• Title/Summary/Keyword: Mass Concentration

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Development of Analytical Method for Kasugamycin in Agricultural Products using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 Kasugamycin 시험법 개발)

  • Lee, Han Sol;Do, Jung-Ah;Park, Ji-Su;Cho, Sung Min;Shin, Hye-Sun;Jang, Dong Eun;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.3
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    • pp.235-241
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    • 2019
  • An analytical method was developed for the determination of an antibiotic fungicide, kasugamycin, in agricultural products (hulled rice, potato, soybean, mandarin and green pepper) using liquid chromatographytandem mass spectrometry (LC-MS/MS). Samples were extracted with methanol adjusted to pH 13 using 1 N sodium hydroxide, and purified with a HLB (hydrophilic lipophilic balance) cartridge. Linearity of a matrix-matched calibration curve using seven concentration levels, from 0.001 to 0.1 mg/kg, was excellent with a correlation coefficient ($R^2$) of more than 0.9998. The limits of detection (LOD) and quantification (LOQ) of instrument were 0.0005 and $0.001{\mu}g/mL$, respectively, and the LOQ of analytical method calculated as 0.01 mg/kg. The average recoveries at three spiking levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n=5) were in the range of 71.2~95.4% with relative standard deviation of less than 12.1%. The developed method was simple and all optimized results was satisfied with the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. The present study could be served as a reference for the establishment of maximum residue limits (MRL) of kasugamycin and be used as basic data for safety management relative to kasugamycin residues in imported and domestic agricultural products.

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.

Characteristics and pedigree selection of a shortened cultivation period strain in Lepista nuda (재배기간이 짧은 민자주방망이버섯 우량계통 선발 및 특성)

  • Jeon, Jong-Ock;Lee, Kwan-Woo;Lee, Kyoung-Jun;Kim, Min-Ja;Kim, In-Jae;Kim, Young-Ho
    • Journal of Mushroom
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    • v.18 no.4
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    • pp.331-338
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    • 2020
  • This study was conducted to cultivate new Lepista nuda varieties with shorter cultivation period and better fruiting body compared to that of wild strains, for mass production and commercial application. Eighteen genetic resources of L. nuda were collected and grown in boxes using rice straw-fermented growth medium. Four lines with fruiting bodies were formed and selected as cross-breeding lines. Although 657 combinations were crossed through monospore crossing, only 17 combinations were bred between the 'CBMLN-19' line and the 'CBMLN-30' line. Among them, 8 lines with fast mycelial growth and high density were selected. After inoculating the rice straw-fermented growth medium with 14 genetic resources and 8 cross-breeding lines, their incubation period was investigated. Six of the cross-breeding lines completed their incubation in 20 days, while 7 of the 14 genetic resources took more than 40 days to complete their incubation, reducing the incubation period by more than 20 days in most cross-breeding lines. After the incubations were completed, the clay loam soil was covered with for post-cultivation, and when the mycelial cultivation was complete, the formation of fruiting bodies was induced after scraping the mycelial bodies under these environmental conditions: 14℃, 95% relative humidity or higher, and 1,500 to 2,000 ppm CO2 concentration. The temperature was reduced to 6℃ at night, resulting in a low temperature shock. Thus, 4 lines of fruiting bodies occurred from two genetic resources 'CBMLN-31' and 'CBMLN-44' and two cross-bred lines 'CBMLN-96' and 'CBMLN-103'. After inoculation, the longest period for fruiting bodies to occur was 100 days for the control:, the genetic resource 'CBMLN-31', and the shortest period (45 days) was observed for the cross-breeding line 'CBMLN-103'. The result of the investigation of the fruiting body characteristics shows that the cross-bred line 'CBMLN-103' showed a small form with 1.9 g of individual weight and 123validstipes per box, which was the highest incidence among the four lines. Another cross-bred line, 'CBMLN-96', had an individual weight of 5.5 g, which is larger than that of 'CBMLN-103'; however, the number of valid stipes per box was 30 less than that of 'CBMLN-103'. Quantity analysis showed that the control, 'CBMLN-31', had the highest quantity of 783 g per box, followed by the cross-bred line, 'CBMLN-96' with 165 g per box, and then the 'CBMLN-103' with 232 g. The quantity of the two crossbred lines was lower than that of the control 'CBMLN-31'; however, the amount of fruiting bodies was higher, and the cultivation period was shortened by 32 to 33 days. Therefore, these two lines would be selected as superior lines.

Development of simultaneous analytical method for investigation of ketamine and dexmedetomidine in feed (사료 내 케타민과 덱스메데토미딘의 잔류조사를 위한 동시분석법 개발)

  • Chae, Hyun-young;Park, Hyejin;Seo, Hyung-Ju;Jang, Su-nyeong;Lee, Seung Hwa;Jeong, Min-Hee;Cho, Hyunjeong;Hong, Seong-Hee;Na, Tae Woong
    • Analytical Science and Technology
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    • v.35 no.3
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    • pp.136-142
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    • 2022
  • According to media reports, the carcasses of euthanized abandoned dogs were processed at high temperature and pressure to make powder, and then used as feed materials (meat and bone meal), raising the possibility of residuals in the feed of the anesthetic ketamine and dexmedetomidine used for euthanasia. Therefore, a simultaneous analysis method using QuEChERS combined with high-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry was developed for rapid residue analysis. The method developed in this study exhibited linearity of 0.999 and higher. Selectivity was evaluated by analyzing blank and spiked samples at the limit of quantification. The MRM chromatograms of blank samples were compared with those of spiked samples with the analyte, and there were no interferences at the respective retention times of ketamine and dexmedetomidine. The detection and quantitation limits of the instrument were 0.6 ㎍/L and 2 ㎍/L, respectively. The limit of quantitation for the method was 10 ㎍/kg. The results of the recovery test on meat and bone meal, meat meal, and pet food showed ketamine in the range of 80.48-98.63 % with less than 5.00 % RSD, and dexmedetomidine in the range of 72.75-93.00 % with less than 4.83 % RSD. As a result of collecting and analyzing six feeds, such as meat and bone meal, prepared at the time the raw material was distributed, 10.8 ㎍/kg of ketamine was detected in one sample of meat and bone meal, while dexmedetomidine was found to have a concentration below the limit of quantitation. It was confirmed that the detected sample was distributed before the safety issue was known, and thereafter, all the meat and bone meal made with the carcasses of euthanized abandoned dogs was recalled and completely discarded. To ensure the safety of the meat and bone meal, 32 samples of the meat and bone meal as well as compound feed were collected, and additional residue investigations were conducted for ketamine and dexmedetomidine. As a result of the analysis, no component was detected. However, through this investigation, it was confirmed that some animal drugs, such as anesthetics, can remain without decomposition even at high temperature and pressure; therefore, there is a need for further investigation of other potentially hazardous substances not controlled in the feed.

Effects of Shading Rate, Rooting Media and Plant Growth Regulators on Rooting of Veronoca L. by Cuttings (삽목 번식 시 차광정도, 삽목용토 및 생장조절제 처리가 꼬리풀(Veronica L.)의 발근에 미치는 영향)

  • Cheon Young, Song;Ja Young, Moon;Jung Won, Sung;Byeong Seon, Park;Jae Ik, Nam;Jeong Min, Kim
    • Journal of Practical Agriculture & Fisheries Research
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    • v.24 no.4
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    • pp.35-44
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    • 2022
  • This study was conducted to develop a mass production for a commercial use by cutting of 4 kinds of V. glabrifolia Kitag., V. pusanensis Y.N.Lee, V. glabrifolia Kitag. × V. Spicata 'Alba' and V. spicata 'Ulster Blue Dwarf' × V. longifolia. Veronica L. Effects of shade, media and concentrations of plant growth regulators on the rooting of Veronica L. were examined. The rooting rate of V. glabrifolia Kitag. was higher as a 60% than the V. pusanensis Y.N.Lee as a 20% in the control of commercial media. In shading treatment, the rooting rate was highest at 30% or 60% shading, and the 30% shading was the best in number of root and root length, but the 90% shading was lower than no shading treatment. For cutting media, the rock wool and 100% perlite increased the rooting rate by more than 10% compared to commercial media, and increased the number of roots by 2 or 3 times. However the Cocopeat of media was lower of rooting rate, root number, and root length compared to another treatment. In the plant growth regulator treatment, the rate of rooting increased in all treatment compared to control, and was highest at IBA 1,000mg·L-1 as a 82.2% and NAA 200 or 400mg·L-1 as a 82.2% or 84.4% respectively, in the V. glabrifolia Kitag. × V. Spicata 'Alba'. However, the root number and root length was decreased as the concentration of growth regulators increased.

Characterization of Sedimentation and pH Neutralization as Pretreatment of Acid Contaminated Water (산 오염수 전처리용 침전 및 중화 특성)

  • Im, Jongdo;Lee, Sangbin;Park, Jae-Woo
    • Journal of the Korean GEO-environmental Society
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    • v.23 no.9
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    • pp.33-40
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    • 2022
  • Sedimentation and pH neutralization has been investigated as preteatment of acid contaminate water. The settling and neutralizing process derive more effective degradation efficiency as the pre-treatment process before the removal process of adsorption, volatile, biodegradation, or oxidation. Settling velocity, uniformity coefficient, coefficient of curvature, and grain size index can define in the sedimentation process for characteristics of the soil. The stainless steel sieve has been used to separate each particle size of the dry soil by assembling in order of 4, 10, 20, 40, 80, 100, and 200 mesh sizes. The soil from Gamcheon Port in Busan drops upper side of the sieve and shakes back and forth to separate each different size of the particle. The 1L of Imhoff cone and 200 mL of the mass cylinder were used as settling tanks to calculate settling velocity. Stokes' equation was used to figure out the average density of dry soil with a value from settling velocity. In the results, the average particle density and lowest settling velocity were 1.93 g/cm3 and 0.11 cm/s, respectively. These values can detect the range of settling points of sediment to prevent chemical accidents. In pH neutralization, the initial pH of 2, 3, 4, and 5 of nitric acid and sulfuric acid are used as an acid solution; 0.1, 0.01, and 0.001 M of sodium hydroxide and calcium hydroxide are used as a base solution. The main goal of this experiment is to figure out the volume percentage of the acid solution becomes pH 7. The concentration of 0.001 M of base solution exceeds all the conditions, 0.01 M exceeds partially, and 0.1 M does not exceed 5 v/v% except pH 2. Calcium hydroxide present less volume than sodium hydroxide at pH neutralization both sulfuric and nitric acid.

A study on the calibration characteristics of organic fatty acids designated as new offensive odorants by cryogenic trapping-thermal desorption technique (유기지방산 신규악취물질에 대한 저온농축 열탈착방식 (Thermal desorber)의 검량특성 연구)

  • Ahn, Ji-Won;Kim, Ki-Hyun;Im, Moon-Soon;Ju, Do-Weon
    • Analytical Science and Technology
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    • v.22 no.6
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    • pp.488-497
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    • 2009
  • In this study, analytical methodology for several organic fatty acids (OFA: propionic acid (PA), butyric acid (BA), isovaleric acid (IA), and valeric acid (VA)) designated as new offensive odorants in Korea (as of year 2010) was investigated along with some odorous VOCs (styrene, toluene, xylene, methyl ethyl ketone, methyl isobutyl ketone, butyl acetate, and isobutyl alcohol). For this purpose, working standards (WS) containing all of these 13 compounds were loaded into adsorption tube filled with Tenax TA, and analyzed by gas chromatography (GC) system thermal desorber interfaced with. The analytical sensitivities of organic fatty acids expressed in terms of detection limit (both in absolute mass (ng) and concentration (ppb)) were lower by 1.5-2 times than other compounds (PA: 0.24 ng (0.16 ppb), BA: 0.19 ng (0.11 ppb), IA: 0.15 ng (0.07 ppb), and VA: 0.28 ng (0.13 ppb)). The precision of BA, IA, and VA, if assessed in terms of relative standard error (RSE), maintained above 5%, while the precison of other compounds were below 5%. The reproducibility of analysis improved with the aid of internal standard calibration (PA: $1.1{\pm}0.4%$, BA: $10{\pm}0.46$, IA; $12{\pm}0.3%$, VA: $4{\pm}0.1%$), respectively. The results of this study showed that organic fatty acid can be analyzed using adsorption tube and thermal desorber in a more reliable way to replace alkali absorption method introduced in the odor prevention law of the Korea Ministry of Environment (KMOE).

Chemical characteristics of PM2.5 fine particles collected at 1100 site of Mt. Halla during spring seasons between 1998 and 2004 (1998-2004년 봄철에 한라산 1100 고지에서 채취한 PM2.5 미세먼지의 화학 특성)

  • Kim, Won-Hyung;Kang, Chang-Hee;Hong, Sang-Bum;Ko, Hee-Jung;Lee, Won
    • Analytical Science and Technology
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    • v.20 no.5
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    • pp.383-392
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    • 2007
  • The water soluble components were analyzed in the $PM_{2.5}$ fine particles collected at the 1100 site of Mt. Halla for the spring seasons between 1998 and 2004. The $PM_{2.5}$ mass concentrations were within $13.4{\pm}9.6{\sim}21.7{\pm}20.0{\mu}g/m^3$, and the concentrations of ionic components were in the order of nss-$SO{_4}^{2-}$ > $NH{_4}{^+}$ > $NO{_3}{^-}$ > $Ca^{2+}$ > $K^+$ > $Na^+$ > $Cl^-$ > $Mg^{2+}$, in which the concentration of nss-$SO{_4}^{2-}$($3.41{\pm}2.42{\mu}g/m^3$) was the highest. The concentrations of $NH{_4}{^+}$, $SO{_4}^{2-}$, and $NO{_3}{^-}$, the secondary pollutants, were respectively 0.60~1.50, 2.86~4.42, and $0.24{\sim}1.57{\mu}g/m^3$, which had occupied 88 % of the total ionic components, on the other hand, the concentrations of marine species were less than 5 %. The nss-$SO{_4}^{2-}$ showed the high correlation with $NH{_4}{^+}$, $K^+$, so that $NH{_4}{^+}$ and nss-$SO{_4}^{2-}$ might exist in the form of $(NH_4)_3H(SO_4)_2$ and $(NH_4)_2SO_4$ in fine particles. From the backward trajectory analysis, in case of high concentrations of $NH{_4}{^+}$ and nss-$SO{_4}^{2-}$ simultaneously, the air masses were originated and stagnated at the east region of China for a while, then moved into the atmosphere of Jeju. However, in case of $NO{_3}{^-}$ and nss-$Ca^{2+}$, the air masses originated at China and Siberia were moved into Jeju via the eastern China.

Physiological and Proteomic Responses of Barley Seedlings to Salt Stress (보리의 생육초기 염 스트레스에 따른 생리적 반응과 프로테옴 변화)

  • Kim, Dea-Wook;Yun, Seong-Kun;Park, Hyoung-Ho;Hwang, Jong-Jin;Han, Ok-Kyu;Park, Tae-Il;Jung, Gun-Ho;Lee, Jae-Eun;Kim, Sun-Lim;Chung, Young-Ho
    • Journal of the Korean Society of International Agriculture
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    • v.23 no.5
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    • pp.537-545
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    • 2011
  • This study was conducted to obtain basic information on physiological and proteomic responses of barley seedlings to salt stress. Shoot dry weight decreased significantly as the level of soil salinity increased. Salt stress-induced decrease of relative shoot dry weight was lower in cv. "Sanglok" than in cv. "Sunwoo". Under the salt stress, SPAD value decreased, and the value was higher in cv. "Sanglok" than in cv. "Sunwoo". Sodium ion content in the leaves increased as NaCl concentration increased, and the content was higher in cv. "Sunwoo" than in cv. "Sanglok". The K+/Na+ ratio was higher in cv. "Sanglok" than in cv. "Sunwoo". Salt stress-induced alterations in protein expression of the leaves were detected by two dimensional electrophoresis, and 47 protein spots showing altered expression were selected. Among the selected protein spots, 17 protein spots were up-regulated and 28 spots down-regulated in cv. "Sanglok". In cv. "Sunwoo", 14 protein spots were up-regulated and 27 spots down-regulated. Out of 47 deferentially expressed protein spots, 18 protein spots were identified using mass spectrometry and NCBI protein database. Among the identified proteins, ten proteins are known to be involved in various stress responses, but the others are not directly involved in stress responses.

Analytical Method for Determination of Laccaic Acids in Foods with HPLC-PDA and Monitoring (식품 중 락카인산 성분 분리정제를 통한 분석법 확립 및 실태조사)

  • Jae Wook Shin;Hyun Ju Lee;Eunjoo Lim;Jung Bok Kim
    • Journal of Food Hygiene and Safety
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    • v.38 no.5
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    • pp.390-401
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    • 2023
  • Major components of lac coloring include laccaic acids A, B, C, and E. The Korean Food Additive Code regulates the use of lac coloring and prohibits its use in ten types of food products including natural food products. Since no commercial standards are available for laccaic acids A, B, C, and E, a standard for lac pigment itself was used to separate laccaic acids from the lac pigment molecule. A standard for each laccaic acid was then obtained by fractionation. To obtain pure lac pigment for use in food by High performance Liquid Chromatography Photo Diode Array (PDA), a C8 column yielded the best resolution among various tested columns and mobile phases. A qualitative analytical method using High Performance Liquid Chromatography (HPLC) Tandem Mass(LC-MS/MS) was developed. The conditions for fast and precise sample preparation begin with extraction using methanol and 0.3% ammonium phosphate, followed by concentration. The degree of precision observed for the analyses of ham, tomato juice and Red pepper paste was 0.3-13.1% (Relative Standard Deviation (RSD%)), degree of accuracy was 90.3-122.2% with r2=0.999 or above, and recovery rate was 91.6-114.9%. The limit of detection was 0.01-0.15 ㎍/mL, and the limits of quantitation ranged from 0.02 to 0.47 ㎍/mL. Lac pigment was not detected in 117 food products in the 10 food categories for which the use of lac pigment is banned. Multiple laccaic acids were detected in 105 food products in 6 food categories that are allowed to use lac color. Lac pigment concentrations range from 0.08 to 16.67 ㎍/mL.