• Title/Summary/Keyword: 검출효율

Search Result 2,422, Processing Time 0.031 seconds

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
    • /
    • v.31 no.3
    • /
    • pp.186-193
    • /
    • 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.

Analytical Methods of Hydroxyl Radical Produced by TiO2 Photo-catalytic Oxidation (TiO2 광촉매 산화 반응에서 생성된 수산기 라디칼 분석 방법)

  • Kim, Seong Hee;Lee, Sang-Woo;Kim, Jeong Jin;Kim, Soon-Oh
    • Journal of the Mineralogical Society of Korea
    • /
    • v.28 no.3
    • /
    • pp.245-253
    • /
    • 2015
  • The performance of $TiO_2$ photo-catalytic oxidation process is significantly dependent on the amount of hydroxyl radicals produced during the process, and it is an essential prerequisite to quantify its production. However, precise and accurate methods for quantification of hydroxyl radicals have not been developed so far. For this reason, this study was initiated to compare existing methods for analysis of hydroxyl radicals produced by $TiO_2$ photo-catalytic oxidation and to propose a new method to overcome the limitation of established methods. To simulate $TiO_2$ photo-catalytic oxidation process, Degussa P25 which has been widely used as a standard $TiO_2$ photo-catalyst was used with the dose of 0.05 g/L. The light source of process was UVC mercury low-pressure lamp (11 W, $2,975mW/cm^2$). The results indicate that both potassium iodide (KI)/UV-vis spectrometer and terephthalic acid (TPA)/fluorescence spectrometer methods could be applied to qualitatively measure hydroxyl radicals via detection of triiodide ion ($I_3{^-}$) and 2-hydroxyterephthalic acid which are produced by reactions of iodine ion ($I^-$) and TPA with hydroxyl radicals, respectively. However, it was possible to quantitatively measure hydroxyl radicals using TPA method coupled with high-performance liquid chromatograph (HPLC). The analytical results using TPA/HPLC method show that hydroxyl radical of 0.013 M was produced after 8 hours operation of photo-catalytic oxidation under specific experimental conditions of this study. The proposed method is expected to contribute to precise the evaluation of the performance of photo-catalytic oxidation process.

Effects of Addition of Perilla Leaf Powder and Carcass Grade on the Quality and Palatability of Pork Sausage (깻잎 분말 첨가와 도체등급이 돈육소시지의 품질 및 기호성에 미치는 영향)

  • 정인철;강세주;김종기;현재석;김미숙;문윤희
    • Journal of the Korean Society of Food Science and Nutrition
    • /
    • v.32 no.3
    • /
    • pp.350-355
    • /
    • 2003
  • This study was carried out to clarify the effect of addition of perilla leaf powder (PLP) and carcass grade on the quality and palatability of pork sausage. The chemical composition, pH, calorie, water holding capacity, surface color, textural properties and amino acid composition of the samples were determined, and sensory characteristics were evaluated. Moisture and crude ash were not different among sausage of four type. Crude fat of grade B sausage was higher than that of grade E sausage, and grade B sausage added PLP was higher than grade B sausage without PLP. Crude Protein of grade E sausage was higher than that of grade B sausage. The pH of grade E sausage added PLP was highest, and calorie of grade B sausage without PLP was highest among sausage of four type. Water holding capacity of grade B added and free PLP was significantly higher than grade I sausage. The residual nitrite of sausage added PLP was significantly lower than sausage without PLP. In case of Hunter's $L^{*}$, grade B sausage and free PLP sausage were significantly higher than grade E sausage and sausage added PLP, respectively. In case of Hunter' $a^{*}$, grade E sausage and free PLP sausage were significantly higher than grade B sausage and sausage added PLP. Hunter's $b^{*}$ of sausage added PLP was higher than that of free PLP sausage. Textural properties, hardness, springiness, cohesiveness and chewiness were significantly different among sausage of four type, but gumminess of grade E added PLP was lowest among sausage of four type. Total amino acid was not significantly different among sausage of four type. Sensory color and texture of grade B sausage were superior to grade I sausage, palatability of free PLP sausage was superior.sage was superior.

Studies on Reaction Parameters for Composting of Paper Mill Sludge in a Small-Scale Reactor and Static Piles (제지슬럿지의 퇴비화를 위한 반응변수 연구)

  • Han, Shin Ho;Chung, Young Ryun;Cho, Cheon Hee;Kang, Moon Hee;Oh, Say Kyun
    • Journal of the Korea Organic Resources Recycling Association
    • /
    • v.2 no.2
    • /
    • pp.19-29
    • /
    • 1994
  • A large volume of paper mill sludge(PMS) is produced every day from paper industries after treatments of waste water and it costs too much to dispose of the sludge. Since PMS consists mostly of biodegradable organic matter, cellulose, it is desirable to recycle it by proper treatments such as composting. In this study, experiments were conducted using a small scale reactor(12l) to establish optimum conditions for efficient composting of PMS of which initial pH, C/N ratio, and moisture content were 7.1, 28~30, and 60~65%, respectively. No heavy metals such as mercury, cadmimum, and lead were not detected in the PMS. Various levels of forced aeration, 1 minute aeration per every 30, 60, 120, 240, and 480 minutes were applied and 1 minute aeration per 60 and 120 minutes found to be proper for composting of 8l PMS in this system. Relationship between $CO_2$ production and temperatures was positively correlated with r> 0.82 suggesting that the normal decomposition of PMS by microorganisms occurred. However, under the condition of aeration interval over than 240 minutes, a negative relationship between two parameters was found indicating the occurrence of abnormal(maybe anaerobic) degradation. The amount of added nitrogen also affected composting of PMS resulting in the increase of $CO_2$ production and temperature. Semi-field tests using 100kg PMS in a static pile sysem showed that PMS could be composted efficiently under optimal environmental conditions. The parameters determining efficiency of composting such as C/N ratio, aeration, moisture content, and pH need to be monitored.

  • PDF

Operator Exposure to Indoxacarb Wettable Powder and Water Dispersible Granule during Mixing/loading and Risk Assessment (Indoxacarb의 수화제 및 입상수화제 살포액 조제 시 농작업자의 노출량 측정 및 위해성 평가)

  • Kim, Eunhye;Hwang, Yon-Jin;Kim, Suhee;Lee, Hyeri;Hong, Soonsung;Park, Kyung-Hun;Kim, Jeong-Han
    • The Korean Journal of Pesticide Science
    • /
    • v.16 no.4
    • /
    • pp.343-349
    • /
    • 2012
  • Exposure and risk assessments were conducted to evaluate the relative safety of mixing/loading work of indoxacarb between wettable powder (WP) and water dispersible granule (WG). Hand exposure was monitored using cotton gloves while inhalation exposure was measured using personal air monitor. Method validation for the exposure monitoring was established successfully through several experiments. Limit of determination and limit of quantitation were 0.25 and 1 ng, respectively. $R^2$ of calibration curve linearity was more than 0.9999 and reproducibility was 0.7-6. Recovery of indoxacarb from gloves, solid sorbent and glass fiber filter at three different levels was 81.5-108.8%. Trapping efficiency and breakthrough tests gave 981.5-108.8% of recovery. During mixing/loading procedure, hand exposure amount (75 percentile of 30 repetitions) for indoxacarb WP was 6 folds (459.8 mg/kg a.i) than that of WG (81.4 mg/kg a.i). This result indicates that WG has less drift than WP thanks to its granular type of formulation. Inhalation amount was $10^{-8}-10^{-7}%$ of spray mixture prepared and $10^{-4}-10^{-3}%$ of hand exposure. In inhalation case, no significant differences were observed between two formulations. Margin of safety was calculated for risk assessment using male Korean average body weight and acceptable operator exposure level as the important exposure factors. Mixing/loading procedures for both of the formulations were considered to be of least risk because calculated MOS values were more than 1.

The analysis of pesticide residue in leafy vegetables using the modified QuEChERS pre-treatment methods (QuEChERS 시료 처리법을 활용한 엽채류 중 잔류농약분석)

  • Kim, Yang-Hyeon;Hong, Su-Myeong;Son, Kyung-Ae;Lee, Ju-Young;Min, Zaw Win;Kwon, Hye-Young;Kim, Taek-Kyum;Kyung, Kee-Sung
    • The Korean Journal of Pesticide Science
    • /
    • v.16 no.2
    • /
    • pp.121-130
    • /
    • 2012
  • In analyzing pesticide residue, LLE (liquid liquid extraction) is generally applied as one of the existing methods, but needed quite a lot of organic solvents and analytical apparatuses for the sample pre-treatment. In addition to its long analysis time and complex analytical processes, it is required to develop a more rapid and efficient method at present. In order to establish an economic and simple pesticide residue analytical method, this study carried out a comparative experiment on the existing analytical method with a new sample pre-treatment method named QuEChERS (quick, easy, cheap, effective, rugged and safe), which extracts and refines pesticide components by directly adding solid powder into the sample. Both the two analytical methods showed favorable values of correlation coefficient ($R^2$ > 0.99) of calibration curves. In terms of the detection limit (identification limit), imidacloprid showed 0.02 mg/kg, while the rest of pesticides showed a level around 0.05 mg/kg. The results of this experiment revealed that the recovery of LLE was 92.8-100.9% and the RSD was below 2.5%. On the other hand, the recovery of QuEChERS was 92.2-101.6% and RSD was below 1.9%. As a result of comparing the amount of pesticide residue by the time between the two analytical methods by using Paired t-Test, there was no significant difference between the two analytical methods as the p-value ranged from 0.3148-0.9890. Considering the results of the two methods, the QuEChERS method had similar recovery, compared to the analytical method using the existing LLE, and the analytical time was shortened by about one fourth of that of the existing method. Moreover, since it excludes the use of harmful organic solvents like dichloromethane during the process of extraction, thus leading to protecting experimenters health and remarkably reducing the amount of disused solvents, it is judged as an echo-friendly and economic analytical method.

Establishment of PCR Conditions for the Identification of Stenotrophomonas maltophilia Isolated from Boar Semen and Antimicrobial Susceptibility Patterns of the Isolates (돼지 정액에서 분리된 Stenotrophomonas maltophilia 확인을 위한 PCR 기법 개발 및 분리 균주의 항생제 감수성 양상)

  • Jung, Byeong-Yeal;Park, Bum-Soo;Kim, Ha-Young;Byun, Jae-Won;Kim, Ae-Ran;Jeon, Albert Byung-Yun;Kim, In-Cheul;Chung, Ki-Hwa
    • Journal of Life Science
    • /
    • v.22 no.8
    • /
    • pp.1114-1119
    • /
    • 2012
  • Bacteria are frequently contaminated during the collection and processing procedures of boar semen. Of the contaminants, Stenotrophomonas (S.) maltophilia is a Gram-negative bacterium that is widely distributed in a variety of habitats. Although PCR assays have been developed for the detection of S. maltophilia, they cross-react with some species of Xanthomonas. In this study, we designed a primer set for the detection of S. maltophilia in order to target the chiA (GenBank accession no. NC_010943) gene. The specific PCR products were amplified from S. maltophilia only, not from other tested strains that are frequently found in semen. The detection limit of the PCR was $1.5{\times}10^3$ CFU/ml with pure-cultured S. maltophilia and $1.5{\times}10^4$ CFU/ml with S. maltophilia spiked in semen. Twenty-six (5.9%) S. maltophilia were isolated from 440 semen samples. The PCR results exhibited 98.9% agreement with a comparison of S. maltophilia isolation. Also, the sensitivity and specificity of the PCR were 100% and 98.7%, respectively. In the antimicrobial susceptibility test, S. maltophilia isolates were highly susceptible to enrofloxacin and florfenicol, while the majority of them were resistant to amoxicillin/clavulanic acid, apramycin, ceftiofur, penicillin, and spectinomycin. These results indicated that the PCR using the chiA gene was proven to be reliable and effective for the detection of S. maltophilia with high levels of sensitivity and specificity.

Characteristics of Seaweed Salts Prepared with Seaweeds (해조소금의 제조에 관한 연구)

  • Kim, Dong-Han;Lee, Sang-Bok;Rhim, Jong-Whan
    • Korean Journal of Food Science and Technology
    • /
    • v.36 no.6
    • /
    • pp.937-942
    • /
    • 2004
  • Physicochemical properties and mineral composition of seaweed salts prepared by incineration and osmotic dehydration methods were determined. As the incineration temperature increased, yield of seaweed salts, insoluble solids, pH, alkalinity, and oxidation-reduction potential (ORP) decreased. Alkalinity of salt prepared with sea tangle was higher than that of sea mustard. ORP decreased by incineration above $700^{\circ}C$, and was lower in salt with sea tangle. As incineration temperature increased, amounts of K and Ca in seaweed salt increased, whereas that of Mg decreased. Potassium and Ca contents of seaweed salt increased remarkably compared with those of common salt. Potassium content of sea tangle salt was higher than that of sea mustard. As incineration time increased, yield of seaweed salts, insoluble solid content, and pH decreased, whereas ORP of the salt increased. Potassium content of seaweed salt with incineration time, while Ca and Na contents decreased after incineration of 8 and 4 hr, respectively. Yield of seaweed salt by osmotic dehydration increased as immersion time in sea water increased. pH of salt from sea mustard was higher than that of sea tangle. ORP of seaweed salt dried three times was -128.8 mV, significantly lower than that of salt prepared by incineration method. As sea water immersion time increased, Mg content of seaweed salt increased significantly, while Ca content decreased. Potassium content of seaweed salt was higher in sea tangle salt. In case of salt prepared by incineration of residuals, pH increased with immersion time but ORP decreased.

Method Development for the Sample Preparation and Quantitative Analysis of Synthetic Colors in Foods (식품 중 식용타르색소의 시료별 전처리방법 확립 및 함량 분석)

  • Park, Sung-Kwan;Lee, Tal-Su;Park, Seung-Kook
    • Korean Journal of Food Science and Technology
    • /
    • v.36 no.6
    • /
    • pp.893-899
    • /
    • 2004
  • Method for sample preparation and quantitative analysis of 19 permitted and non-permitted synthetic colors in foods was developed based on reversed-phase ion-pairing high performance liquid chromatography. For color extraction of samples, deionized water was added, and pH was appropriately adjusted with 1% ammonia water. Any undissolved matters were extracted with 50% ethanol or 70% methanol. Lipid in snacks was first removed using n-hexane with centrifugation, water was added to extract colors, followed by clean-up and concentration using Sep-Pak $C_{18}$ cartridge. Recovery efficiencies at known concentrations of 19 standard food colors spiked into foods were in 90.3-97.9% range far soft drink, 79.2-101.9% for candy, 84.1-103.4% for jelly, 86.4-100.8% for chewing gum, 83.5-103.4% for ice cream, and 78.5-95.6% for snack.

Development and Validation of an Analytical Method for Determination of Fungicide Benzovindiflupyr in Agricultural Commodities Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살균제 벤조빈디플루피르의 잔류시험법 개발 및 검증)

  • Lim, Seung-Hee;Do, Jung-Ah;Park, Shin-Min;Pak, Won-Min;Yoon, Ji Hye;Kim, Ji Young;Chang, Moon-Ik
    • Journal of Food Hygiene and Safety
    • /
    • v.32 no.4
    • /
    • pp.298-305
    • /
    • 2017
  • Benzovindiflupyr is a new pyrazole carboxamide fungicide that inhibits succinate dehydrogenase of mitochondrial respiratory chain. This study was carried out to develop an analytical method for the determination of benzovindiflupyr residues in agricultural commodities using LC-MS/MS. The benzovindiflupyr residues in samples were extracted by using acetonitrile, partitioned with dichloromethane, and then purified with silica solid phase extraction (SPE) cartridge. Correlation coefficient ($r^2$) of benzovindiflupyr standard solution was 0.99 over the calibration ranges ($0.001{\sim}0.5{\mu}g/mL$). Recovery tests were conducted on 5 representative agricultural commodities (mandarin, green pepper, potato, soybean, and hulled rice) to validate the analytical method. The recoveries ranged from 79.3% to 110.0% and then relative standard deviation (RSD) was less than 9.1%. Also the limit of detection (LOD) and limit of quantification (LOQ) were 0.0005 and 0.005 mg/kg, respectively. The recoveries of interlaboratory validation ranged from 83.4% to 117.3% and the coefficient of variation (CV) was 9.0%. All results were followed with Codex guideline (CAC/GL 40) and Ministry of Food and Safety guideline (MFDS, 2016). The proposed new analytical method proved to be accurate, effective, and sensitive for benzovindiflupyr determination and would be used as an official analytical method.