• Korean Journal of Environmental Agriculture
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• v.32 no.1
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• pp.70-77
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• 2013

BACKGROUND: Nitroxoline is an antibiotic agent. It is used for the treatment of the second bacterial infection by the colibacillosis, salmonellosis and viral disease of the poultry. When the nitroxoline is indiscreetly used, the problem about the abuse of the antibiotics can occur. Therefore, this study presented the residue analytical method of nitroxoline in food for the safety management of animal farming products. METHODS AND RESULTS: A simple, sensitive and specific method for nitroxoline in chicken muscle by high performance liquid chromatograph with PDA was developed. Sample extraction with acetonitrile, purification with SPE cartridge (MCX) were applied, then quantitation by HPLC with C18 column under the gradient condition with 0.1 % tetrabutylammonium hydroxide-phosphoric acid and methanol was performed. Standard calibration curve presented linearity with the correlation coefficient ($r^2$) > 0.999, analysed from 0.02 to 0.5 mg/L concentration. Limit of quantitation in chicken muscle showed 0.02 mg/kg, and average recoveries ranged from 72.9 to 88.1 % in chicken muscle. The repeatability of measurements expressed as coefficient of variation (CV %) was less than 12 % in 0.02 and 0.04 mg/kg. CONCLUSION(S): Newly developed method for nitroxoline in chicken muscle was applicable to food inspection with the acceptable level of sensitivity, repeatability and reproducibility.

• Journal of Food Hygiene and Safety
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• v.31 no.5
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• pp.327-334
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• 2016

This study was conducted to establish the standard method for the contents of biotin in milk formulas. To optimize the method, we compared several conditions for liquid extraction, purification and instrumental measurement using spiked samples and certified reference material (NIST SRM 1849a) as test materials. LC-MS/MS method for biotin was established using $C_{18}$ column and binary gradient 0.1% formic acid/acetonitrile, 0.1% formic acid/water mobile phase is applied for biotin. Product-ion traces at m/z 245.1 ${\rightarrow}$ 227.1, 166.1 are used for quantitative analysis of biotin. The linearity was over $R^2=0.999$ in range of $5{\sim}60{\mu}g/L$. For purification, chloroform was used as a solvent for eliminating lipids in milk formula. The linearity was over 0.999 in range of 5~60 ng/mL. The detection limit and quantification limit were 0.10, 0.31 ng/mL. The accuracy and precision of LC-MS/MS method using CRM were 103%, 2.5% respectively. Optimized methods were applied in sample analysis to verify the reliability. All the tested milk formulas were acceptable contents of biotin compared with component specification and standards for nutrition labeling. The standard operating procedures were prepared for biotin to provide experimental information and to strengthen the management of nutrient in milk formula.

• Journal of the Korean Society of Food Science and Nutrition
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• v.40 no.6
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• pp.903-911
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• 2011

In this study, Bacillus polyfermenticus CJ6 harboring antibacterial activity was isolated from meju. The antibacterial activity of Bacillus polyfermenticus CJ6 was stable in the pH range of 3.0~9.0, but it disappeared after culture at $70^{\circ}C$ for 24 hr. Antibacterial activity was inactivated by proteinase K, protease, and ${\alpha}$-chymotrypsin, indicating its proteinaceous nature. The growth inhibitory effects of B. polyfermenticus CJ6 culture on food-borne pathogens such as Staphylococcus aureus, Salmonella Typhi, Listeria monocytogenes, and Escherichia coli O157:H7 were examined in this study. Approximately 6~6.2 log CFU/mL of each pathogen was co-cultured with B. polyfermenticus CJ6 in a 50 mL culture volume for 24 hr. Growth of S. aureus and L. monocytogenes was completely inhibited after 3 hr of incubation. Growth of S. Typhi and E. coli O157:H7 was also completely inhibited after 6 hr of incubation. The antibacterial compounds from B. polyfermenticus CJ6 were purified by solid phase extraction (C18 Sep-pak cartridge), recycling preparative HPLC, and analytical HPLC. Ultra-high performance liquid chromatography and electrospray ionization tandem mass spectrometry analysis were used to identify the purified antibacterial compounds, which were confirmed to be five peptides (757.4153 Da, 750.3444 Da, 1024.5282 Da, 1123.6083 Da, and 1617.8170 Da).

• Journal of Food Hygiene and Safety
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• v.32 no.3
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• pp.187-192
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• 2017

The consumption of herbal medicines has been increasing with growing interest in health. However, due to recent climate change and the complex distribution process of herbal medicines with high import dependence the likelihood of contamination with mycotoxin has been increased. Mycotoxins are emerging as key indicators for ensuring safety of herbal medicines. A total of 498 herbal medicine samples were screened for mycotoxin contamination in this study. Aflatoxin in the herbal medicine samples was extracted by using immunoaffinity column, then the extracted aflatoxin was quantified via high performance liquid chromatography coupled with fluorescence detection (HPLC-FLD) method. The extraction method was verified by linearity, recovery, LOD and LOQ. Aflatoxins were detected in 39/498 samples in an average of $7.670{\mu}g/kg$ ($0.610-77.452{\mu}g/kg$ range). Although safety standards for Corydalis Tuber is not currently available in korea, five of the 39 samples had high concentration of aflatoxins (average of $14.9{\pm}4.1{\mu}g/kg$). In conclusion, it is urgent to establish safety criteria of aflatoxin in Corydalis Tuber. The results of the current study suggest that continuous monitoring is necessary for proactive management of herbal medicine safety.

• Journal of the Korean Applied Science and Technology
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• v.29 no.3
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• pp.486-494
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• 2012

Nano-emulsion with phase inversion temperature (PIT) emulsifying system was prepared to use rapeseed oil from originating Jeju in order to apply various cosmetic applications. Natural rape seed oil (NRSO) extraction was extracted using n-hexane as a solvent. NRSO extract showed a light yellowish color of viscous liquid as well as yield was $43{\pm}2.5%$. Acid value was $2.76{\pm}0.5$ and gravity was $0.89{\pm}0.05$. Droplet size of PIT-Yuche-NE with 20wt% of rapeseed oil was 50-120nm (average: $82{\pm}5.8nm$) and zeta potential was -29.5mV. It was thermodynamically good stable emulsion due to $(PEG)_{5-30}$fattyacidether. Some conclusions from the result of characteristic experiment were obtained as follows. First, the anti-oxidative activity was measured by free radical scavenging activity using DPPH (1,1-diphenyl-2-picrylhydrazyl radical). Anti-oxidative activity of PIT-Yuche-NE was $37.2{\pm}6.7%$ on 10mg/mL compared with PIT-Toco-NE (Natural tocopherol nano-emulsion, $28.8{\pm}6.5%$ on 10 mg/mL) and PIT-Nokcha-NE (Green tea extract nano-emulsion, $29.6{\pm}7.2%$ on 10mg/mL). Second, the collagen synthesis activity of PIT-Yuche-NE was $148{\pm}15.2%$ compared with PIT-Toco-NE (Natural tocopherol nano-emulsion, $121{\pm}13.5%$ on 10mg/mL) and PIT-Nokcha-NE (Green tea extract nano-emulsion, $95{\pm}12.7%$ on 10mg/mL). Third, the effectiveness of moisturizing activity of Yuche-CRM with Aramo-TS after 6 hours increase $47{\pm}3.9%$ (*p-value￡0.05, n=7) whereas Both Toco-CRM was $30{\pm}5.2%$ (*p-value￡0.05, n=7) and Nokcha-CRM was $35{\pm}4.5%$. Therefore, Yuche-CRM has higher moisturizing effect than other two creams. Finally, Nano-emulsion stabilizing rapeseed oil using PIT emulsifying system of this study can be used to apply cosmetics industry and pharmaceutical industry.

• The Korean Journal of Pesticide Science
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• v.21 no.1
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• pp.68-74
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• 2017

An analytical method for detecting metamifop residue in paddy water, soil, and rice with high performance liquid chromatography (HPLC) was developed. Water was extracted with ethyl acetate before analyzing by HPLC. Soil residues were extracted with acetone under acidic condition and after purifying with $Extrelut^{(R)}$ NT, and silica SPE, the residue was analyzed by HPLC. For residue analysis in rice, the procedure involved extraction with acetone, purification with $Extrelut^{(R)}$ NT, partitioning between acetonitrile/hexane, purification with silica SPE cartridge, and analysis by HPLC. The limit of detection (LOD) was 1.0 ng, limit of quantitation (LOQ) was 3.0 ng, and method limit of quantitation (MLOQ) were 0.001 mg/L for paddy water, 0.01 mg/kg for rice and soil, respectively. Standard calibration curve shows linearity from 0.05 mg/kg to 5.0 mg/kg ($R^2=0.9999$). The recoveries in fortified paddy water were $91.3{\pm}3.5%$ (0.01 mg/L level) and $93.2{\pm}6.3%$ (0.05 mg/L level). The recoveries in fortified paddy soils were $92.5{\pm}4.0%$ (0.1 mg/kg level) and $92.7{\pm}4.0%$ (0.5 mg/kg level) in soil A, while, $102.3{\pm}4.4%$ (0.1 mg/kg level) and $98.9{\pm}7.9%$ (0.5 mg/kg level) in soil B, respectively. The recoveries in fortified rice were $93.0{\pm}6.9%$ (0.1 mg/kg level) and $85.0{\pm}3.5%$ (0.5 mg/kg level). This method was proved to be effective and can be used to determine the metamifop residue in paddy water, paddy soil, and rice.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.40 no.2
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• pp.203-214
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• 2014

We measured the contact dermatitis-causing substances concentrations in 28 commercial oxidative hair-coloring products. This study was aimed to provide the fundamental data about oxidative hair-coloring products. We selected 10 oxidation dyes (p-phenylenediamine, toluene-2,5-diamine, m-phenylenediamine, nitro-p-phenylenediamine, p-aminophenol, m-aminophenol, o-aminophenol, p-methylaminophenol, N,N'-bis(2-hydroxyethyl)-p-phenylenediamine sulfate, 2-methyl-5-hydroxyethylaminophenol) and 4 heavy metal (nikel; Ni, chromium; Cr, cobalt; Co, copper; Cu) as contact dermatitis-causing substances. To identify 10 oxidation dyes, hexane-2% sodium sulfite was used for the rapid and simple extraction and ultra performance liquid chromatography (UPLC) analysis was used for simultaneous analysis in 12 minutes. 10 oxidative dyes were detected as indicated on the product packaging and each concentration was lower than prescribed upper concentration limit by pharmaceutical manufacturing standards. And we analysed inductively coupled plasma-optical emission spectrophotometer (ICP-OES) for content search of heavy metal after microwave digestion. The heavy metal average concentration in oxidative hair-coloring products was 0.572 ${\mu}g/g$ for Ni, 3.161 ${\mu}g/g$ for Cr, 2.029 ${\mu}g/g$ for Co, 0.420 ${\mu}g/g$ for Cu, respectively. The average of concentration in powder type (henna) was higher than those of other foam and cream type oxidative hair-coloring products as follows; 1.800 ${\mu}g/g$ for Ni, 10.127 ${\mu}g/g$ for Cr, 7.082 ${\mu}g/g$ for Co, 1.451 ${\mu}g/g$ for Cu. Hair coloring products were classified into the six colors - black, dark brown, brown, dark brown, light brown, red brown and analyzed. Brown color had the highest average concentration of Co and the others had the highest average concentration of Cr.

• Journal of Food Hygiene and Safety
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• v.26 no.2
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• pp.142-149
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• 2011

An isocratic high performance liquid chromatography (HPLC) method for routine analysis of deoxynivalenol in noodles was validated and estimated the measurement uncertainty. Noodles (dried noodle and ramyeon) were analyzed by HPLC-ultraviolet detection using immunoaffinity column for clean-up. The limits of detection (LOD) and quantification (LOQ) were 7.5 ${\mu}g$/kg and 18.8 ${\mu}g$/kg, respectively. The calibration curve showed a good linearity, with correlation coefficients $r^2$ of 0.9999 in the concentration range from 20 to 500 ${\mu}g$/kg. Recoveries and Repeatabilities expressed as coefficients of variation (CV) spiked with 200 and 500 ${\mu}g$/kg were $82{\pm}2.7%$ and $87{\pm}1.3%$% in dried noodle, and $97{\pm}1.6%$ and $91{\pm}12.0%$ in ramyeon, respectively. The uncertainty sources in measurement process were identified as sample weight, final volume, and sample concentration in extraction volume as well as components such as standard stock solution, working standard solution, 5 standard solutions, calibration curve, matrix, and instrument. Deoxynivalenol concentration and expanded uncertainty in two matrixes spiked with 200 ${\mu}g$/kg and 500 ${\mu}g$/kg were estimated to be $163.8{\pm}52.1$ and $435.2{\pm}91.6\;{\mu}g$/kg for dried noodle, and $194.3{\pm}33.0$ and $453.2{\pm}91.1\;{\mu}g$/kg for ramyeon using a coverage factor of two which gives a level of statistical confidence with approximately 95%. The most influential component among uncertainty sources was the recovery of matrix, followed by calibration curve.

• Analytical Science and Technology
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• v.25 no.4
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• pp.257-264
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• 2012

Penicillins belong to the ${\beta}$-lactam class of antibiotics, and are frequently used in human and veterinary medicine. Despite the positive effects of these drugs, improper use of penicillins poses a potential health risk to consumers. This study has been undertaken to determinate multi-residues of penicillins, including amoxicillin, ampicillin, oxacillin, bezylpenicillin, cloxacillin, dicloxacillin, and nafcillin, using liquid chromatographic tandem mass spectrometer (LC-MS/MS). The developed method was validated for specificity, precision, recovery, and linearity in livestock and marine products. The analytes were extracted with 80% acetonitrile and clean-up by a single reversed-phase solid-phase extraction step. Six penicillins presented recoveries higher than 76% with the exception of Amoxicillin. Relative standard deviations (RSDs) were not more than 10%. The method was applied to 225 real samples. Benzylpenicillin was detected in 12 livestock products and 7 marine products. Amoxicillin, ampicillin, cloxacilllin, dicloxacillin, nafcillin and oxacillin were not detected. The detected levels were 0.001~0.009 mg/kg in livestock products excluding eggs and milk. In marine products, the detected levels were under 0.03 mg/kg. They were under the MRL levels. As monitoring results, it is identified to be safe but it is considered that safety management of antibiotics should continue by monitoring.

• Korean Journal of Food Science and Technology
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• v.36 no.6
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• pp.893-899
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• 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.