• Korean Journal of Food Science and Technology
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• v.33 no.1
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• pp.33-39
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• 2001

To develop a method for separation process using Sep-pak $C_18$, simultaneous and systematic analysis of 8 permitted and 11 non-permitted synthetic food colors in Korea, optimization of analysis conditions for reverse phase ion-pair high performance liquid chromatography was carried out. For the best result of Sep-pak $C_18$ separation the pH of color standard mixture solution was $5{\sim}6$ and 0.1% HCl-methanol solution were set as eluent. The colors eluated from Sep-pak $C_18$ cartridge were determined and confirmed by high performance liquid chromatography with a photodiode array detector at 420 nm for yellow colors type, at 520 nm for red colors type, at 600 nm for blue and green colors type and at 254 nm for mixed colors. Conditions for HPLC analysis were as follows: column, Symmetry $C_18$ (5 m, 3.9 mm $i.d.{\times}150\;mm$); mobile phase, 0.025 M ammonium acetate (containing 0.01 M tetrabutylammonium bromide) : acetonitrile : methanol (65 : 25 : 10) and 0.025 M ammonium acetate(containing 0.01 M tetrabutylammonium bromide) : acetonitrile : methanol (40 : 50 : 10); flow rate, 1 mL/min. It takes 35 minutes for simultaneaus analysis and 18 minutes for systematic analysis. The detection limits range of each colors were $0.01{\sim}0.05\;{\mu}g/g$.

• Korean Journal of Food Science and Technology
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• v.40 no.2
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• pp.123-128
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• 2008

The MRLs (maximum residue limits) of DDT (DDD and DDE) in fresh ginseng, dried ginseng, and steamed red ginseng are set as low as 0.01 mg/kg, 0.05 mg/kg, and 0.05 mg/kg, respectively. Therefore, this study was undertaken to develop a simple and highly sensitive analysis method, as well as to reduce interfering ginseng matrix peaks, for the determination of DDT isomers (o,p'-DDE, p,p'-DDE, o,p'-DDD, p,p'-DDD, o,p'-DDT, and p,p'-DDT) in fresh ginseng, dried ginseng, and steamed red ginseng at the 0.01 mg/kg level. The method used acetonitrile extraction according to simultaneous analysis, followed by normal-phase Florisil solid-phase extraction column clean-up. The purification method entailed the following steps: (1) dissolve the concentrated sample extract in 7 mL hexane; (2) add 3 mL of $H_2SO_4$; (3) vigorously shake on avortex mixer; (4) cetrifuge at 2000 rpm for 5 min; (5) transfer 3.5 mL of the supernatant to the Florisil-SPE (500 mg/6 mL);and (6) elute the SPE column with 1.5 mL of hexane and 10 mL of ether/hexane (6:94). The determination of DDT isomers was carried out by a gas chromatography-electron capture detector (GC-${\mu}$ECD). The hexane and ether/hexane (6:94) eluate significantly removed chromatographic interferences, and the addition of 30% $H_2SO_4$ to the acetonitrile extract effectively reduced many interfering ginseng matrix peaks, to allow for the determination of the DDT isomers at the 0.01 mg/kg level. The recoveries of the 6 fortified (most at 0.01 mg/kg) DDT isomers from fresh ginseng, dried ginseng, and steamed red ginseng ranged from 87.9 to 99.6%. The MDLs (method detection limits) ranged from 0.003 to 0.009 mg/kg. Finally, the application of this method for the determination of DDT isomers is sensitive, rapid, simple, and inexpensive.

• Korean Journal of Environmental Agriculture
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• v.33 no.4
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• pp.388-394
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• 2014

BACKGROUND: Aclonifen is used as a systemic and selective herbicide to control a wide spectrum broad-leaf weeds by inhibition carotenoid biosynthesis, and then its MRLs(Maximum Residue Limits) will be determined in onion and garlic. In this study, a new official method was developed for aclonifen determination in agricultural products to routinely inspect the violation of MRL as well as to evaluate the terminal residue level. METHODS AND RESULTS: Aclonifen was extracted from crop samples with acetone and the extract was partitioned with dichloromethane and then purified by silica solid phase extraction(SPE) cartridge. The purified samples were detected GC using an ECD detector. Limits of detection(LOD) was 0.001 mg/kg and quantification(LOQ) was 0.005 mg/kg, respectively. For validation purposes, recovery studies were carried out at three different concentration levels (LOQ, $10{\times}LOQ$, $50{\times}LOQ$, n=5). The recoveries were ranged from 74.3 to 95.0% with relative standard deviations(RSDs) of less than 8%. All values were consistent with the criteria ranges requested in the Codex guidelines(CAC/GL 40). CONCLUSION: The proposed analytical method was accurate, effective and sensitive for aclonifen determination and it will be used to as an official method in Korea.

• Journal of Food Hygiene and Safety
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• v.20 no.3
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• pp.141-146
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• 2005

A simple and sensitive analysis method based on reverse phase (RP) HPLC with UV detector was developed for simultaneous determination of chlorophyll a and b, pheophorbide a and $\beta-Carotene$ in Chlorella and Spirulina products. For added concentration $(50\;\mug/ml)$ of chlorophyll a and b, pheophorbide a and $\beta-Carotene$, recoveries of those were 70.3, 71.6, 60.1 and $90.5\%$, respectively, with relative standard deviations of 2.8,6.0, 10.6 and $10.4\%$. Limit of detection and quantification had ranges of $0.1\sim1.0\;\mug/ml$ and $0.2\sim2.0\;\mug/ml$, respectively. Calibration curve was linear with correlation coefficient of 0.995 for chlorophyll a and b, pheophorbide a and $\beta-Carotene$. Results of simultaneous determination in Chlorella and Spirulina products were showed ranges of $121.g\sim543.0\;\mug/ml$ for chlorophyll a,$0.6\sim160.0\;\mug/ml$ for chlorophyll b, $19.2\sim60.3\;\mug/ml$ for pheophorbide a and $383.6\sim1713.7\;\mug/ml$ for $\beta-Carotene$, respectively. Chlorophyll b contents in Chlorella products were detected above 30 times level to those in Spirulina products. $\beta-Carotene$ contents in Spirulina products were detected 2.7 times level to those in Chlorella products.

• 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.

• Analytical Science and Technology
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• v.24 no.2
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• pp.150-157
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• 2011

Aflatoxins are secondary metabolites of the molds of Aspergillus flavus and Aspergillus parasiticus. They are highly carcinogenic compounds and can affect a wide range of vegetable commodities such as cereals (especially corn), nuts, peanuts, fruits and oil seeds, in the field and during storage. In fact, oilseeds are often stored for weeks in conditions that promote the mould growth, and the possible consequent presence of aflatoxins in oilseeds can lead to their transfer in oil. In addition, aflatoxins can be found as a natural contaminant in multi-cereals and beans making baby food for infants and young-children. The objective of this study was to validate the liquid extraction method or develop an analytical method for edible oil and infant-children foods. Therefore, this study developed condition of extract for aflatoxins ($B_1$, $B_2$, $G_1$ and $G_2$) in edible oil using a high performance liquid chromatography with florescence detector (HPLC/FLD). Aflatoxins were extracted from edible oil samples by means of MSPD (Matrix solid phased dispersion), utilizing $C_{18}$ as dispersing material and purified by using immunoaffinity column. The gression line coefficients were above 0.999. The recoveries for aflatoxins ranged from 85.9 to 93.0%, and relative standard deviations were below 5.7%. The new developed method of aflatoxins effectively enhanced recoveries by using MSPD-Immunoaffinity column compared with liquid extraction. The analytical method for liquid extraction of aflatoxin was appropriate for infant-children food. Reviewing the current method, the recoveries of aflatoxins ($B_1$, $B_2$, $G_1$ and $G_2$) were 89.5~92.3%.

• 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.

• The Bulletin of The Korean Astronomical Society
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• v.39 no.2
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• pp.90-90
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• 2014

The Immersion Grating Infrared Spectrometer (IGRINS) is the first astronomical spectrograph that uses a silicon immersion grating as its dispersive element. IGRINS fully covers the H and K band atmospheric transmission windows in a single exposure. It is a compact high-resolution cross-dispersion spectrometer whose resolving power R is 40,000. An individual volume phase holographic grating serves as a secondary dispersing element for each of the H and K spectrograph arms. On the 2.7m Harlan J. Smith telescope at the McDonald Observatory, the slit size is $1^{{\prime}{\prime}}{\times}15^{{\prime}{\prime}}$. IGRINS has a plate scale of 0.27" pixel-1 on a $2048{\times}2048$ pixel Teledyne Scientific & Imaging HAWAII-2RG detector with a SIDECAR ASIC cryogenic controller. The instrument includes four subsystems; a calibration unit, an input relay optics module, a slit-viewing camera, and nearly identical H and K spectrograph modules. The use of a silicon immersion grating and a compact white pupil design allows the spectrograph collimated beam size to be 25mm, which permits the entire cryogenic system to be contained in a moderately sized ($0.96m{\times}0.6m{\times}0.38m$) rectangular Dewar. The fabrication and assembly of the optical and mechanical components were completed in 2013. From January to July of this year, we completed the system optical alignment and carried out commissioning observations on three runs to improve the efficiency of the instrument software and hardware. We describe the major design characteristics of the instrument including the system requirements and the technical strategy to meet them. We also present the instrumental performance test results derived from the commissioning runs at the McDonald Observatory.

• Journal of the Korean Society of Food Science and Nutrition
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• v.44 no.3
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• pp.418-424
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• 2015

The content of ${\beta}$-carotene in agricultural foods, such as seasonings, tea, vegetables, cereals, nuts & seeds, oils & fats, and fruits, were quantitatively analyzed using reversed-phase HPLC with an UV/visible detector. Standard reference material (SRM) 2385 was used as a control material to validate measurement of ${\beta}$-carotene in this study. Recovery percentage and relative standard deviation of ${\beta}$-carotene in SRM 2385 were 102% and 1.73%, respectively. Vegetables and tea contained relatively high concentrations of ${\beta}$-carotene (young barley powder, $17,293.95{\mu}g/100g$; raw young barley, $2,755.15{\mu}g/100g$; dried green tea leaves, $13,671.85{\mu}g/100g$; green tea powder, $7,579.04{\mu}g/100g$). Contents of ${\beta}$-carotene in nuts & seeds as well as oils & fats ranged from $11.32{\mu}g/100g$ in almond products (roasted with salt) to $58.56{\mu}g/100g$ in perilla seed oil. Among 20 fruits, a high content of ${\beta}$-carotene was found in apricots (raw), which contained $2,280.35{\mu}g/100g$.

• 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.