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Development of an Analytical Method for Fluxapyroxad Determination in Agricultural Commodities by HPLC-UVD (HPLC-UVD를 이용한 농산물 중 Fluxapyroxad 잔류분석법 개발)

  • Kwon, Ji-Eun;Kim, HeeJung;Do, Jung-Ah;Park, Hyejin;Yoon, Ji-Young;Lee, Ji-Young;Chang, Moon-Ik;Rhee, Gyu-Seek
    • Journal of Food Hygiene and Safety
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    • v.29 no.3
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    • pp.234-240
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    • 2014
  • Fluxapyroxad is classified as carboxamide fungicide that inhibits succinate dehydrogenase in complex II of mitochondrial respiratory chain, which results in inhibition of mycelial growth within the fungus target species. This study was carried out to assure the safety of fluxapyroxad residues in agricultural products by developing an official analytical method. A new, reliable analytical method was developed and validated using High Performance liquid Chromatograph-UV/visible detector (HPLC-UVD) for the determination of fluxapyroxad residues. The fluxapyroxad residues in samples were extracted with acetonitrile, partitioned with dichloromethane, and then purified with silica solid phase extraction (SPE) cartridge. Correlation coefficient($R^2$) of fluxapyroxad standard solution was 0.9999. The method was validated using apple, pear, peanut, pepper, hulled rice, potato, and soybean spiked with fluxapyroxad at 0.05 and 0.5 mg/kg. Average recoveries were 80.6~114.0% with relative standard deviation less than 10%, and limit of detection (LOD) and limit of quantification (LOQ) were 0.01 and 0.05 mg/kg, respectively. All validation parameters were followed with Codex guideline (CAC/GL 40). LC-MS (Liquid Chromatograph-Mass Spectrometer) was also applied to confirm the analytical method. Base on these results, this method was found to be appropriate fluxapyroxad residue determination and can be used as the official method of analysis.

Study on Management of Artificial Flavors in Korea (국내 합성착향료 관리제도 설정을 위한 연구)

  • Hong Ki-Hyoung;Lee Tal-Soo;Jang Yaung-Mi;Park Sung-Kwan;Park Sung-Kug;Kwon Yong-Kwan;Jang Sun-Yaung;Han Ynun-Jeong;Won Hye-Jin;Hwang Hye-Shin;Kim Byung-Sub;Kim Eun-Jung;Kim Myung-Chul
    • Journal of Food Hygiene and Safety
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    • v.20 no.4
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    • pp.253-257
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    • 2005
  • This study was performed to develop management system of artificial flavor in Korea that considered the usage and management of artificial flavor within or outside (Europe, USA and JECFA) and to offer a yardstick for judgement and prevent from confusing when manufacture or import artificial flavoring substances. In questionnaire survey for flavoring manufacture form, ideal management system and others in companies related artificial flavor, the replier answered that artificial flavor was mainly used to drinks as water soluble from and that the countries exporting flavoring substances most frequently to Korea were Japan. Europe and America sequentially. On the basis of above results, we prepared the positive list (proposal) on about 1800 artificial flavoring substances for application to regulations in Korea Food Additives Code.

Simultaneous Analysis for Veterinary Drug Residues in Honey by HPLC/MS/MS (HPLC-MS/MS를 이용한 벌꿀 중 동물용의약품 동시분석방법 연구)

  • Kim, Jong-Hwa;Moon, Sun-Ea;Kim, Ki-Yu;Jung, You-Jung;Lee, Chang-Hee;Ku, Eun-Jung;Yoon, Mi-Hye;Lee, Jong-Bok
    • Journal of Food Hygiene and Safety
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    • v.31 no.2
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    • pp.94-98
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    • 2016
  • This study was conducted to establish the simultaneous analysis method for veterinary drug residues in honey by high performance liquid chromatography tandem mass spectrometry (HPLC/MS/MS). The eleven targeting veterinary drugs with honey test method in Korean Food Standards Codex were divided into Group 1 (streptomycine dihydrostreptomycine, neomycine) and Group 2 (oxytetracycline, enrofloxacin, ciprofloxacin, cymiazole, chloramphenicol, amitraz, coumaphos, fluvalinate) to be analyzed simultaneously. From the results, the retention time (RT) of the targeting drugs was within 15 min, the range of detection limits was 0.0056 to $0.0643{\mu}g/g$ and the range of quantification limits was 0.0169 to $0.1948{\mu}g/g$. The coefficients of determination ($R^2$) for Group 1 ($0.05{\sim}1.0{\mu}g/mL$) and Group 2 ($0.01{\sim}1.0{\mu}g/mL$) were 0.9917~0.9987 and 0.9923~1.000 respectively, and showed the good linearity. The recovery rates for Group 1 (final conc. $0.25{\mu}g/g$) and Group 2 (final conc. $1.0{\mu}g/g$) were 65.1~80.6% and 64.2~90.3% respectively. Also, the analysis results of inter day (n = 3) and intra day (n = 6) RSD (%) for area and retention time showed that the RSD (%) for area and retention time was below 10.92% and 1.57%. Therefore, the simultaneous analysis method of this study is evaluated to be a good test method for veterinary drug residues in honey.

Study on Suggestions for the Nutritional and Hygienic Standards and Guidelines for Quality Certification in Children's Preferable Food (어린이 기호식품 품질인증을 위한 영양 및 위생기준 설정에 대한 연구)

  • Yun, Jee-Hye;Cho, Sun-Duk;Kim, Seo-Young;Lee, Eun-Ju;Park, Hye-Kyung;Kim, Myung-Chul;Kim, Gun-Hee
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.37 no.5
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    • pp.589-597
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    • 2008
  • The purpose of this study is to arrange for the systematic execution of safety control in children's foods through nutrition and hygiene standard suggestions and guidelines for quality certification system in children's preferable food. Aiming to achieve this objective, the study researched the present status of children’s preferable food sold near elementary schools, elicited the hazards and problems of those foods and selected nutritional and hygienic hazard components in those foods. To suggest the standards and guidelines for quality certification in children's preferable food, the study referred to sundry records, surveyed the practical cases of relevant policies and standards at home and abroad. We studied the standard of nutrition for the quality certification in those foods for sugar, fat, sodium, and additives (tar color: red No. 2 in a ban on use, caffeine), microorganism (aflatoxin $B_1$ (${\mu}g$/kg) and pathogenic bacteria (Staphylococcus aureus, Bacillus cereus, Salmonella spp.), which are the nutrients that may hamper health when taken in a large amount, and the standard for a diet restricted to under 200 kcal per one serving size. Results of distribution of processed foods (242 samples) by nutrition standards were as follows. In case of all ‘low’ level in total sugar, total fat and sodium, 0.4% of total samples was possible to be certified, In case of all ‘medium’ level in total sugar, total fat and sodium, maximumly 22.3% of total samples was possible to be certified. In case of all medium level in nutrients and $\leq$200 kcal/serving, 17.8% of total samples was possible to be certified. Certified food types was milk products and beverages.

Development and Validation of an Analytical Method for the Insecticide Sulfoxaflor in Agricultural Commodities using HPLC-UVD (HPLC-UVD를 이용한 농산물 중 살충제 sulfoxaflor의 시험법 개발 및 검증)

  • Do, Jung-Ah;Lee, Mi-Young;Park, Hyejin;Kwon, Ji-Eun;Jang, Hyojin;Cho, Yoon-Jae;Kang, Il-Hyun;Lee, Sang-Mok;Chang, Moon-Ik;Oh, Jae-Ho;Hwang, In-Gyun
    • Korean Journal of Food Science and Technology
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    • v.45 no.2
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    • pp.148-155
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    • 2013
  • Sulfoxaflor is a new active ingredient within the sulfoximine insecticide class that acts via a unique interaction with the nicotinic receptor. The MRLs (maximun residue limit) of sulfoxaflor in apple and pear are set at 0.4 mg/kg and that in pepper is set at 0.5 mg/kg. The purpose of this study was to develop an analytical method for the determination of sulfoxaflor residues in agricultural commodities using HPLC-UVD and LC-MS. The analysis of sulfoxaflor was performed by reverse phase-HPLC using an UV detector. Acetone and methanol were used for the extraction and aminopropyl ($NH_2$) cartridge was used for the clean-up in the samples. Recovery experiments were conducted on 7 representative agricultural products to validate the analytical method. The recoveries of the proposed method ranged from 82.8% to 108.2% and relative standard deviations were less than 10%. Finally, LC-MS with selected ion monitoring was also applied to confirm the suspected residues of sulfoxaflor in agricultural commodities.

Development and Validation of an Analytical Method for Ametoctradin Residue Determination in Domestic Agricultural Commodities by HPLC-PDA (HPLC-PDA를 이용한 국내 유통 농산물 중 ametoctradin 잔류량 분석법 개발 및 검증)

  • Do, Jung-Ah;Kwon, Ji-Eun;Lee, Eun-Mi;Kim, Mi-Ra;Kuk, Ju-Hee;Cho, Yoon-Jae;Kang, Il-Hyun;Kim, Hyung-Su;Kwon, Kisung;Oh, Jae-Ho
    • Korean Journal of Food Science and Technology
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    • v.45 no.3
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    • pp.285-292
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    • 2013
  • This study was carried out to validate the safety of ametoctradin residues in agricultural commodities by developing an official analysis method. An analytical method was developed and validated using HPLC-PDA detectors. The samples were extracted with methanol, subsequently partitioned with dichloromethane and purified with florisil column chromatograph using acetone/hexane (30/70, v/v) as solvent. The method was validated by using grape, hulled rice, mandarin, and potato spiked with ametoctradin at 0.05 and 5.0 mg/kg, and pepper at 0.05 and 2.0 mg/kg. Average recoveries were 76-114.8% with relative standard deviation less than 10%, and the limit of detection and limit of quantification were 0.0125 and 0.05 mg/kg, respectively. The result of recoveries and overall coefficient of variation of the laboratory results from Gwangju regional Food and Drug Administration (FDA) and Daejeon regional FDA was accorded with Codex Alimentarius Commission Guideline (CAC/GL 40). Based on these results, this method was found to be appropriate for ametoctradin residue determination and can be used as the official method of analysis.

Fermentation Property of Chinese Cabbage Kimchi by Fermentation Temperature and Salt Concentration (발효온도 및 소금농도에 따른 배추김치의 발효 특성)

  • Chang, Moon-Jeong;Kim, Myung-Hwan
    • Applied Biological Chemistry
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    • v.43 no.1
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    • pp.7-11
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    • 2000
  • The effects of fermentation temperature$(0{\sim}l5^{\circ}C)$ and salt concentration$(1.5{\sim}4.0%)$ on the fermentation property of Chinese cabbage Kimchi were analyzed by response surface methodology. The pH decreased and acidity increased with increasing fermentation time. The reduction and increment velocities of pH and acidity were increased by increasing fermentation temperature and decreasing salt concentration. The optimum pH 4.2 was reached within $14{\sim}24$ days at $5{\sim}15^{\circ}C$, while pHs of 24 days at $0{\sim}5^{\circ}C$ were still lower value than 4.2. The effect of salt concentration more affected terminal fermentation period than initial fermentation period. The maximum edible acidity, 0.75%, was reached within 8 days at $15^{\circ}C$, while acidifies of 24 days at $0^{\circ}C$ were $0.35{\sim}0.43%$. The effects of salt concentration at $0^{\circ}C$ was higher than those at $15^{\circ}C$. The fermentation time, fermentation temperature and salt concentration were the first, second and third affecting factors on the pH and acidity of Kimchi. Based on the coefficients of determination, pH and acidity were highly fitted to the experimental data$(r^2>0.9276)$. For the suitable acidity range, $0.40{\sim}0.75%$, the edible period of Kimchi at $15^{\circ}C,\;10^{\circ}C\;and\;5^{\circ}C$ were 4 days, 10 days and 18 days at the 2.75% of salt concentration, respectively. The edible period increased from 14 days to 19 days with increased salt concentration from 1.50% to 4.00% at $5^{\circ}C$ of fermentation temperature.

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

  • Pak, Won-Min;Do, Jung-Ah;Lim, Seung-Hee;Park, Shin-Min;Yoon, Ji-Hye;Lee, Dong-seouk;Chang, Moon-Ik
    • Journal of Food Hygiene and Safety
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    • v.32 no.4
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    • pp.290-297
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    • 2017
  • The purpose of this study was developed for the determination of tridemorph in agricultural commodities samples. Tridemorph residues in samples were extracted with acetonitrile, partitioned with saline water, and then purified using and aminopropyl ($NH_2$) SPE catridge. The purified samples 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 (0.005~2.5 ng) into a blank extract with $r^2$ > 0.999. The limits of detection and quantification were 0.001 and 0.005 mg/kg, respectively. The average recovery ranged between 75.9% and 103.7% at different concentration levels (LOQ, 10 LOQ, 50 LOQ, n = 5) with relative standard deviations (RSDs) less than 9.0%. An interlaboratory study was conducted to validate the method by Korea Advanced Food Research Institute. The average recovery ranged between 87.0% and 109.2% at different concentration levels (LOQ, $10{\times}LOQ$, $50{\times}LOQ$, n = 5) with relative standard deviations (RSDs) less than 8.0%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL40, 2003) and Food Safety Evaluation Department guidelines (2016). The results prove that the developed analytical methods is accurate, effective and sensitive for tridemorph determination.

Establishment of an Analytical Method for Novobiocin in Livestock Products Using HPLC-UVD (HPLC-UVD를 이용한 축산식품 중 Novobiocin의 시험법 확립)

  • Park, Hee-Ra;Kwon, Chan-Hyeok;Lee, Jong-Goo;Kim, Hyung-Soo;Chae, Young-Sik;Oh, Jae-Ho;Kwon, Ki-Sung
    • Korean Journal of Food Science and Technology
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    • v.44 no.3
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    • pp.263-268
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    • 2012
  • Novobiocin is a coumarin-containing antibiotic, and has a longer half-life in various animals than other veterinary medicines. A simple and rapid high-performance liquid chromatography assay for the determination of residual novobiocin levels in chicken, beef and milk has been developed and validated. The separation condition for HPLC/UVD was optimized by a MG II $C_{18}$ (4.6 mm $ID{\times}250$ mm, 5 ${\mu}m$) column with 0.1% formic acid in $H_2O$/0.1% formic acid in Acetonitrile (40/60, v/v) as the mobile phase at a flow rate of 1.0 mL/min and the detection wavelength was set at 340 nm. Residues were extracted from tissue by blending with methanol. After liquid-liquid partitioning, lipid materials were removed with n-hexane and purification as Silica (1 g, 6 mL) cartridge with 10 mL acetone/dichloromethane (10/90, v/v). Limit of quantification and linearity performed by the analytical method were 0.02 mg/kg and 0.999 ($r^2$), and the recovery range was $88.8{\pm}5.6-100.3{\pm}4.4$, $88.8{\pm}7.2-97.0{\pm}3.2$ and $88.1{\pm}4.3-92.8{\pm}3.6%$. It is expected that this analytical method with regards to novobiocin in chicken, beef and milk could be applied as an official method to administer food safety on veterinary medicines.

Physicochemical properties of edible cricket (Gryllus bimaculatus) in different districts (산지별 식용 귀뚜라미의 이화학적 특성)

  • Kim, Eun-Mi;Kim, Dae-Hyun;Lim, Jeong-Ho;Chang, Yoon-Je;Lee, Yong-Hwan;Park, Jin Ju;Ahn, Mi-Young
    • Food Science and Preservation
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    • v.22 no.6
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    • pp.831-837
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    • 2015
  • Insects have gained increasing attention as an alternative protein and nutrient rich food source for humans. This study was conducted to investigate the physicochemical characteristics and harmful components of edible crickets (Gryllus bimaculatus) in the 6 districts of Yeonggwang (YG), Jeongseon (JS), Wonju (WJ), Hwaseong (HS), Geochang (GC), and Chungju (CJ). The average crude protein and crude lipid contents on a dry basis were 64.34% and 16.60%, respectively. The crude protein content of CJ was the highest (67.40%), whereas YG (59.42%) had the lowest content. On the other hand, the crude fat content of YG was the highest (20.61%), whereas CJ (14.04%) had the lowest content. The unsaturated fatty acid contents were 57.97-63.93 g/100 g of the total fatty acid content in the crickets of the 6 districts. The major fatty acids of the crickets in the 6 districts were palmitic acid, oleic acid, and linoleic acid. Among the essential amino acids, valine, leucine, and lysine were the most abundant. GC had the highest total amino acids (57.93 g/100 g), whereas YG (48.65 g/100 g) had the lowest. Major mineral contents included potassium (K, 0.92~1.01 mg/100 mg) and phosphorus (P, 0.74~0.88 mg/100 mg). The mineral composition was fairly similar among the crickets. Crickets in the 6 districts were verified to have safe levels of residual heavy metals according to the Korea Food & Drug Administration (KFDA) advisory levels.