• Journal of the Korean Society of Food Science and Nutrition
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• v.46 no.2
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• pp.210-219
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• 2017

This study aimed to establish an optimal extraction process and high-performance liquid chromatography (HPLC)-photodiode array (PDA) analytical method for determination of marker compounds, dihydrokaempferol (DHK) and 3-O-methylquercetin (3-MeQ), as a part of materials standardization for the development of health functional foods from stems of Opuntia ficus-indica var. saboten (OFS). The quantitative determination method of marker compounds was optimized by HPLC analysis, and the correlation coefficient for the calibration curve showed very good linearity. The HPLC-PDA method was applied successfully to quantification of marker compounds in OFS after validation of the method in terms of linearity, accuracy, and precision. Ethanolic extracts from stems of O. ficus-indica var. saboten (OFSEs) were evaluated by reflux extraction at 70 and $80^{\circ}C$ with 50, 70, and 80% ethanol for 3, 4, 5, and 6 h. Among OFSEs, OFS70E at $80^{\circ}C$ showed the highest contents of DHK and 3-MeQ of $26.42{\pm}0.65$ and $3.88{\pm}0.29mg/OFS100g$, respectively. Furthermore, OFSEs were determined for their antioxidant activities by measuring 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging and lipid peroxidation (LPO) inhibitory activities in rat liver homogenate. OFS70E at $70^{\circ}C$ showed the most potent antioxidant activities with $IC_{50}$ values of $1.19{\pm}0.11$ and $0.89{\pm}0.09mg/mL$ in the DPPH radical scavenging and LPO inhibitory assays, respectively. To identify active components of OFS, various chromatographic separation of OFS70E led to isolation of 11 flavonoids: dihydrokaempferol, dihydroquercetin, 3-O-methylquercetin, quercetin, isorhamnetin 3-O-glucoside, isorhamnetin 3-O-galactoside, narcissin, kaempferol 7-O-glucoside, quercetin 3-O-galactoside, isorhamnetin, and kaempferol 3-O-rutinoside. The results suggest that standardization of DHK in OFSEs using HPLC-PDA analysis would be an acceptable method for the development of health functional foods.

• Korean Journal of Food Science and Technology
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• v.28 no.4
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• pp.616-623
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• 1996

Eum Yang Kwak, the aerial part of Epimedium koreanum, is widely used as a folk medicine for stimulant in man, tonic, and hypotensive purpose. The plant contains icariin (a specific flavonoid), magnoflorine (an alkaloid) and tannin, but their contents are not known until now. In this paper, a quantitative analysis method for them was developed. Determination of icariin and magnoflorine was successfully achived by high performance liquid chromatography equipped with a UV detector in the ranges of $0.1{\sim}0.4\;mg$ and $0.002{\sim}0.1\;mg\;per\;ml$ sample, respectively. Extraction of the plant was carried out with water or 50% ethanol using different decocting temperatures and times. Icariin was well extracted either by water ($100^{\circ}C$, 3hr) or 50% ethanol ($85^{\circ}C$, 1hr), and its content in the plant was measured to be 0.94%. On the other hand, magnoflorine was fully extracted by 50% ethanol ($85^{\circ}C$, 1hr), and its content was determined to be 0.16%. Therefore, decoction of the medicinal plant with water at $100^{\circ}C$ for 3hr turned out to be recommendable for the best extraction.

• Journal of the Korean Society of Food Science and Nutrition
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• v.44 no.12
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• pp.1847-1855
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• 2015

Supercritical carbon dioxide ($SC-CO_2$) treatment has been becoming an important method for substituting the use of organic solvents for samples extraction prior to analysis due to its low toxicity, ease of handling, low cost of disposal etc. Freeze-dried bovine liver was treated with $SC-CO_2$ under different pressures (200, 300, and 450 bar) in order to investigate effects on physicochemical properties and reduction of microbial load. The yield of lipid extraction from bovine liver by $SC-CO_2$ treatment increased with increasing pressure, with values of 84, 86, and 90% in response to 200, 300, and 450 bar, respectively. Results of high performance liquid chromatography analysis showed that vitamin A and coenzyme $Q_{10}$ ($CoQ_{10}$), which is soluble in lipid, were almost removed from bovine liver by $SC-CO_2$ treatment. Saturated fatty acids ratio of bovine liver decreased with increasing pressure, whereas polyunsaturated fatty acids increased with increasing pressure. Total content of amino acids in bovine liver treated by $SC-CO_2$ was less than that of the control sample without treatment. The number of aerobic bacteria in bovine liver, which was stored at $5^{\circ}C$ for 5 days and freeze-dried, decreased from 6.2 to 4.2 log CFU/g by $SC-CO_2$ treatment at 100 bar for 3 h. Interestingly, coliform bacteria were not found in the bovine liver sample by $SC-CO_2$ at 100 bar for 3 h under all storage conditions. This indicates that $SC-CO_2$ treatment can effectively reduce coliform bacteria in the food matrix even at low moisture. In conclusion, freeze-dried bovine liver by proper $SC-CO_2$ treatment may be used as a potential high protein source, with increasing microbial safety and stability of lipid oxidation.

• Journal of Food Hygiene and Safety
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• v.32 no.5
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• pp.424-433
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• 2017

Antioxidants are used in the manufacturing of commercial food packages made of polyolefin plastic such as polyethylene and polypropylene for the purpose to delay the oxidation reaction of the polymer due to oxygen or traces of ozone in the atmosphere. Additives in plastics may be migrated from the packaging materials into foods, thereby presenting a potential health risk to the consumer. Therefore, it is necessary to determine migration level of antioxidants from food packaging materials to foodstuffs in order to take proactive management. In this study, we have developed a method for the analysis of 10 antioxidants, which are butylated hydroxyanisole (BHA), butylated hydroxytoluene (BHT), Cyanox 2246, 425 and 1790, Irgafos 168, and Irganox 1010, 1330, 3114 and 1076, migrated from the food packaging materials into four food simulants for aqueous, acidic, alcoholic and fatty foods. The antioxidants were determined by reversed-phase high-performance liquid chromatograph-ultraviolet detector with 276 nm after solid-phase extraction with a hydrophilic-lipophilic balance (HLB) cartridge or dilution with isopropanol. The analytical method showed a good linearity of coefficient ($R^2{\geq}0.99$), limits of detection (0.11~0.41 mg/L), and limits of quantification (0.34~1.24 mg/L). The recoveries of antioxidants spiked to four food simulants ranged from 71.3% to 109.4%. The migrated antioxidants in this study were within the safety levels that resulted from the safety assessment by the estimated daily intake to the tolerable daily intake.

• Journal of Food Hygiene and Safety
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• v.32 no.5
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• pp.434-442
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• 2017

The UV light in sunlight breaks down the chemical bonds in a polyolefin polymer through a process called photodegradation, ultimately causing cracking, chalking, colour changes, and loss of physical properties such as impact strength, tensile strength, elongation, and others. UV absorbers are used to prevent or terminate the oxidation of plastics by UV light. They are receptive to UV radiation and dissipate the energy harmlessly as heat. Benzotriazoles and benzophenones are used mainly in polyolefins such as polyethylene and polypropylene. In this study, we have developed a method for the analysis of 12 UV absorbers, which are Uvinul 3000, Cyasorb UV 24, Uvinul 3040, Tinuvin 312 and P, Seesorb 202, Chimassorb 81, Tinuvin 329, 234, 326, 328 and 327, migrated from the food packaging materials into four food simulants for aqueous, acidic, alcoholic and fatty foods. The UV absorbers in food simulants were determined by reversed-phase high performance liquid chromatograph-ultraviolet detector with 310 nm after solid-phase extraction with a hydrophilic-lipophilic balance (HLB) cartridge or dilution with isopropanol. The analytical method showed a good linearity of coefficient ($R^2{\geq}0.99$), limits of detection (0.049~0.370 mg/L), and limits of quantification (0.149~1.120 mg/L). The recoveries of UV absorbers spiked to four food simulants ranged from 70.05% to 110.13%. The developed method would be used as a reliable tool to determine concentrations of the migrated UV absorbers.

• Journal of Korean Society of Environmental Engineers
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• v.31 no.10
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• pp.845-854
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• 2009

There has been increased concern regarding the release of antibiotics to different environmental compartments due to the possibility of the development of antibiotic resistant bacteria. However, limited information is available regarding the occurrence, fate, and transport of antibiotics in Korea in both the aqueous phase and in solid phases such as sediment and soil. Therefore, this study was conducted to monitor the concentration of released antibiotics in surface water, sediment, and soil adjacent to a cattle manure composting facility in Korea. Specifically, the following six antibiotics were monitored: tetracycline (TC), chlortetracycline (CTC), oxytetracycline (OTC), sulfamethazine (SMT), sulfamethoxazole (SMX), and sulfathiazole (STZ). To extract and quantify the antibiotics from different environmental compartments, solid phase extraction (SPE) and high performance liquid chromatography mass spectrometry (HPLC/MS) techniques were adopted. The concentration of the six antibiotics ranged from below the detection limit (BDL) to 0.71 ${\mu}g$/L in surface water, from BDL to 27.61 ${\mu}g$/L in sediment, and from 0.12 to 157.33 ${\mu}g$/L in soil. In addition, higher concentrations of antibiotics were observed in surface water and sediment at locations closer to the composting facility indicating that composting is the source of the antibiotics found in the environment. Furthermore, higher concentrations of antibiotics were observed in the solid phase (sediment and soil) than the aqueous phase. These findings indicate that the possibility of antibiotic resistant bacteria is increased because such bacteria are more stable in the solid phase. Overall, longterm monitoring of the aqueous phase and solid phase is necessary to gain a better understanding of the impact of antibiotics from source on the environment in Korea.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.39 no.3
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• pp.195-203
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• 2013

In this study, antioxidative effects of the extracts of different species and flowering periods of Inula britannica were investigated. According to the free radical (1,1-diphenyl-2-picrylhydrazyl, DPPH) scavenging activity of the extracts, The I. britannica var. chinensis flower extract (500 ${\mu}g/mL$) was measured in a 79.89% free radical scavenging activity, but the flower extracts of similar species (I. britannica var. linariaefolia Regel, I. britannica var. ramosa, I. salicina var. asiatica) did not show any effect on the free radical scavenging activity. The effects of the free radical scavenging activity of I. britannica var. chinensis flower extracts were exhibited in the order of full bloom (93.68%), bud (43.28%), and fallen blossom (14.11%). Next, we established optimum condition of extract solvent, temperature, extraction time. The extract from ethanol at $60^{\circ}C$ showed the most free radical scavenging activity among other conditions and extraction time not relevant in free radical scavenging activity. The protective effects of the extract of I. britannica var. chinensis flower on the photohemolysis of human erythrocytes by using rose bengal were increased in a concentration-dependent manner (5 ~ 50 ${\mu}g/mL$). In particular, the extract in 50 ${\mu}g/mL$ concentration exhibited better protective activity (${\tau}_{50}$ = 116.1 min) than (+)-${\alpha}$-tocopherol (${\tau}_{50}$ = 73.44 min), which is a known lipophilic antioxidant. Principle component of I. britannica var. chinensis flower was identified as quercetin of flavonoids by high-performance liquid chromatography (HPLC). These results indicate that the extract of I. britannica var. chinensis flower can function as antioxidants in biological systems, particularly skin exposed to UV radiation by scavenging free radical and $^1O_2$, and protect cellular membranes against ROS. It is concluded that the antioxidative effects of the extract of I. britannica var. chinensis flower could be applicable to functional cosmetics.

• Journal of the Korean Society of Food Science and Nutrition
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• v.41 no.12
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• pp.1740-1746
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• 2012

Sparassis (S.) crispa is an edible mushroom abundant in dietary fiber and ${\beta}$-glucan. The aim of this study was to prepare extracts and residues of the fruit bodies of S. crispa fermented with Lactobacillus (L.) brevis and Monascus (M.) pilosus and to measure the remaining dietary fiber and ${\beta}$-glucan. Dried powder of S. crispa containing 64.4 g/100 g total dietary fiber (2.6 g/100 g soluble and 61.8 g/100 g insoluble dietary fibers) and 24.0 g/100 g ${\beta}$-glucan was used as the starting material for the extraction. Raw and fermented S. crispa were extracted with hot water and three kinds of aqueous ethanol (50, 70, and 90%, v/v), respectively. A hot water extract from S. crispa fermented with M. pilosus had greater soluble dietary fiber content (19.3 g/100 g) than that from raw S. crispa with 14.6 g/100 g soluble dietary fiber or that from L. brevis-fermented S. crispa with 8.2 g/100 g soluble dietary fiber. The yield of the extract was 16.6% of intial weight of dried S. crispa. After hot water extraction of S. crispa fermented with M. pilosus, residues containing 90.5 g/100 g total dietary fiber (1.3 g/100 g soluble and 89.2 g/100 g insoluble dietary fibers) were obtained, and the yield was 69.6% of intial weight of dried S. crispa. The residue (31.0 g/100 g) contained more ${\beta}$-glucan than raw S. crispa or M. pilosus-fermented S. crispa (24.4 g/100 g). The resulting hot water extract and residue from S. crispa fermented with M. pilosus would be suitable for use in preparing liquid and powdered health functional foods, respectively.

• Journal of Food Hygiene and Safety
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• v.34 no.2
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• pp.115-123
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• 2019

An analytical method was developed for the determination of fenpropimorph, a morpholine fungicide, in hulled rice, potato, soybean, mandarin and green pepper using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) sample preparation and LC-MS/MS (liquid chromatography-tandem mass spectrometry). The QuEChERS extraction was performed with acetonitrile followed by addition of anhydrous magnesium sulfate and sodium chloride. After centrifugation, d-SPE (dispersive solid phase extraction) cleanup was conducted using anhydrous magnesium sulfate, primary secondary amine sorbents and graphitized carbon black. The matrix-matched calibration curves were constructed using seven concentration levels, from 0.0025 to 0.25 mg/kg, and their correlation coefficient ($R^2$) of five agricultural products were higher than 0.9899. The limits of detection (LOD) and quantification (LOQ) were 0.001 and 0.0025 mg/kg, respectively, and the limits of quantification for the analytical method were 0.01 mg/kg. Average recoveries spiked at three levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n=5) and were in the range of 90.9~110.5% with associated relative standard deviation values less than 5.7%. As a result of the inter-laboratory validation, the average recoveries between the two laboratories were 88.6~101.4% and the coefficient of variation was also below 15%. All optimized results were satisfied the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. This study could serve as a reference for safety management relative to fenpropimorph residues in imported and domestic agricultural products.

• The Korean Journal of Pesticide Science
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• v.17 no.4
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• pp.314-334
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• 2013

This study explored an efficient modified Quick, Easy, Cheap, Effective, Rugged and safe (QuEChERS) method combined with liquid chromatography-electrospray ionization with tandem mass spectrometric detection for the analysis of residues of 76 pesticides in brown rice, barley and corn including acidic sulfonylurea herbicides. Formic acid (1%) acid in acetonitrile and dispersive solid phase extractions used for extraction of pesticides and clean-up of the extract respectively. Two fortified spikes at 50 and 200 ng $g^{-1}$ levels were performed for recovery test. Mean recoveries of majority of pesticides at two spike levels ranged from 73.2 to 132.2, 80.9 to 136.8, 66.6 to 143.5 for brown rice, barley and corn respectively with standard error (CV) less than 10%. Good linearity of calibration curves were achieved with $R^2$ > 0.9907 within the observed concentration ranged. The modified method also provided satisfactory results for sulfonylurea herbicides. The method was applied to the determination of residues of target pesticides in real samples. A total of 26 pesticides in 36 out of 98 tasted samples were observed. The highest concentration was observed for tricyclazole at 1.17 mg $kg^{-1}$ in brown rice. This pesticide in two brown rice samples exceeded their MRLs regulated for rice in republic of Korea. Except tricyclazole none of the observed pesticides' concentration was higher than their MRLs. The results reveal that the method is effectively applicable to routine analysis of residues of target pesticides in brown rice, barley and corn.