• Journal of Food Hygiene and Safety
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• v.26 no.4
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• pp.424-434
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• 2011

The increase in the consumption of herb medicines have made their use a public health problem due to the potential fungal contamination and the risk of the presence of my cot ox ins. 360 samples of herb medicines were evaluated for the aflatoxin contamination. The natural occurrence of aflatoxins in these samples were determined using immunoaffinity column clean up and high performance liquid chromatography (HPLC) with post-column derivatization. For samples analyzed, mean levels (incidence) of AFB1, AFB2, AFG1 and AFG2 in positive samples were $1.4\;{\mu}g/kg$(46.4%), $0.4\;{\mu}g/kg$(25.4%), $1.1\;{\mu}g/kg$(37.8%) and $0.9\;{\mu}g/kg$(24.3%), respectively. Recoveries of the full analytical procedure were 71.7~99.7% for AFB1, 88.1~99.2% for AFB2, 82.8~95.5% for AFG1 and 77.9~90.0% for AFG2. The excess cancer risk estimated using the cancer potency of aflatoxin B1 (7 $(mg/kg/day)^{-1}$ for $HBsAg^-$ and 230 $(mg/kg/day)^{-1}$ for $HBsAg^+$) were $1.30{\times}10^{-5}{\sim}1.22{\times}10^{-7}$ for hepatits B surface antigen negative ($HBsAg^-$) and $3.31{\times}10^{-4}{\sim}3.12{\times}10^{-6}$ for hepatits B surface antigen positive ($HBsAg^+$) respectively. In conclusion, although the contamination levels of samples used in the study were low, further actions are also required to undertake a program of herbal surveys in order to access mycotoxin contamination overall so that the safety of public will be protected.

• Journal of the Korean Society of Food Science and Nutrition
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• v.39 no.8
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• pp.1165-1170
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• 2010

A method for the determination of four pesticide compounds, urea (isoproturon), bis-carbamate (phenmedipham), thiocarbamate (pyridate) and vinyllidenediamine (nitenpyram) were examined and analyzed by HPLC with C-18 column ($250\;mm{\times}4.6\;mm$, $5\;{\mu}m$ diameter particle size). Mobile phase consisted of deionized water, acetonitrile and 50 mM $KH_2PO_4$ (pH 2.5). Isoproturon and phenmedipham analytical condition was isocratic elution of the column with 50% solvent A (acetonitrile) and 50% solvent B (deionized water); pyridate was 85% solvent A (acetonitrile) and 15% solvent B (deionized water) at a flow rate of 1 mL/min; and nitenpyram analytical condition was 90% solvent A (50 mM $KH_2PO_4$, pH 2.5) and 10% solvent B (acetonitrile) at a flow rate of 1 mL/min. In results, retention times were 6.12, 8.63, 9.40 and 12.76 min for isoproturon, phenmedipham, pyridate and nitenpyram, respectively. All injection volumes were $10\;{\mu}L$ and the limit of quantitation was 0.05 mg/kg for four pesticide compounds, respectively. Recovery rate test was performed with three farm products, rice, apple and soybean. Four pesticide compounds were spiked at concentrations of 0.05, 0.1 and 0.5 mg/kg. The recovery rates were ranged from 70.18% to 118.08% and the standard deviations of all experiments were within 10%.

• Journal of the Korean Society of Food Science and Nutrition
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• v.12 no.3
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• pp.189-195
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• 1983

Changes of lipid composition in the Improvement-Meju inoculated with Aspergillus oryzae were examined. To investigate those changes systematically, silicic acid column chromatography was used for analysis of glycolipid, neutral lipid, phospholipid, and gas chromatography to examine the change of those fatty acid content. Following results were obtained. The lipid fraction obtained from soaked soybean and cooked soybean were mainly composed of about 93~94% neutral lipid, whereas phospholipid and glycolipid was 4.0~5.0%, 2.0~2.1% level, respectively. During meju incuvation period, neutral lipid decreased gradually, but glycolipid and phospholipid increased. Among the nonpolar lipids prepared from cooked soybean and soaked soybean, triglyceride content was mainly composed of 88~89%, and the content of sterol ester, free fatty acid, diglyceride and sterol was higher in soaked soybean than in cooked soybean. During meju incuvation period, triglyceride content decreased remarkablely, whereas content of sterol ester, free fatty acid and diglyceride increased gradually. From the soaked soybean and the cooked soybean, the fatty acids content of crude lipid, neutral lipid, glycolipid and phospholipid were composed of linoleic acid 54~70%, oleic acid 20.0~22.6%, palmitic acid 11.0~12.4%, linolenic acid 6.0~7.8% and stearic acid 3.4~4.3% in turn and myristic acid showed the trace, palmitic acid was a little higher in glycolipid and phospholipid than in crude lipid and neutral lipid. During meju incuvation period, the change of fatty acid content showed linoleic acid and linolenic acid reduction gradually in the neutral lipid, glycolipid and phospholipid. On the other hand, palmitic acid, stearic acid and oleic acid increased gradually, the maximum value was at the 4-days. The change of glycolipid fatty acid and phospholipid fatty acid was examined. 9-kinds including traced 3-kinds was detected. It was supposed that traced 2-kinks was occurred for incuvation, and those are the matter investigating in the future.

• Journal of Food Hygiene and Safety
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• v.34 no.5
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• pp.413-420
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• 2019

In this study, a sample preparation method and a simultaneous determination method by ultra-high performance liquid chromatography coupled with tandem mass spectrometry for 9 isomers of chlorogenic acid and arbutin in fruits were developed. The samples were extracted using 90% methanol (pH 3.0), with the solutions being shaken and then sonicated for 10 min each. After centrifugation at 4,000 rpm for 10 min, the extraction was concentrated under a vacuum at $40^{\circ}C$ using a vacuum evaporator. The residue was dissolved in 5 mL of 5% methanol and filtered through a $0.45{\mu}m$ membrane before UHPLC-MS/MS analysis. The separations were performed on a C18 column with gradient elution of water (containing 0.1% formic acid) and methanol (containing 0.1% formic acid). The specificity, linearity, limit of detection, limit of quantification, accuracy, and precision of the proposed methods were also evaluated.

• The Sea:JOURNAL OF THE KOREAN SOCIETY OF OCEANOGRAPHY
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• v.14 no.1
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• pp.48-55
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• 2009

Seasonal variations of microalgal biomass and community composition in both the sediment and the seawater were investigated by HPLC pigment analysis in an estuarine muddy sandflat of Gwangyang Bay from January to November 2002. Based on the photosynthetic pigments, fucoxanthin, diadinoxanthin, and diatoxanthin were the most dominant pigments all the year round, indicating that diatoms were the predominant algal groups of both the sediment and the seawater in Gwangyang Bay. The other algal pigments except the diatom-marker pigments showed relatively low concentrations. Microphytobenthic chlorophyll ${\alpha}$ concentrations in the upper layer (0.5 cm) of sediments ranged from 3.44 (March at the middle site of the tidal flat) to 169 (July at the upper site) mg $m^{-2}$, with the annual mean concentrations of $68.4{\pm}45.5,\;21.3{\pm}14.3,\;22.9{\pm}15.6mg\;m^{-2}$ at the upper, middle, and lower tidal sites, respectively. Depth-integrated chlorophyll ${\alpha}$ concentrations in the overlying water column ranged from 1.66 (November) to 11.7 (July) mg $m^{-2}$, with an annual mean of $6.96{\pm}3.04mg\;m^{-2}$. Microphytobenthic biomasses were about 3${\sim}$10 times higher than depth-integrated phytoplankton biomass in the overlying water column. The physical characteristics of this shallow estuarine tidal flat, similarity in taxonomic composition of the phytoplankton and microphytobenthos, and similar seasonal patterns in their biomasses suggest that resuspended microphytobenthos are an important component of phytoplankton biomass in Gwangyang Bay. Therefore, considering the importance of microphytobenthos as possible food source for the estuarine benthic and pelagic consumers, a consistent monitoring work on the behavior of microphytobenthos is needed in the tidal flat ecosystems.

• Journal of Food Hygiene and Safety
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• v.39 no.2
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• pp.72-82
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• 2024

This study aimed to develop a scientifically and systematically standardized xylooligosaccharide analytical method that can be applied to products with various formulations. The analysis method was conducted using HPLC with Cadenza C₁₈ column, involving pre-column derivatization with 1-phenyl-3-methyl-5-pyrazoline (PMP) and UV detection at 254 nm. The xylooligosaccharide content was analyzed by converting xylooligosaccharide into xylose through acid hydrolysis. The pre-treated methods were compared and evaluated by varying sonication time, acid hydrolysis time, and concentration. Optimal equipment conditions were achieved with a mobile phase consisting of 20 mM potassium phosphate buffer (pH 6)-acetonitrile (78:22, v/v) through isocratic elution at a flow rate of 0.5 mL/min (254 nm). Furthermore, we validated the advanced standardized analysis method to support the suitability of the proposed analytical procedure such as specificity, linearity, detection limits (LOD), quantitative limits (LOQ), accuracy, and precision. The standardized analysis method is now in use for monitoring relevant health-functional food products available in the market. Our results have demonstrated that the standardized analysis method is expected to enhance the reliability of quality control for healthy functional foods containing xylooligosaccharide.

• Journal of The Korean Society of Grassland and Forage Science
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• v.36 no.4
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• pp.333-339
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• 2016

The objective of this study was to optimize analytical methods for ochratoxin A (OTA) and zearalenone (ZEA) in rice straw silage and winter forage crops using ultra-high performance liquid chromatography (UHPLC). Samples free of mycotoxins were spiked with $50{\mu}g/kg$, $250{\mu}g/kg$, or $500{\mu}g/kg$ of OTA and $300{\mu}g/kg$, $1500{\mu}g/kg$, or $3000{\mu}g/kg$ of ZEA. OTA and ZEA were extracted by acetonitrile and cleaned-up using an immunoaffinity column. They were then subjected to analysis with UHPLC equipped with a fluorescence detector. The correlation coefficients of calibration curves showed high linearity ($R^2{\geq_-}0.9999$ for OTA and $R^2{\geq_-}0.9995$ for ZEA). The limit of detection and quantification were $0.1{\mu}g/kg$ and $0.3{\mu}g/kg$, respectively, for OTA and $5{\mu}g/kg$ and $16.7{\mu}g/kg$, respectively, for ZEA. The recovery and relative standard deviation (RSD) of OTA were as follows: rice straw = 84.23~95.33%, 2.59~4.77%; Italian ryegrass = 79.02~95%, 0.86~5.83%; barley = 74.93~97%, 0.85~9.19%; rye = 77.99~96.67%, 0.33~6.26%. The recovery and RSD of ZEA were: rice straw = 109.6~114.22%, 0.67~7.15%; Italian ryegrass = 98.01~109.44%, 1.65~4.81%; barley = 98~113.53%, 0.25~5.85%; rye = 90.44~108.56%, 2.5~4.66%. They both satisfied the standards of European Commission criteria (EC 401-2006) for quantitative analysis. These results showed that the optimized methods could be used for mycotoxin analysis of forages.

• Korean Journal of Food Science and Technology
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• v.42 no.3
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• pp.287-291
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• 2010

In this study, a simple and rapid pre-treatment method based on liquid extraction was applied for the simultaneous determination of three macrolides (spiramycin, tylosin, and tilmicosin) residues. In these studies, the stock farm products was used as a matrix sample. When the liquid extraction method was compared with the solid phase extraction (SPE) method, the former showed higher recovery percentages and simpler steps than the latter. The macrolids were separated using a reverse-phase C18 ($250\;mm{\times}4.6\;mm$, $5\;{\mu}m$) column and a gradient elution with mobile phases consisting of phosphate buffer (pH 2.5) and acetonitrile. Tylosin and tilmicosin were detected at 288 nm and spiramycin was detected at 232 nm. The average recovery percentage ranged between 83.0-90.2% for samples spiked with the three macrolids at 50 and 100 ng/g The validation results showed that the limit of detection (7 (spiramycin), 12 (tilmiconsin), 12 (tylosin) ng/g)) was under the regulatory tolerances and the linearity from calibration curves was satisfactory for determining the multi-residue of three macrolids in farm products. Monitoring samples were collected at the main cities in Korea as Seoul, Busan, Deajeon, Incheon, Deagu, and Gwangju. Microlide antibiotics were not detected in most samples.

• Journal of Food Hygiene and Safety
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• v.26 no.1
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• pp.16-24
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• 2011

A method was established for the simultaneous determination of sugar alcohols, erythritol, xylitol, sorbitol, inositol, mannitol, maltitiol, lactitol and isomalt by High Performance Liquid Chromatography (HPLC). The sugar alcohols were converted into strong ultraviolet (UV)-absorbing derivatives with p-nitrobenzoyl chloride (PNBC). HPLC was performed on Imtakt Unison US-$C_18$ column, using acetonitrile: water (77:23) as a mobile phase and UV detection (260 nm). The calibration curves for all sugar alcohols tested were linear in the 10~200 mg/L range. The average recoveries of the sugar alcohols from three confectioneries spiked at 100 ppm of eight sugar alcohol standards ranged from 81.2 to 123.1% with relative standard deviations ranging fromo 0.2 to 4.9%. The limits of detection (LODs) were $0.5{\sim}8\;{\mu}g/L$ and the limits of quantification (LOQs) were $2{\sim}17\;{\mu}g/L$. Reproducibility of 8 sugar alcohols was 0.28~1.97 %RSD. The results of the analysis of confectioneries showed that 89 samples of 130 were detected and the sugar alcohols content of samples investigated varied between 0.4 and 693.7 g/kg. A method for the simultaneous determination of eight sugar alcohols will be used as basic data for control of sugar alcohols in confectioneries, and quality control in food manufacturing.

• Korean Journal of Food Science and Technology
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• v.31 no.4
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• pp.945-951
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• 1999

A simple and practical method for the determination of gardenia yellow in foods was developed. In this method, analysis of gardenia yellow in food products has been carried out by the detection of crocetin and/or geniposide as indicator compounds. As a new analytical method for gardenia yellow, we adopted crocetin, which is produced from colored components of gardenia yellow by alkaline hydrolysis, as an indicator compound. The analysis of gardenia yellow was performed by reverse phase high performance liquid chromatography using a Capcell pak $C_{18}$ column at wave length 240 nm (geniposide) and 435 nm (crocetin). The recovery rates of geniposide and crocetin were found to be 93.4% and 87.8% for Dan Mu Ji, 90.2% and 85.9% for milk, 92.8% and 86.5% for snack, respectively. With this method, the range of crocetin and geniposide contents $({\mu}g/g)$ were as follows: $ND{\sim}1.7$ and $ND{\sim}14.1$ for Dan Mu Ji, $ND{\sim}0.2$ and $ND{\sim}13.6$ for milk, $ND{\sim}1.6$ and $ND{\sim}0.9$ for snack, respectively. The detection limits of crocetin and geniposide were 0.07 ${\mu}g/g$ and 0.05 ${\mu}g/g$, respectively.