trimethylsilyl derivatization (TMS) and GC-MS quantification using selected ion monitoring. The formation of TMS derivative of the 1 carboxylic and 2 hydroxyl functional groups was performed by reacting BSTFA (with 10% TMCS) for 5 min at 80 ℃. For selected ion monitoring, quantification and confirmation ions were determined based on specific ions (m/z 384, m/z 341 and m/z 252) of the TMS derivative of HGA. Calibration curves of pooled normal plasma specimens showed a linear relationship in the range of 1-100 ng/µL. The precision and accuracy were within a relative standard deviation (RSD) of 1 to 15% and a bias of -5 to 25%. Recoveries were obtained in the range of 99-125% and 95-115% for intra-day and inter-day assay, respectively, at 2, 20 and 80 ng/µL. The limit of detection (LOD) and limit of quantification (LOQ) were 0.4 ng/µL and 4 ng/µL, respectively. No homogentisic acid was excreted from normal Korean plasma samples. Collectively, the results from the present study suggest that this method could be useful for routine diagnosis and therapeutic monitoring of alkaptonuria patients with excellent sensitivity and rapidity.

Study on Iron-making and Manufacturing Technology of Iron Swords with Ring Pommel Excavated in Ipbuk-dong, Suwon (수원 입북동 출토 철제환두도의 제철과 제작기술 연구)

  • Kim, Soo-Ki
    • Journal of Conservation Science
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    • v.32 no.4
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    • pp.579-588
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    • 2016
  • This study analyzed nonmetallic inclusions in iron swords with a ring pommel excavated in the Ipbuk-dong, Suwon. Scanning electron microscopy with energy dispersive spectroscopy(SEM-EDS) was used to estimate the iron-making temperature, and we compared the oxide with $SiO_2$ to investigate the heat-treatment technology in the production of iron swords with a ring pommel by investigating the artificial insertion of a slag former and the metallurgical structure. From the wustite observed in most of the specimens, it is judged that these swords were produced by heating and forging iron smelted at a low temperature using the solid reduction method. In addition, judging from the partial presence of $P_2O_5$, it is assumed that they were smelted directly with natural ore, not calcined. From the ratios of $CaO/SiO_2$ and $TiO_2/SiO_2$, it is judged that the raw material for iron-making was iron ore and that a calcareous slag former was not artificially inserted. The structure of the blade part on the front end was pure iron. From the high carbon content of the blade part on the ring pommel and the formation of a martensitic structure and pearlite colony, it is judged that they were tempered after carburizing and that the back, handle part, and ring pommel were unintentionally carburized. Judging from the structure of these specimens, it was noted that they were produced by applying artificial partial heat-treatment technology. This study attempted to present a more scientific analysis by using the method of interpretation through component analysis of nonmetallic inclusions appearing in one relic by the ratio of the oxide divided by $SiO_2$. It is judged that reinterpreting the arguments by the results of the existing analysis and research in this way can obtain different interpretations.

Evaluation of the Potential of Nitrogen Plasma to Cosmetics (질소 플라즈마의 화장품 가능성 평가)

  • Lee, So Min;Jung, So Young;Brito, Sofia;Heo, Hyojin;Cha, Byungsun;Lei, Lei;Lee, Sang Hun;Lee, Mi-Gi;Bin, Bum-Ho;Kwak, Byeong-Mun
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.48 no.3
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    • pp.189-196
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    • 2022
  • Plasma refers to an ionized gas that is often referred to as "the fourth phase of matter", following solid, liquid, and gas. Plasma has traditionally been utilized for industrial applications such as welding and neon signs, but its promise in biomedical fields such as cancer treatment and dermatology has lately been recognized. Indeed, due to its beneficial effects in promoting collagen production, improving skin tone, and eliminating harmful bacteria in the skin, plasma treatment constitutes an important target for dermatological research. In this study, a plasma device for cosmetic manufacturing based on nitrogen, the main component of the atmosphere, was designed and assembled. Moreover, nitric oxide (NO) was selected since is easier to follow and evaluate than other nitrogen plasma active species, and its contents were measured to perform a quantitative and qualitative evaluation of plasma. First, an injection method, using different proximities labeled "sinking" and "non sinking" treatments, was performed to test the most efficient plasma treatment method. As a result, it was observed that the formulation obtained by a non sinking treatment was more effective. Furthermore, toner and ampoule were selected as cosmetics formulations, and the characteristics of the formulation and changes in the injected plasma state were observed. In both formulations, the successful injection of NO plasma was 2 times higher in toner formulation than ampoule formulation, and it gradually decreased with time, having dissipated after a week. It was confirmed that the nitrogen plasma used did not affect the stability of the toner and ampoule formulations at low temperature (4 ℃), room temperature (25 ℃), and high temperature (37 ℃ and 50 ℃) conditions. The results of this study demonstrate the potential of plasma cosmetics and highlight the importance of securing the stability of the injected plasma.