• Korean Journal of Environmental Agriculture
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• v.18 no.3
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• pp.221-228
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• 1999

This study was carried out to extract the natural antioxidants from Bovine bile and to investigate their effects on various antioxidant activities. It also characterized the patterns of antioxidants by GC/FID and GC/MS. The antioxidative activities and chemical structure of the antioxidant were elucidated by examining the effects of biological activity and the analysis of GC/MS. The antioxidant materials extracted from bovine bile were isolated and purified by silica gel column chromatography and TLC. It was confirmed that there were effects of antioxidants such as Xanthine Oxidase(XO) and Glutathione-S-Transferase(GSH-T) on antioxidative activities. When they were compared with BHT, bile extracts showed the relative effects of 51.2% on the antioxidant activity, the inhibition effects of 48.3% on XO activity, and the synergism effects of 85.7% on the GSH-T activity. According to the results of investigation at neuron cell of mouse, the rate of cell activity in the treatment of 6mM glutathione was 96%, While it in the treatment of 140mg of bile extract was 78%. Based on the TLC analysis of EtOAc extracts from the Bovine bile, the antioxidant activity appeared at $R_f$ value, 0.72. These results suggested that the antioxidant may be coprostan 3-ol.

• Proceedings of the Plant Resources Society of Korea Conference
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• 2018.04a
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• pp.77-77
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• 2018

미역의 뿌리부분인 미역귀에는 알긴산과 후코이단 성분이 풍부하고 고혈압과 당뇨등과 같은 성인병을 예방하는데 도움이 된다. 후코이단은 미역과 다시마 같은 갈조류에서 추출된 천연물질로 특히 면역력을 활성화하고 항암작용으로 잘 알려져 있다. 알긴산 등 유용성분이 함유된 것으로 알려진 미역귀의 유용성분을 분석하여, 향후 미역귀를 활용한 제품개발의 기초자료를 제공하고자 본 연구를 수행하였다. 본 연구에 사용된 미역귀는 2015년 12월 완도 금일수산에서 제공받아 연구재료로 활용하였다. AOAC방법에 따라 분석한 미역귀의 일반성분은 수분이 대부분을 차지하였으며, 조섬유와 가용성 무질소물 함량이 높게 나타났다. 이는 시료로 사용한 미역귀가 수확 후 바로 냉동보관 되어서 수분함량이 높은 것으로 보여진다. 유리당은 미역귀 1g에 증류수를 가하여 $60^{\circ}C$에서 4시간 추출 한 후, 원심분리(3,000 rpm, 30 min)하여 $0.45{\mu}m$ membrane filter (Millipore Co., USA)로 여과한 여액을 HPLC (High Performance Liquid Chromatography)를 이용하여 분석한 결과, 미역귀의 유리당은 Galactose 1종만이 검출되었다. 미역귀의 구성아미노산과 유리아미노산은 $0.45{\mu}m$ membrane filter로 여과하여 얻은 여액을 일정량 취하여 AccQ-Tag 시약을 사용하여 유도체화 시킨 후 HPLC로 분석하였다. 미역귀의 구성아미노산은 glutamic acid, aspartic acid, alanine, lysine, threonine, valine, arginine 순으로 높은 함량을 나타내었으며, 유리아미노산은 glutamic acid, alanine, threonine, arginine, lysine 순으로 높은 함량을 나타내었다. 미역귀의 유리아미노산함량은 표고에 비하여 현저히 낮은 함량이 나타났으며, 주요아미노산은 해조류의 풍미를 대표하는 아미노산인 glutamic acid와 alanine으로 나타났다.

• Journal of Food Hygiene and Safety
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• v.32 no.2
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• pp.89-95
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• 2017

A rapid, sensitive analytical method for glucuronolactone in beverages was developed and validated using hydrophilic interaction liquid chromatography coupled to electrospray ionization tandem mass spectrometry (HILIC-ESI-MS/MS). To determine the optimum analytical conditions for glucuronolactone, three different kinds of HILIC columns and two mobile phases with different pH values were examined. An amide-bonded stationary phase with a pH 9 acetonitrile-rich mobile phase was the best condition in terms of column retention, ESI-MS/MS response area, and signal-to-noise ratio. After extraction, glucuronolactone was separated through the HILIC amide column and detected by negative ESI-MS/MS in selected reaction monitoring (SRM) mode. Nine energy drinks sold in Korea were spiked with glucuronolactone at a concentration of 5 ng/mL; the Monster $Energy^{TM}$ sample showed the smallest peak area and its signal-to-noise ratio was used for method validation. Good linearity was obtained in the concentration range from 20 to 1500 ng/mL with a correlation coefficient > 0.998. The developed method had a limit of detection (LOD) of 6 ng/mL and a limit of quantitation (LOQ) of 20 ng/mL. The recovery of this method at concentration of 20, 100, 500, and 1000 ng/mL was 96.3%-99.2% with relative standard deviations (RSD) of 1.6%-14.0%. A reproducibility precision assessment at concentration of 100 and 500 ng/mL was carried out among three laboratories. The recovery of that evaluation was 95.1%-102.3% with RSD of 2.7%-7.0%. An analysis of variance indicated that there was no difference between the recovery results of the three laboratories at the 5% significance level. The validated method is applicable to inspecting beverages adulterated with glucuronolactone in Korea.

• Analytical Science and Technology
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• v.28 no.5
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• pp.323-330
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• 2015

Alkaptonuria, a rare inherited metabolic disease, is characterized by a lack of homogentisate dioxygenase and accumulation of homogentisic acid (HGA), leading to homogentisic aciduria, arthritis, and ochronosis. In this study, a rapid analytical method, without an expensive and tedious solid phase extraction step, was developed to quantify HGA in plasma using GC-MS. HGA-spiked pooled plasma samples were subjected to liquid-liquid extraction (LLE) with ethyl acetate, followed by trimethylsilyl derivatization (TMS) and GC-MS quantification using selected ion monitoring. The formation of TMS derivative of the 1 carboxylic and 2 hydroxyl functional groups was performed by reacting BSTFA (with 10% TMCS) for 5 min at 80 ℃. For selected ion monitoring, quantification and confirmation ions were determined based on specific ions (m/z 384, m/z 341 and m/z 252) of the TMS derivative of HGA. Calibration curves of pooled normal plasma specimens showed a linear relationship in the range of 1-100 ng/µL. The precision and accuracy were within a relative standard deviation (RSD) of 1 to 15% and a bias of -5 to 25%. Recoveries were obtained in the range of 99-125% and 95-115% for intra-day and inter-day assay, respectively, at 2, 20 and 80 ng/µL. The limit of detection (LOD) and limit of quantification (LOQ) were 0.4 ng/µL and 4 ng/µL, respectively. No homogentisic acid was excreted from normal Korean plasma samples. Collectively, the results from the present study suggest that this method could be useful for routine diagnosis and therapeutic monitoring of alkaptonuria patients with excellent sensitivity and rapidity.

• Korean Journal of Weed Science
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• v.30 no.4
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• pp.361-370
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• 2010

This study was carried out to establish the analytical method of MCPA residue in brown rice and rice straw by HPLC/UVD. When MCPA was extracted from sample under the pH 3.6 by adding acetone 200 mL and 1N-HCl 100 mL, the extraction efficiency was high by 87%. And purification efficiency was high by 83% when 5 mL of 1% methanol/acetonitrile was eluated by the florisil Sep-pak cartridge column. From spiking of $0.1{\mu}g\;mL^{-1}$ and $0.25{\mu}g\;mL^{-1}$ of MCPA to control sample, respectively, average recovery rate of MCPA in brown rice was 96.0% and 94.9% and that in rice straw was 92.5% and 88.2%, respectively. Precision of experiment was very high by relative standard deviation of 1.5% to 5.7%. In brown rice and rice straw treated with bentazone+MCPA (11+1.2%) of 30 kg and 60 kg per ha at 30 days after rice transplanting, respectively, maximum residue limit was under $0.05{\mu}g\;mL^{-1}$ of the recommended rate of Korean Food and Drug Administration. From the above results, the analytical procedure of MCPA in plants such as hydrolysis, saponification and derivatization were ommited, and retention time was faster and recovery rate was higher than the existed results of HPLC/UVD. Therefore, these results were greatly improved and seemed to be usefully applied for residue analysis of MCPA in plants.

• Journal of Food Hygiene and Safety
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• v.25 no.1
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• pp.36-42
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• 2010

The method for the determination of ethylenediamine (EDA) and hexamethylenediamine (HMDA) in food simulants was developed, and migration amounts of these compounds was monitored for 124 polyamide (PA) utensils. The diurethane derivatives of EDA and HMDA, which produced by reaction with ethyl chloroformate, were analyzed by using gas chromatograph (GC)/flame ionization detector (FID) and GC/mass spectrometer (MS). The developed method was validated with $0.3\;{\mu}g/mL$ of limit of detection (LOD) for EDA and $0.1\;{\mu}g/mL$ of LOD for HMDA, > 0.999 of linearity($r^2$) and > 88% of recovery. The EDA was detected 1.31 and $02.06\;{\mu}g/mL$ for 2 samples in water. The HMDA was detected $0.29\;-\;0.93\;{\mu}g/mL$ for 3 samples in 20% ethanol and $0.26\;-\;0.44\;{\mu}g/mL$ for 10 samples in n-heptane. These migration levels were below the specific migration limits (SML) of $12\;{\mu}g/mL$ and $2.4\;{\mu}g/mL$ for EDA and HMDA established in EU.

• Korean Journal of Environmental Agriculture
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• v.30 no.3
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• pp.281-287
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• 2011

BACKGROUND: According to Korean regulations, bottled waters (BWs) can not be treated with chemical disinfectants like chlorine, so UV and ozone disinfection is applied. During the past several years, chemicals were detected in some BWs, and the public was concerned about the safety of BWs. METHODS AND RESULTS: Mineral waters were stored for 180 days at $25^{\circ}C$ and $50^{\circ}C$, tested acetaldehyde and formaldehyde by HPLC. When mineral waters were put in a PET bottles, the formaldehyde level ranged from 5 to $66{\mu}g/L$ during 180 days at $50^{\circ}C$. While the acetaldehyde level ranged from 31 to $221{\mu}g/L$, it was low than $16{\mu}g/L$ in glass bottle. CONCLUSION(s): This result showed that formaldehyde and acetaldehyde were detected higher in PET bottles than glass bottles, these also increased depending on the time of storage. Concentration of formaldehyde and acetaldehyde could be significantly influenced by the time of storage and temperature.

• 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.