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Development and Validation of the Analytical Method for Oxytetracycline in Agricultural Products using QuEChERS and LC-MS/MS (QuEChERS법 및 LC-MS/MS를 이용한 농산물 중 Oxytetracycline의 잔류시험법 개발 및 검증)

  • Cho, Sung Min;Do, Jung-Ah;Lee, Han Sol;Park, Ji-Su;Shin, Hye-Sun;Jang, Dong Eun;Cho, Myong-Shik;Jung, ong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.3
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    • pp.227-234
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    • 2019
  • An analytical method was developed for the determination of oxytetracycline in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). After the samples were extracted with methanol, the extracts were adjusted to pH 4 by formic acid and sodium chloride was added to remove water. Dispersive solid phase extraction (d-SPE) cleanup was carried out using $MgSO_4$ (anhydrous magnesium sulfate), PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed with LC-MS/MS using ESI (electrospray ionization) in positive ion MRM (multiple reaction monitoring) mode. The matrix-matched calibration curves were constructed using six levels ($0.001{\sim}0.25{\mu}g/mL$) and coefficient of determination ($r^2$) was above 0.99. Recovery results at three concentrations (LOQ, $10{\times}LOQ$, and $50{\times}LOQ$, n=5) were from 80.0 to 108.2% with relative standard deviations (RSDs) less than of 11.4%. For inter-laboratory validation, the average recovery was in the range of 83.5~103.2% and the coefficient of variation (CV) was below 14.1%. All results satisfied the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for oxytetracycline determination in agricultural commodities. This study could be useful for safety management of oxytetracycline residues in agricultural products.

Development and Validation of an Analytical Method for Fungicide Fluoxastrobin Determination in Agricultural Products (농산물 중 살균제 Fluoxastrobin의 시험법 개발 및 유효성 검증)

  • So Eun, Lee;Su Jung, Lee;Sun Young, Gu;Chae Young, Park;Hye-Sun, Shin;Sung Eun, Kang;Jung Mi, Lee;Yun Mi, Chung;Gui Hyun, Jang;Guiim, Moon
    • Journal of Food Hygiene and Safety
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    • v.37 no.6
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    • pp.373-384
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    • 2022
  • Fluoxastrobin a fungicide developed from Strobilurus species mushroom extracts, can be used as an effective pesticide to control fungal diseases. In this study, we optimized the extraction and purification of fluoxastrobin according to its physical and chemical properties using the QuEChERS method and developed an LC-MS/MS-based analysis method. For extraction, we used acetonitrile as the extraction solvent, along with MgSO4 and PSA. The limit of quantitation of fluoxastrobin was 0.01 mg/kg. We used 0.01, 0.1, and 0.5 mg/kg of five representative agricultural products and treated them with fluoxastrobin. The coefficients of determination (R2) of fluoxastrobin and fluoxastrobin Z isomer were > 0.998. The average recovery rates of fluoxastrobin (n=5) and fluoxastrobin Z isomer were 75.5-100.3% and 75.0-103.9%, respectively. The relative standard deviations (RSDs) were < 5.5% and < 4.3% for fluoxastrobin and fluoxastrobin Z isomer, respectively. We also performed an interlaboratory validation at Gwangju Regional Food and Drug Administration and compared the recovery rates and RSDs obtained for fluoxastrobin and fluoxastrobin Z isomer at the external lab with our results to validate our analysis method. In the external lab, the average recovery rates and RSDs of fluoxastrobin and fluoxastrobin Z isomer at each concentration were 79.5-100.5% and 78.8-104.7% and < 18.1% and < 10.2%, respectively. In all treatment groups, the concentrations were less than those described by the 'Codex Alimentarius Commission' and the 'Standard procedure for preparing test methods for food, etc.'. Therefore, fluoxastrobin is safe for use as a pesticide.

Air Pollution and Its Effects on E.N.T. Field (대기오염과 이비인후과)

  • 박인용
    • Proceedings of the KOR-BRONCHOESO Conference
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    • 1972.03a
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    • pp.6-7
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    • 1972
  • The air pollutants can be classified into the irritant gas and the asphixation gas, and the irritant gas is closely related to the otorhinolaryngological diseases. The common irritant gases are nitrogen oxides, sulfur oxides, hydrogen carbon compounds, and the potent and irritating PAN (peroxy acyl nitrate) which is secondarily liberated from photosynthesis. Those gases adhers to the mucous membrane to result in ulceration and secondary infection due to their potent oxidizing power. 1. Sulfur dioxide gas Sulfur dioxide gas has the typical characteristics of the air pollutants. Because of its high solubility it gets easily absorbed in the respiratory tract, when the symptoms and signs by irritation become manifested initially and later the resistance in the respiratory tract brings central about pulmonary edema and respiratory paralysis of origin. Chronic exposure to the gas leads to rhinitis, pharyngitis, laryngitis, and olfactory or gustatory disturbances. 2. Carbon monoxide Toxicity of carbon monoxide is due to its deprivation of the oxygen carrying capacity of the hemoglobin. The degree of the carbon monoxide intoxication varies according to its concentration and the duration of inhalation. It starts with headache, vertigo, nausea, vomiting and tinnitus, which can progress to respiratory difficulty, muscular laxity, syncope, and coma leading to death. 3. Nitrogen dioxide Nitrogen dioxide causes respiratory disturbances by formation of methemoglobin. In acute poisoning, it can cause pulmonary congestion, pulmonary edema, bronchitis, and pneumonia due to its strong irritation on the eyes and the nose. In chronic poisoning, it causes chronic pulmonary fibrosis and pulmonary edema. 4. Ozone It has offending irritating odor, and causes dryness of na sopharyngolaryngeal mucosa, headache and depressed pulmonary function which may eventually lead to pulmonary congestion or edema. 5. Smog The most outstanding incident of the smog occurred in London from December 5 through 8, 1952, because of which the mortality of the respiratory diseases increased fourfold. The smog was thought to be due to the smoke produced by incomplete combustion and its byproduct the sulfur oxides, and the dust was thought to play the secondary role. In new sense, hazardous is the photochemical smog which is produced by combination of light energy and the hydrocarbons and oxidant in the air. The Yonsei University Institute for Environmental :pollution Research launched a project to determine the relationship between the pollution and the medical, ophthalmological and rhinopharyngological disorders. The students (469) of the "S" Technical School in the most heavily polluted area in Pusan (Uham Dong district) were compared with those (345) of "K" High School in the less polluted area. The investigated group had those with subjective symptoms twice as much as the control group, 22.6% (106) in investigated group and 11.3% (39) in the control group. Among those symptomatic students of the investigated group. There were 29 with respiratory symptoms (29%), 22 with eye symptoms (21%), 50 with stuffy nose and rhinorrhea (47%), and 5 with sore thorat (5%), which revealed that more than half the students (52%) had subjective symptoms of the rhinopharyngological aspects. Physical examination revealed that the investigated group had more number of students with signs than those of the control group by 10%, 180 (38.4%) versus 99 (28.8%). Among the preceding 180 students of the investigated group, there were 8 with eye diseases (44%), 1 with respiratory disease (0.6%), 97 with rhinitis (54%), and 74 with pharyngotonsillitis (41%) which means that 95% of them had rharygoical diseases. The preceding data revealed that the otolaryngological diseases are conspicuously outnumbered in the heavily polluted area, and that there must be very close relationship between the air pollution and the otolaryngological diseases, and the anti-pollution measure is urgently needed.

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