• 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.

• Korean Journal of Environmental Agriculture
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• v.16 no.1
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• pp.37-43
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• 1997

Tolerance mechanism to simazine (6-chloro-N,N'-diethyl-1,3,5-triazine-2,4-diamine) in Coix lacryma-jobi was investigated with respect to herbicide detoxification via glutathione conjugation. Simazine was initially absorbed by seedlings of C. lacryma-jobi and corn, but after 12 hours of treatment, no significant difference in simazine absorption was found in both species. Simazine absorbed was rapidly metabolized to glutathione-simazine conjugate. One to six hours after treatment, metabolism was approximately 2-fold faster in C. lacryma-jobi than in corn. Glutathione content was found 1.5- and 2.3-fold higher in coleoptile and root of C. lacryma-jobi, respectively, compared with corn. In both species, the highest concentration of glutathione was found in coleoptile tissue. Glutathione S-transferase that exhibits activity with 1-chloro-2,4-dinitrobenzene was not significantly different between two species. However, glutathione S-transferase activity with simazine was approximately 2-fold greater in C. lacryma-jobi than in corn. The glutathione S-transferase activity was 20 to 30% greater in shoot of either species than in root. Fast protein liquid chromatography-anion exchange column was used to separate glutathione S-transferase isozymes in coleoptiles of C. lacryma-jobi and corn. A peak of glutathione S-transferase activity with 1-chloro-2,4-dinitrobenzene and two peaks of glutathione S-transferase activity with simazine from C. lacryma-jobi were coeluted with those from corn, but showed greater activity than in the case of corn. Another glutathione S-transferase isozyme that exhibits activity with simazine was detected in the elution of C. lacryma-jobi extract, but not in corn. Electron transport in chloroplast thylakoids isolated from leaves of both species was equally sensitive to simazine applied at 1 to 100 nM. These results indicate that the simazine tolerance in C. lacryma-jobi is due to its capacity to detoxify the herbicide via glutathione conjugation, which is positively correlated with the level of glutathione content and glutathione S-transferase activity.

• 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.

• Korean Journal of Food Science and Technology
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• v.14 no.2
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• pp.97-105
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• 1982

The edible portion of chestnut, Castenea crenata Sieb, et Zucc, were freeze-dried and subjected to analysis of minerals, lipid classes and fatty acid composition by silicic acid column chromatography and gas-liquid chromatography. The results of analysis for the minerals in chestnut showed that the contents of magnesium, iron and phosphorus were decreased during storage after freeze-drying. The contents of neutral lipids, glycolipids and phospholipids in the raw edible portion were 34.6, 38.6, and 26.8%, respectively. The contents of neutral lipids and phospholipids of the freeze-dried chestnut were decreased, while glycolipids were increased during storage. In the fatty acid composition of total lipid, $C_{16:0}$, $C_{18:2}$ and $C_{18:3}$ acid were abundant in the raw edible portion, but freeze-dried chestnut contained relatively much amount of $C_{16:0}$, $C_{18:1}$, and $C_{18:2}$ acid. It is noticeable that $C_{18:2}$ and $C_{18:3}$ acid in the freeze-dried chestnut were remarkably decreased during storage. Upon the fatty acid composition, total lipid contained $C_{18:2}$ and $C_{16:0}$ acid in the highest proportion, but neutral lipids, glycolipids and phospholipids contained $C_{16:0}$ and $C_{18:2}$ acid in the highest proportion. Cycloartenol (20.6%) was a major component in the 4-monomethylsterol fraction separated by thin layer chromatography and cyclolaudenol, cycloeucalenol, and citrostadienol were detected as minor components. Sitosterol (74.6%) was a major component in the 4-desmethylsterol fraction separated by thin-layer chromatography and ${\Delta}^5-avensterol$, campesterol, stigmasterol and brassicasterol were also detected as minor components.

• Korean Journal of Food Science and Technology
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• v.20 no.5
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• pp.674-682
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• 1988

Total lipids from the roe, muscle and viscus of L. carinata were analyzed for lipid composition by column chromatography, thin-layer chromatography and gas-liquid chromatography. The roe lipids were characterized by a high level of wax esters (63.1%) and a low proportion of trigiycerides (9.9%). The viscus lipids also contained wax esters (32.8%) as its main component, followed by free fatty alcohols and acids (23.5%). On the other hand, the muscle lipids were found to contain a large amount of triglycerides (66.1%) with a trace of wax esters. The main fatty alcohol component of roe and viscus wax esters was C16:0 alcohol (53.0%; 61.7%), accompanied by C18:1 alcohol (10.2%) in the former and by C15:0 alcohol (8.8%) in the latter. Considerable amounts of odd-numbered fatty alcohols were found in both wax esters. On the other hand, the fatty acids of the roe and viscus wax esters contained a high percentage of monounsaturated (49.7%-56.6%) consisting of C16:1, C18:1 and C17:1 acid, and a significant amount of polyunsaturated (41.2%-32.9%), particularly C20:5${\omega}$3. The fatty acid components of triglycerides and phospholipids were different among the tissues tested, especially between roe and muscle or viscus. The fatty acid compositions of free fatty acids from the muscle and viscus were characterized by a higher level of polyunsaturated fatty acids (46.0-34.3%) compared to those of triglycerides 'in the roe, muscle and viscus (28.4%, 19.4% and 19.2%).

• Microbiology and Biotechnology Letters
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• v.41 no.2
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• pp.198-206
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• 2013

The five anti-complementary polysaccharides (MFKF-NP, MFKF-AP1${\alpha}$, ${\beta}$, and MFKF-AP2${\alpha}$, ${\beta}$) were separated from hot water extracts of fruiting bodies of Fomes fomentarius by two subsequent column chromatography using DEAE-sepharose FF and Concanavalin A-sepharose 4B. The order of anti-complementary activity was MFKF-AP1${\beta}$ > MFKF-AP1${\alpha}$ > MFKF-AP2${\alpha}$ > MFKF-AP2${\beta}$ > MFKF-NP > Polysaccharide Krestine (PSK). Especially, MFKF-AP1${\beta}$ among those showed the most excellent anti-complementary activity (70% of ITCH50 value at $20{\mu}g/ml$). The monosaccharide composition analysis by gas chromatography indicates that MFKF-AP1${\alpha}$ and ${\beta}$ are a kind of homoxylan consisted mainly of xylose above 97%. Molecular weight of MFKF-AP1${\beta}$, major anti-complementary polysaccharide, was estimated to be about 12,000 by high performance liquid chromatography (HPLC). After the incubation of the serum with MFKF-AP1${\beta}$ in the presence or absence of $Mg^{++}$ and $Ca^{++}$ ions, its anti-complementary activity was investigated. This result indicated that MFKF-AP1${\beta}$ seems to be activator both on the classical and the alternative pathway of complement activation.

• Journal of Sericultural and Entomological Science
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• v.47 no.2
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• pp.51-55
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• 2005

Resveratrol is naturally occurring phytoalexin compounds produced by grape berries, peanuts, and their products in response to stress such as fungal infection, heavy metal ions or UV irradiation. The objective of this study was to develope a reliable high performance liquid chromatographic (HPLC) method for the quantitative determination of trans-resveratrol in mulberry fruit. Samples were extracted in 80% MeOH and filtered with $0.45{\mu}m$ syringe filter. The transresveratrol was separated Waters $C_{18}$ column, using a mobile phase containing 0.025% trifluroacetic acid in 5% acetonitril and 0.035% trifluroacetic acid in 50% acetonitril, detected by photodiode array detector (PDA) at 254 nm and the flow rate was 1ml/min. Under this analytical condition, the mean content of mulberry fruits (fifty varieties) was $777.3{\pm}585.9ppm$. Among the tested samples, 'Mansaengbaekpinosang (II)' was the highest level in 3450.6 ppm. However four accessions including 'Gukbu', 'Sabangso (I)', 'Simseol' and yield mulberry fruit were not able to detected. Eight suitable varieties selected for the production of fruit were 'Jeolgokchosaeng (Chungbuk)' 777.8 ppm, 'Dangsang 7' 771.1 ppm, 'Jangsosang' 133.9 ppm, 'Susungppong' 31.1 ppm, 'Suwonnosang' 639.7 ppm, 'Palcheongsipyung' 1475.9 ppm, 'Kangsun' 864.0 ppm, and 'Jukcheonchosaeng' 1458.5 ppm. 'Daesungppong' which was the first authorized variety for the production of mulberry fruit was 1236.7 ppm. In conclusion, these results suggest that mulberry including fruit and leaf may a good new resource for resveratrol production.

• 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.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.19 no.4
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• pp.321-326
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• 1986

Oyster (Crassostrea gigas), arkshell (Anadare(Scapharce) broughtonii) and sea-mussel (Mytilus edulis) were investigated as to their lipid classes. Lipid extracts from shellfishes were fractionated into neutral lipid (NL), glycolipid (GL) and phospho-lipid (PL) by column chromatography with silicic acid. The fatty acid compositions of their lipid classes and lipid fractions were determined by gas liquid chromatography (GLC). Total lipid contents of shellfishes were $3.5\%$ in the oyster, $1.4\%$ in the arkshell, $1.0\%$ in the sea-mussel. The major fatty acids of total lipids were palmitic acid, eicosapentaenoic acid and docosahexaenoic acid in the oyster and the sea-mussel, palmitic acid, oleic acid and eicosapentaenoic acid in the arkshell. The lipid composition of neutral lipid fractions in shellfishes was separated and identified as free sterol, free fatty acid, triglyceride, hydrocarbon and esterified sterol by TLC. Of these classes, triglyceride fraction was most abundant, amounting to 55.6, 77.7 and $60.4\%$ in the three samples mentioned above, respectively. The main fatty acids of glycolipid were palmitic acid, eicosaenoic acid and docosahexaenoic acid in oyster, myristic acid, palmitic acid and palmitoleic acid in the arkshell, docosahexaenoic acid, linolenic acid and palmitic acid in the sea-mussel. The major fatty acids of phospholipid were palmitic acid, eicosapentaenoic acid and docosahexaenoic acid in the oyster and sea-mussel, palmitic acid, eicosapentaenoic acid and erucic acid in the arkshell.