• Title/Summary/Keyword: Ion concentration

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Analysis of PAHs (polycyclic aromatic hydrocarbons) in Ground Coffee Using GC-tandem Mass Spectrometry and Estimation of Daily Dose (GC-tandem mass spectrometry를 이용한 분쇄원두커피 중 PAHs(polycyclic aromatic hydrocarbons) 분석법 연구 및 인체노출량 평가)

  • Jung, So-Young;Park, Ju-Sung;Son, Yeo-Joon;Choi, Su-Jeong;Lee, Yun-Jeong;Kim, Mi-Sun;Park, So-Hyun;Lee, Sang-Me;Chae, Young-Zoo
    • Korean Journal of Food Science and Technology
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    • v.43 no.5
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    • pp.544-552
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    • 2011
  • The purpose of this study was to develop an analytical method for determining 15 polycyclic aromatic hydrocarbons (PAHs) of EU priority using gas chromatography (GC)-tandem mass spectrometry (MS). The PAHs in ground coffee were analyzed after being extracted using methods such as saponification-liquid-liquid extraction, Soxhlet extraction, and solid-liquid extraction. The solid-liquid extraction method showed the greatest repeatability and most efficient reduction of the matrix effect. GC-tandem MS for the quantification of the 15 PAHs showed better resolution and lower limit of detections (LODs) than GC-MS-selected ion monitoring (SIM) and high performance liquid chromatography with fluorescence detector. LODs of this method for the ground coffee types were 0.002-0.1 ${\mu}g/kg$ and limit of quantifications (LOQs) were 0.006-0.2 ${\mu}g/kg$ The recoveries ranged from 52.6 to 93.3%. Forty-six commercial types of ground coffee were analyzed to determine their PAHs contamination levels. PAHs concentration ranged from ND to 5.988 ${\mu}g/kg$. This study was conducted with toxicity equivalence factors, the U.S. EPA recommendation to identify dietary risks for PAHs in different types of coffee. The estimated average daily dose of PAHs was $5.24{\times}10^{-8}$ mg/kg body weight/day.

Development of analytical method for determination of spinetoram residues in livestock using LC-MS/MS (LC-MS/MS를 이용한 축산물 중 Spinetoram 공정시험법 개발 및 검증)

  • Ko, Ah-Young;Kim, Heejung;Do, Jung Ah;Jang, Jin;Lee, Eun Hyang;Ju, Yun Ji;Kim, Ji Young;Chang, Moon-Ik;Rhee, Gyu-Seek
    • Analytical Science and Technology
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    • v.29 no.2
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    • pp.94-103
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    • 2016
  • An analytical method was developed to determine the amount of spinetoram (spinetoram J and spinetoram L) in livestock samples. The spinetoram was extracted with acetonitrile and purified through a primary secondary amine (PSA) sorbent. The spinetoram residues were then quantified and confirmed using a liquid chromatography–tandem mass spectrometer (LC-MS/MS) in the positive ion mode using multiple reactions monitoring (MRM). Matrix-matched calibration curves were linear over the calibration ranges (0.005-0.5 mg/kg) into a blank extract with r2 > 0.994. The limits of detection and quantification were 0.002 and 0.01 mg/kg, respectively. The recovery results of spinetram ranged between 81.9-106.4% at different concentration levels (LOQ, 10LOQ, 50LOQ, n=5) with relative standard deviations (RSDs) less than 10%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL40, 2003). An interlaboratory study was conducted to validate the method. The proposed analytical method proved to be accurate, effective, and sensitive for spinetoram determination. The method will be used as an official analytical method in Korea.

The analysis of ethylene glycol and metabolites in biological specimens (생체시료에서 에틸렌 글리콜과 그 대사체 분석에 관한 연구)

  • Park, Seh-Youn;Kim, Yu-Na;Kim, Nam-Yee
    • Analytical Science and Technology
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    • v.24 no.2
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    • pp.69-77
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    • 2011
  • Ethylene glycol (EG) is produced commercially in large amounts and is widely used as antifreeze or deicing solution for cars, boats, and aircraft. EG poisoning occurs in suicide attempts and infrequently, either intentionally through misuse or accidental as EG has a sweet taste. EG has in itself a low toxicity, but is in vivo broken down to higher toxic organic acids which are responsible for extensive cellular damage in various tissues caused principally by the metabolites glycolic acid and oxalic acid. The most conclusive analytical method of diagnosing EG poisoning is determination of EG concentration. However, victims are sometimes admitted at a late stage to hospitals or died during emergency treatment like a gastric lavage or found rotten dead, when blood EG concentrations are low or not detected. Therefore, in this study, the identification of EG was not only performed by gas chromatograpyc-mass spectrometry (GC-MS) following derivatization but also further toxicological analyses of metabolites, glycolic acid (GA) and oxalic acid (OA), were performed by ion chromatography in various biological specimens. A ranges of blood concentrations (3 cases) was $10\sim2,400\;{\mu}g/mL$ for EG, $224\sim1,164\;{\mu}g/mL$ for GA and ND $\sim40\;{\mu}g/mL$ for OA, respectively, In other biological specimens (liver, kidney, bile and pleural fluid), a range of concentrations (3 cases) was ND $\sim55,000\;{\mu}g/mL$ for EG, ND $\sim1,124\;{\mu}g/mL$ for GA and ND $\sim60\;{\mu}g/mL$ for OA, respectively. Liver and kidney tissues were recommended specimens including blood because OA, a final metabolite of EG, was identified large amounts in these despite no detectable EG caused by some therapy.

Development of Simultaneous Analytical Method for Determination of Isoxaflutole and its Metabolite (Diketonitrile) residues in Agricultural Commodities Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 Isoxaflutole과 대사산물(Diketonitrile)의 동시시험법 개발)

  • Ko, Ah-Young;Kim, Heejung;Do, Jung Ah;Jang, Jin;Lee, Eun-Hyang;Ju, Yunji;Kim, Ji Young;Chang, Moon-Ik;Rhee, Gyu-Seek
    • The Korean Journal of Pesticide Science
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    • v.20 no.2
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    • pp.93-103
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    • 2016
  • A simultaneous analytical method was developed for the determination of isoxaflutole and metabolite (diketonitrile) in agricultural commodities. Samples were extracted with 0.1% acetic acid in water/acetonitrile (2/8, v/v) and partitioned with dichloromethane to remove the interference obtained from sample extracts, adjusting pH to 2 by 1 N hydrochloric acid. The analytes were quantified and confirmed via liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive-ion mode using multiple reaction monitoring (MRM). Matrix matched calibration curves were linear over the calibration ranges ($0.02-2.0{\mu}g/mL$) for all the analytes into blank extract with $r^2$ > 0.997. For validation purposes, recovery studies were carried out at three different concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. The recoveries were ranged between 72.9 to 107.3%, with relative standard deviations (RSDs) less than 10% for all analytes. All values were consistent with the criteria ranges requested in the Codex guideline (CAC/GL40, 2003). Furthermore, inter-laboratory study was conducted to validate the method. The proposed analytical method was accurate, effective, and sensitive for isoxaflutole and diketonitrile determination in agricultural commodities.

Studies on the Bacteriophages of Brevibacterium lactofermentum (L-글루타민산 생산균 Brevibacterium lactofermentum의 Bacteriophag에 관한 연구)

  • 이태우
    • Korean Journal of Microbiology
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    • v.17 no.3
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    • pp.97-130
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    • 1979
  • Many industrial processes those employ bacteria are subjected to phage infestations. In L-glutamic acid fermentions using acetic acid, the phage infestations of the organisms have been recently recognized. In efforts to elucidate the sources of phage contamination involved in the abnormal fermentation, a series of study was conducted to isolate the phages both from the contents of abnormally fermented tanks and the soil or sewage samples from the surroundings of a fermentation factory, to define major charateristics of the phage isolates, and finally to determine the correlation between the phage isolates and temperate phages originating from the miscellaneous bacterial species isolated from the soil or sewage samples. The results are summarized as follows; 1) All phages were isolated from the irregular fermentation tanks and soil or sewage samples, and they were designated as phage PR-1, PR-2, PR-3, PR-4, PR-5, PR-6, and PR-7, in the order of isolation. These PR-series phages were proved to be highly specific for the variant strains of Br. lactofermentum only, namely, phage PR-1 and PR-2 for Br. lactofermentum No. 468-5 and phage PR-3~PR-7 for Br. lactofemrentum No. 2256. By cross-neutralization test, the 7 phagescould be subdivided into 3 groups, i. e., phage PR-I and PR-2 the first, phage PR-3, PR-4, PR-5, PR-6 the second, and the phage PR-7 the third. 2) The 7 phages were virulent under the experimental conditions. They produced plaques with clear and relatively sharp margins without distinct halo. The mean sizes of plaques were 1.5mm in diameter for phage PR-1 and PR-2, and 1. Omm for phages PR-3~PR-7. Double layer technique modified by Hongo and described by Adams, was applied to assay of the PR-series phages. The factors influencing the plaques were as follows;young age cells of host bacteria cultured for 3-6 hours represented the largest number and size, optimum was pH 7.0, incubation temperature was $30^{\circ}C$, and agar concentration and amount of overlayer medium were 0.6% and 0.2ml, respectively. 3) PR-series phages were stable in 0.05M tris buffer and 0.1M ammonium acetate buffer solution. The addition of $5{\times}10^{-3}M$ magnesium ion effectively increased the stability. Thermostability experiments indicated that PR-series phages were stable at the teinperture between $50^{\circ}{\sim}55^{\circ}C$ in nutrient medium, $45^{\circ}{\sim}50^{\circ}C$ in buffer solution. However, the phages mere completely inactivated at 603C and 65$^{\circ}$C within 10 minutes. The phages were stable at the range of pH6~9 in nutrient medium and of pH 8-9 in buffer solution, respectively. Exposure of the phages to UV for 25, 60 and 100 seconds resulted in the complete loss of infectivily, respectively. 4) Electron microscopy showed that PR-series phage particles exhibited rather similar morphology, differing in the size All of PR-series phages had a multilateral head and had a simple long tiil about three to five times long as compared with head. By the size, phage PR-1 and PR-2, PR-3, PR-4, PR-5, and PR-6 and PR-7 were classified into same groups, respectively. The head and tail size of phage PR-1, PR-5, PR-5(T) and PR-7 were 85nm, 74nm and 235nm and 350mm, and 72nm and 210nm, respectively. 5) Nucleic acids of PR-series phages were double stranded DNA. The G+C contents of phage PR-1, PR-5 and PR-7 were 56.1, 52.9 and 53.7, respectively. The values of G+C contents derived from the $T_m$ were in agreement with the chemically determined values. 6) PR-series phages effectively adsorbed on their host bacteria at the rate of more than 90% during 5 min. K value for phage PR-1, PR-5 and PR-7 were calculated to be $6{\times}10^9 ml$ per minute, respectiveky. The pH of the medium did effect adsorption rate, but both temperature and age of host cells did not. Generally, optimum adsorption condition of phages seemed to be almost same as optimum growth conditions of host bacteria. 7) In one-step growth experiments, the latent periods at $30^{\circ}C$ for PR-1, and PR-7 were about 70, 50 and 55 min, respectively. The corresponding average burst size was 200, 70 and 90, respectively. Lpsis period according to the multiplicity of infection and a phage series. In case of m. o. i. 100, strain No. 2256 (PR-5) and No. 468-5(PR-1) failed to grow and turbidity decreased after 50 and 70min, respectively. 8) In the lysate of a plaque purified phage PR-5 infected bacteria, there observed 2 types ofphage particles, i. e., phage PR-5 and PR-5 (T) of similar morphology but differing at the length of phage tail, and phage tail like particles. The phage taillike particles could be divided into 4 types by the length. Induction experiments of Br. lactofermentum with UV irradiation, mitomycin C or bacitracin treatment produced neither phage PR-5 (T) or phage tail-like particles. 9) No lysis occured when the growth of 7 strains of miscellaneous bacteria, isolated from soil and sewage samples, were inoculated with either phage PR-5 (T) or phage tail-like particles the inoculation of phage PR-5 pellet resulted in the growth inhibition of the orgainsms in the spot test. The lysates obtained from 3 miscellaneous soil derived bacteria following mitomycin C treatment the growth of Br. lactofermentum, but did not lyze the bacterium.

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Oxide perovskite crystals type ABCO4:application and growth

  • Pajaczkowska, A.
    • Proceedings of the Korea Association of Crystal Growth Conference
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    • 1996.06a
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    • pp.258-292
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    • 1996
  • In the last year great interest appears to YBCO thin films preparation on different substrate materials. Preparation of epitaxial film is a very difficult problem. There are many requirements to substrate materials that must be fullfilled. Main problems are lattice mismatch (misfit) and similarity of structure. From paper [1] or follows that difference in interatomic distances and angles of substrate and film is mire important problem than similarity of structure. In this work we present interatomic distances and angle relations between substrate materials belonging to ABCO4 group (where A-Sr or Ca, B-rare earth element, C-Al or Ga) of different orientations and YBCO thin films. There are many materials used as substrates for HTsC thin films. ABCO4 group of compounds is characterized by small dielectric constants (it is necessary for microwave applications of HTsC films), absence of twins and small misfit [2]. There most interesting compounds CaNdAlO4, SrLaAlO4 and SrLaGaO4 were investigated. All these compounds are of pseudo-perovskite structure with space group 14/mmm. This structure is very similar to structure of YBCO. SLG substrate has the lowest misfit (0.3%) and dielectric constant. For preparation of then films of substrates of this group of compound plane of <100> orientation are mainly used. Good quality films of <001> orientations are obtained [3]. In this case not only a-a misfit play role, but c-3b misfit is very important too. Sometimes, for preparation of thin films substrates of <001> and <110> orientations were manufactured [3]. Different misfits for different YBCO faces have been analyzed. It has been found that the mismatching factor for (100) face is very similar to that for (001) face so there is possibility of preparation of thin films on both orientations. SrLaAlO4(SLA) and SrLaGaO4(SLG) crystals of general formula ABCO4 have been grown by the Czochralski method. The quality of SLA and SLG crystals strongly depends on axial gradient of temperature and growth and rotation rates. High quality crystals were obtained at axial gradient of temperature near crystal-melt interface lower than 50℃/cm, growth rate 1-3 mm/h and the rotation rate changing from 10-20pm[4]. Strong anisotropy in morphology of SLA and SLG single crystals grown by the Czochralski method is clearly visible. On the basics of our considerations for ABCO4 type of the tetragonal crystals there can appear {001}, {101}, and {110} faces for ionic type model [5]. Morphology of these crystals depend on ionic-covalent character of bonding and crystal growth parameters. Point defects are observed in crystals and they are reflected in color changes (colorless, yellow, green). Point defects are detected in directions perpendicular to oxide planes and are connected with instability of oxygen position in lattice. To investigate facets formations crystals were doped with Cr3+, Er3+, Pr3+, Ba2+. Chromium greater size ion which is substituted for Al3+ clearly induces faceting. There appear easy {110} faces and SLA crystals crack even then the amount of Cr is below 0.3at.% SLG single crystals are not so sensitive to the content of chromium ions. It was also found that if {110} face appears at the beginning of growth process the crystal changes its color on the plane {110} but it happens only on the shoulder part. The projection of {110} face has a great amount of oxygen positions which can be easy defected. Pure and doped SLA and SLG crystals measured by EPR in the<110> direction show more intensive lines than in other directions which allows to suggest that the amount of oxygen defects on the {110} plane is higher. In order to find the origin of colors and their relation with the crystal stability, a set of SLA and SLG crystals were investigated using optical spectroscopy. The colored samples exhibit an absorption band stretching from the UV absorption edge of the crystal, from about 240 nm to about 550 m. In the case of colorless sample, the absorption spectrum consists of a relatively weak band in the UV region. The spectral position and intensities of absorption bands of SLA are typical for imperfection similar to color centers which may be created in most of oxide crystals by UV and X-radiation. It is pointed out that crystal growth process of polycomponent oxide crystals by Czochralski method depends on the preparation of melt and its stoichiometry, orientation of seed, gradient of temperature at crystal-melt interface, parameters of growth (rotation and pulling rate) and control of red-ox atmosphere during seeding and growth (rotation and pulling rate) and control of red-ox atmosphere during seeding and growth. Growth parameters have an influence on the morphology of crystal-melt interface, type and concentration of defects.

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The Development of Functional Seasoning Chicken Products using Natural Extracts of Green Tea and Water Soluble Mineral Ion (녹차와 기능수를 이용한 기능성 양념 계육 개발)

  • 성삼경;조영석;김은주;김수민
    • The Korean Journal of Food And Nutrition
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    • v.16 no.3
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    • pp.171-179
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    • 2003
  • In order to investigate the effects of pickle carrier on physico-chemical characteristics of seasoning chicken products, chicken were cured in seasoning containing 100 ppm germanium water, green tea, water soluble mineral and mixtures(100 ppm germanium water+green tea+water soluble mineral) after addition of 0.1% concentration to the weight of chicken. The determination of pH, salt and sugar contents were carried out, according to curing time. The salt content showed 1.11 %, 1.21 % in cured at 24 hours in control of breast and leg, irrespective of chicken parts, in which showed 19.94 brix, 18.89 brix in sugar content, respectively. These results mean that breast and leg meat added with natural extracts and functional water showed higher sugar content than that of control, in which revealed shortening of curing time by increasing penetrating velocity of salt and sugar content. Thus, salt and sugar content tended to be increased as the curing time of pickle carrier were extended in seasoning chicken after dipping in pickle containing water soluble mineral ions for 6 hours. The seasoning chicken treated with natural extracts and functional water showed a lower than that of control in hardness, irrespective of chicken parts. Overall, the seasoning chicken treated with natural extracts and functional water showed a low TBARS value and Log CFU/g, in which revealed antioxidative and antimicrobial activity. The sensory evaluations of seasoning chicken added with natural extracts and functional water containing water-soluble mineral ions were not significantly different(P<0.05). The glutamic acid among free amino acid contents showed a high in seasoning chicken treated with green tea, compared to control. This amino acid played a important role in taste of seasoning meat. The doneness appearance in seasoning chicken added with natural extracts and functional water containing water-soluble mineral ions tended to not be different, compared to those of control. These results revealed that seasoning chicken added with natural extracts and functional water containing water-soluble mineral ions would be attractive in fast food market on the basis of improvement of tenderness, shortening of curing time and uniformity of roasting appearance in seasoning chicken.

Kinetics and Mechanism of Alkalie Hydrolysis of Cinnamonitrile (II) (Cinnamonitrile의 알카리 가수분해(加水分解) 반응(反應)메카니즘 (II))

  • Sung, Nack Do;Chung, Woo Jin;Kwon, Ki Sung;Park, Byung Kwan
    • Korean Journal of Agricultural Science
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    • v.10 no.2
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    • pp.354-364
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    • 1983
  • Confonmation of (Z)-cinnamonitrile have been studied by molecular orbital theoretically using extended Huckel theory(EHT) and CNDO/2 molecular orbital calculation methods. The results indicate that the stability of conformation is(Z)-gauch>(Z)-planar. The rate constants for alkalie hydrolysis of cinnamonitrile at pH 7.0-14.0 range have been determined by ultra-violet spectrophotometry in 50% methanol at $25^{\circ}C$ and the following rate equation which can be applied over wide pH range was obtained; $${\therefore}k=({\frac{1.41{\times}10^{-14}+1.21{\times}10^7/[H_3O^+]}{2.65{\times}10^{-7}+1.64/[H_3O^+]})+9.14{\times}10^9/[H_3O^+]$$ The rate equation reveals that, at pH 7.0-10.0, the reaction is initiated by the addition of water molecule to unsaturated cabon-carhon double bond of cinnamonitrile and ${\alpha}C-{\beta}C$ bond scission follow subsequently in neutral and alkalie media. At pH 12.0-14.0, in strong alkalie solution, that so-called Michael type nucleophilic addition that the over-all rate constants is only dependent upon the concentration of hydroxide ion occurs competitively and are very complicated. Hence, the reaction mechanism of alkalie hydrolysis of cinnamonitrile which did not carefully before can be fully explained.

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Enzymatic Desugarization of Egg White for Drying with Glucose Oxidase (Glucose Oxidase에 의(依)한 건조용(乾燥用) 난백(卵白)의 효소적(酵素的) 탈당(脫糖))

  • Song, Kwang Taek;Oh, Hong Rock;Kwon, Soon Ki;Lee, Bong Duck
    • Korean Journal of Agricultural Science
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    • v.11 no.2
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    • pp.223-232
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    • 1984
  • The influences of some factors involved in removing glucose from egg white by the glucose oxidase system be fore drying were investigated. And the properties between foams prepared from raw and enzyme-treat ed egg white was compared. The results obtained we re summarized as follows; 1. The dianisidine method was found to be suitable for the measurement of egg white glucose in the range up to 100ug/ml. 2. The optimal pH of glucose oxidase activity on glucose was found to be a bout 5.0, and thats activity was most stable in the pH range of about 4.0~5.0 when that enzyme was treat ed for 30 minute at $50^{\circ}C$. 3. The optimal temperature for glucose oxidase reaction on glucose was found to be about $20^{\circ}C$, and that enzyme activity was s table up to $50^{\circ}C$. 4. The removing rate of glucose from egg white with glucose oxidase was influenced by the enzyme concentration, pH and oxygen addition, and the react ion time of the desugarization was about 10 hour sunder the conditions of 0.5% hydrogen peroxide, pH 7.0 and $26^{\circ}C$. 5. All of the each egg white treated with glucose oxidase, glucose oxidase+pancreatin, glucose oxidase+trypsin showed highly foaming ability than that of natural egg white(control), but thats foam stability, on the contrary, was reversed.

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Establishment of an Analytical Method for Determination of Fungicide Oxathiapiprolin in Agricultural Commodities using HPLC-UV Detector (HPLC-UVD를 이용한 농산물 중 살균제 Oxathiapiprolin의 잔류분석법 확립)

  • Jang, Jin;Kim, Heejung;Do, Jung Ah;Ko, Ah-Young;Lee, Eun Hyang;Ju, Yunji;Kim, Eunju;Chang, Moon-Ik;Rhee, Gyu-Seek
    • Journal of Food Hygiene and Safety
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    • v.31 no.3
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    • pp.186-193
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    • 2016
  • An analytical method was developed for the determination of oxathiapiprolin in agricultural commodities. Oxathiapiprolin is a new oomycide (fungicide of piperidinyl thiazole isoxazoline class) which controls downy mildew in cucurbits caused by Pseudoperonospora cubensis (oomycete plant pathogen). Agricultural commodities were extracted with acetonitrile and partitioned with dichloromethane to remove the interference, adjusting pH between 9 and 10 by 1 N sodium hydroxide. After purification by silica SPE cartridge to clean up the interference of organic compounds, they were finally quantified by HPLC-UVD (high performance liquid chromatograph ultraviolet detector) using a wavelength at 260 nm and confirmed by LC-MS (liquid chromatograph mass spectrometer) in electro-spray ionization positive ion mode. The standard calibration curve was linear with coefficients of determination ($r^2$) 1.00 over the calibration ranges (0.025-2.5 mg/L). Recoveries were ranged between 86.7 to 112.7%, with relative standard deviations less than 10% at three concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates. The overall results were determined and estimated according to the CODEX guidelines (CAC/GL40). The proposed method for determination of oxathiapiprolin residues in agricultural commodities can be used as an official method.