• Title/Summary/Keyword: Quantification Analysis

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Simultaneous Determination of Water Soluble Vitamins B Group in Health Functional Foods etc. by HPLC (건강기능식품 등 중 수용성 비타민 B군의 HPLC를 이용한 동시분석법)

  • Kim, Seon Hee;Kim, Jae-Hyun;Lee, Hwa Jung;Oh, Jae Myoung;Lee, Sung Hye;Bahn, Kyeong Nyeo;Seo, Il Won;Lee, Young Joo;Lee, Jin Hee;Kang, Tae Seok
    • Journal of Food Hygiene and Safety
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    • v.30 no.2
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    • pp.143-149
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    • 2015
  • This study was conducted to simultaneous analysis methods for water soluble vitamins B group (vitamin $B_1$, vitamin $B_2$, nicotinic acid, nicotinamide, vitamin $B_6$) which is used as health functional foods etc. Analytical methods of water-soluble vitamins B group by HPLC were established through instrumental analytical conditions, and the examination of data such as domestic and foreign reliable methods, and papers of journal. HPLC method analyzing water soluble vitamins B group was established using Capcell Pak C18 UG 120 column in 270 nm through test of columns. The validation has been performed on the method to determine linearity, accuracy, limits of quantification (LOQ) and repeatability for water soluble vitamins B group. An excellent linearity ($r^2=0.999$) was observed for vitamin $B_1$, vitamin $B_2$, nicotinic acid, nicotinamide, vitamin $B_6$ in the concentration range ($0.1{\sim}2{\mu}g/mL$). Observed recovery of vitamin $B_1$ was found to be between 100 and 103%, vitamin $B^2$ was found to be between 104 and 112%, nicotinic acid was found to be between 82 and 85%, nicotinamide was found to be between 121 and 124% and vitamin $B_6$ was found to be between 95 and 104%. LOQ of vitamin $B_1$ was found to be $0.04{\mu}g/mL$, vitamin $B_2$ was found to be $0.05{\mu}g/mL$, nicotinic acid was found to be $0.15{\mu}g/mL$, nicotinamide was found to be $0.08{\mu}g/mL$ and vitamin $B_6$ was found to be $0.63{\mu}g/mL$. Repeatability precision for vitamin $B_1$ was found to be 0.4%, vitamin $B_2$ was found to be 0.4%, nicotinic acid was found to be 0.5%, nicotinamide was found to be 0.7% and vitamin $B_6$ was found to be 0.4% relative standard deviation (RSD). Also, verify the accuracy of the simultaneous analysis methods, we monitored the labeled contents of the health functional foods and children's preferred foods.

Monitoring of Benzoic Acid, Sorbic Acid, and Propionic Acid in Spices (향신료에서 유래되는 안식향산, 소브산, 프로피온산의 함유량 조사)

  • Yun, Sang Soon;Lee, Sang Jin;Lim, Do Yeon;Lim, Ho Soo;Lee, Gunyoung;Kim, MeeKyung
    • Journal of Food Hygiene and Safety
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    • v.32 no.5
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    • pp.381-388
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    • 2017
  • In this study, we investigated the levels of natural preservatives of benzoic acid, sorbic acid, and propionic acid in spices. The quantitative analysis was performed using high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) for benzoic acid and sorbic acid and gas chromatography-mass spectrometry (GC-MS) for propionic acid. The sample was extracted with ethanol using sonication, then centrifuged and evaporated to dryness and redissolved to 1 mL with ethanol to use for the instrumental analysis. The analytical method was validated based on linearity, recovery, limit of detection (LOD), and limit of quantification (LOQ). This method was suitable to determine low amounts of naturally occurring preservatives (benzoic acid, sorbic acid, and propionic acid) in various spices. Benzoic acid, sorbic acid, and propionic acid were found in 165 samples, 88 samples, and 398 samples, respectively from the total of 493 samples. The concentration of benzoic acid, sorbic acid, and propionic acid were ranged at ND-391.99 mg/L, ND-57.70 mg/L, and ND-188.21 mg/L in spices, respectively. The highest mean levels of benzoic acid, sorbic acid, and propionic acid were found in cinnamon (167.15 mg/L), basil leaves (22.79 mg/L), and white pepper (51.48 mg/L), respectively. The results in this study provide ranges of concentration regarding naturally occurring benzoic acid, sorbic acid, and propionic acid in spices. Moreover, the results may use to the case of consumer complaint or trade friction due to the inspection services of standard criteria for the preservatives of spices.

Analysis and Safety Assessment of Antioxidants Migrated from Polyethylene and Polypropylene Food Packaging Materials into Food Simulants (폴리에틸렌 및 폴리프로필렌 기구·용기·포장 유래 산화방지제 분석 및 안전성평가)

  • Choi, Heeju;Choi, Jae Chun;Bae, In-Ae;Park, Se-Jong;Kim, MeeKyung
    • 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.

The Analysis and Migration of Bisphenol A Related Compounds from Metal Food Cans (식품용 금속 캔으로부터 비스페놀 A 관련 물질들의 분석 및 이행 연구)

  • Park, Se-Jong;Park, So-Ra;Choi, Jae Chun;Kim, MeeKyung
    • Journal of Food Hygiene and Safety
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    • v.32 no.4
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    • pp.329-335
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    • 2017
  • Analysis method was presented for the simultaneous determination of nine bisphenol A related compounds such as bisphenol A (BPA), phenol, p-tert-butylphenol, bisphenol A diglycidyl ether (BADGE), $BADGE{\cdot}2H_2O$, $BADGE{\cdot}2HCl$, bisphenol F diglycidyl ether (BFDGE), $BFDGE{\cdot}2H_2O$ and $BFDGE{\cdot}2HCl$ migrated from inner coatings of metal food cans by high performance liquid chromatography (HPLC) with fluorescence detection. The method was validated by examining the linearity of calibration curve, the limit of detection (LOD), the limit of quantification (LOQ), recovery and uncertainty. The migration tests of nine BPA related compounds were carried out with four food simulants; deionized water (DW), 4% acetic acid, 50% ethanol and n-heptane. There was not any compound detected in DW, 4% acetic acid and 50% ethanol at $60^{\circ}C$ for 30 min and n-heptane at $25^{\circ}C$ for 60 min. BPA and phenol were migrated into 4% acetic acid and 50% ethanol at $95^{\circ}C$ for 30 min. The concentrations were ranged from 0 to $10.77{\mu}g/L$ of BPA and from 0 to $2.35{\mu}g/L$ of phenol. Canned foodstuffs mostly have long-term shelf life. We investigated migration of nine BPA related compounds according to the variation in storage periods (0~90 days) and temperatures (4, 25 and $60^{\circ}C$). All compounds were not founded during 90 days at $4^{\circ}C$ and $25^{\circ}C$, respectively. However BPA and $BADGE{\cdot}2H_2O$ were founded in DW and 4% acetic acid at $60^{\circ}C$. The migration levels of BPA and $BADGE{\cdot}2H_2O$ were close to the value of LOQ, respectively and did not change significantly as storage period. It was founded from results that the migration of BPA related compounds from metal food cans was controlled to a safe level.

Monitoring of Uniconazole by GC-NPD (GC-NPD 동시분석법을 이용한 유니코나졸 잔류실태조사)

  • Kim, Eun-Jeung;Choi, Bu-Chuhl;Choi, Su-Jeong;Hong, Chae-Kyu;Kim, Eun-Hee;Choi, Chae-Man;Seo, Young-Ho;Hwang, Young-Sook;Jang, Mi-Ra;Hwang, In-Sook;Kim, Moo-Sang;Chae, Young-Zoo
    • Korean Journal of Food Science and Technology
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    • v.44 no.3
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    • pp.378-381
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    • 2012
  • The monitoring of the uniconazole residual pesticide for agricultural products was conducted by multiclass pesticide multiresidue methods. Samples were collected from June to November, 2011. Uniconazole pesticide was detected in 49 samples from a total of 3,939 samples. The amount of uniconazole pesticide ranged from 0.09 to 17.89 mg/kg in 49 samples. This method was described for the simultaneous determination of uniconazole by gas chromatography with a nitrogen phosphorus detector (GC-NPD) and mass spectrometry (MS). The limit of detection and quantification were 0.006 and 0.018 mg/kg GC-NPD, respectively. For an evaluation of the GC-NPD method, uniconazole spiked into gyeojachae at a level of 0.5, 5 mg/kg was determined. The recoveries of uniconazole by the GC-NPD method ranged from 83.4 to 101.4%. The results indicate that the method of simultaneous analysis is applicable to uniconazole analysis.

Methodological Comparison of the Quantification of Total Carbon and Organic Carbon in Marine Sediment (해양 퇴적물내 총탄소 및 유기탄소의 분석기법 고찰)

  • Kim, Kyeong-Hong;Son, Seung-Kyu;Son, Ju-Won;Ju, Se-Jong
    • Journal of the Korean Society for Marine Environment & Energy
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    • v.9 no.4
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    • pp.235-242
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    • 2006
  • The precise estimation of total and organic carbon contents in sediments is fundamental to understand the benthic environment. To test the precision and accuracy of CHN analyzer and the procedure to quantify total and organic carbon contents(using in-situ acidification with sulfurous acid($H_2SO_3$)) in the sediment, the reference material s such as Acetanilide($C_8H_9NO$), Sulfanilammide($C_6H_8N_2O_2S$), and BCSS-1(standard estuary sediment) were used. The results indicate that CHN analyzer to quantify carbon and nitrogen content has high precision(percent error=3.29%) and accuracy(relative standard deviation=1.26%). Additionally, we conducted the instrumental comparison of carbon values analyzed using CHN analyzer and Coulometeric Carbon Analyzer. Total carbon contents measured from two different instruments were highly correlated($R^2=0.9993$, n=84, p<0.0001) with a linear relationship and show no significant differences(paired t-test, p=0.0003). The organic carbon contents from two instruments also showed the similar results with a significant linear relationship($R^2=0.8867$, n=84, p<0.0001) and no significant differences(paired t-test, p<0.0001). Although it is possible to overestimate organic carbon contents for some sediment types having high inorganic carbon contents(such as calcareous ooze) due to procedural and analytical errors, analysis of organic carbon contents in sediments using CHN Analyzer and current procedures seems to provide the best estimates. Therefore, we recommend that this method can be applied to measure the carbon content in normal any sediment samples and are considered to be one of the best procedure far routine analysis of total and organic carbon.

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Analysis of vitamin B12 in fresh cuts of Korean pork for update of national standard food composition table (국가표준식품성분표 개정을 위한 국내산 돈육의 부위별 비타민 B12 함량 분석)

  • Mun, Geum-Ju;Song, Wonju;Park, Sun-Hye;Jeong, Beom-Gyun;Jung, Gil-Rak;Choi, Kap Seong;Kim, Jin-Hyoung;Choi, Youngmin;Chun, Jiyeon
    • Food Science and Preservation
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    • v.24 no.7
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    • pp.983-991
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    • 2017
  • This study was performed to update the National Standard Food Composition Table (NSFCT) published by Korea Rural Development Administration, especially focusing on vitamin $B_{12}$ for Korean pork. Total 7 primal and 22 retail fresh cuts of Korean pork were analyzed for vitamin $B_{12}$ and the applied immunoaffinity-HPLC was validated. Vitamin $B_{12}$ assay by immunoaffinity-HPLC obtained recoveries over 95% and coefficient variations of precision below about 10%, which met the limits required for validation acceptance. Limits of detection and quantification of immunoaffinity-HPLC were 0.01 and $0.33{\mu}g/100g$, respectively. Quality control chart showed that analysis performance was excellent during the entire of study. Vitamin $B_{12}$ contents of pork cuts significantly varied depending the types of primal and its retail cuts (p<0.05). Belly, Boston butt, rib cuts showed relatively high vitamin $B_{12}$ contents compared to other primal cuts. Vitamin $B_{12}$ content of pork retail cuts were also significantly different within the same primal cuts (p<0.05). Among 22 retail cuts, the highest vitamin $B_{12}$ was observed in Tosisal in belly primal part ($0.98{\mu}g/100g$) while both Aldeungsimsal in loin and Hongdukkaesal in hide leg were the lowest by $0.33{\mu}g/100g$. This study provides reliable vitamin $B_{12}$ data for the Korean pork fresh cuts through standard sampling, method validation and analytical quality control, which would be used for update of Korean NSFCT.

EFFECT OF NERVE GROWTH FACTOR GENE INJECTION ON THE NERVE REGENERATION IN RAT LINGUAL NERVE CRUSH-INJURY MODEL (백서 설신경 압박손상모델에서 신경성장인자 유전자 주입이 신경재생에 미치는 영향)

  • Gao, En-Feng;Chung, Hun-Jong;Ahn, Kang-Min;Kim, Soung-Min;Kim, Yun-Hee;Jahng, Jeong-Won;Lee, Jong-Ho
    • Maxillofacial Plastic and Reconstructive Surgery
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    • v.28 no.5
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    • pp.375-395
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    • 2006
  • Purpose: Lingual nerve (LN) damage may be caused by either tumor resection or injury such as wisdom tooth extraction, Although autologous nerve graft is sometimes used to repair the damaged nerve, it has the disadvantage of necessity of another operation for nerve harvesting. Moreover, the results of nerve grafting is not satisfactory. The nerve growth factor (NGF) is well-known to play a critical role in peripheral nerve regeneration and its local delivery to the injured nerve has been continuously tried to enhance nerve regeneration. However, its application has limitations like repeated administration due to short half life of 30 minutes and an in vivo delivery model must allow for direct and local delivery. The aim of this study was to construct a well-functioning $rhNGF-{\beta}$ adenovirus for the ultimate development of improved method to promote peripheral nerve regeneration with enhanced and extended secretion of hNGF from the injured nerve by injecting $rhNGF-{\beta}$ gene directly into crush-injured LN in rat model. Materials and Methods: $hNGF-{\beta}$ gene was prepared from fetal brain cDNA library and cloned into E1/E3 deleted adenoviral vector which contains green fluorescence protein (GFP) gene as a reporter. After large scale production and purification of $rhNGF-{\beta}$ adenovirus, transfection efficiency and its expression at various cells (primary cultured Schwann cells, HEK293 cells, Schwann cell lines, NIH3T3 and CRH cells) were evaluated by fluorescent microscopy, RT-PCR, ELISA, immunocytochemistry. Furthermore, the function of rhNGF-beta, which was secreted from various cells infected with $rhNGF-{\beta}$ adenovirus, was evaluated using neuritogenesis of PC-12 cells. For in vivo evaluation of efficacy of $rhNGF-{\beta}$ adenovirus, the LNs of 8-week old rats were exposed and crush-injured with a small hemostat for 10 seconds. After the injury, $rhNGF-{\beta}$ adenovirus($2{\mu}l,\;1.5{\times}10^{11}pfu$) or saline was administered into the crushed site in the experimental (n=24) and the control group (n=24), respectively. Sham operation of another group of rats (n=9) was performed without administration of either saline or adenovirus. The taste recovery and the change of fungiform papilla were studied at 1, 2, 3 and 4 weeks. Each of the 6 animals was tested with different solutions (0.1M NaCl, 0.1M sucrose, 0.01M QHCl, or 0.01M HCl) by two-bottle test paradigm and the number of papilla was counted using SEM picture of tongue dorsum. LN was explored at the same interval as taste study and evaluated electro-physiologically (peak voltage and nerve conduction velocity) and histomorphometrically (axon count, myelin thickness). Results: The recombinant adenovirus vector carrying $rhNGF-{\beta}$ was constructed and confirmed by restriction endonuclease analysis and DNA sequence analysis. GFP expression was observed in 90% of $rhNGF-{\beta}$ adenovirus infected cells compared with uninfected cells. Total mRNA isolated from $rhNGF-{\beta}$ adenovirus infected cells showed strong RT-PCR band, however uninfected or LacZ recombinant adenovirus infected cells did not. NGF quantification by ELISA showed a maximal release of $18865.4{\pm}310.9pg/ml$ NGF at the 4th day and stably continued till 14 days by $rhNGF-{\beta}$ adenovirus infected Schwann cells. PC-12 cells exposed to media with $rhNGF-{\beta}$ adenovirus infected Schwann cell revealed at the same level of neurite-extension as the commercial NGF did. $rhNGF-{\beta}$ adenovirus injected experimental groups in comparison to the control group exhibited different taste preference ratio. Salty, sweet and sour taste preference ratio were significantly different after 2 weeks from the beginning of the experiment, which were similar to the sham group, but not to the control group.

Simultaneous Analysis of 13 Pesticides in Groundwater and Evaluation of its Persistent Characteristics

  • Song, Dahee;Park, Sunhwa;Jeon, Sang-Ho;Kim, Ki-In;Hwang, Jong Yeon;Kim, Moonsu;Jo, Hun-Je;Kim, Deok-hyun;Lee, Gyeong-Mi;Kim, Hye-Jin;Kim, Tae-Seung;Chung, Hyen Mi;Kim, Hyun-Koo
    • Korean Journal of Soil Science and Fertilizer
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    • v.50 no.5
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    • pp.434-451
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    • 2017
  • For this study, groundwater samples for 3 years from 2011 through 2013 were collected at 106 groundwater monitoring site in Korea. These groundwater samples were analyzed for 13 pesticides such as cabofuran, pentachlorobenzene, hexachlorobenzene, simazine, atrazine, lindane (gamma-HCH), alachlor, heptachlor, chlordane (total), endosulfan (1, 2), dieldrin, endrin, 4,4-DDT. The objectives of this study were to determine the detection frequency and their concentrations of 13 pesticides and evaluate the health risk level considering ingestion, inhalation, and skin contact using concentrations of 13 pesticides in groundwater samples. An analysis was used for the simultaneous determination for 13 pesticides using GC-MS. GC-MS was performed on HP-5ms, using helium ($1ml\;min^{-1}$) as carrier gas. The average recoveries of the pesticides were from 92.8% to 120.8%. The limits of detection (LODs) were between $0.004{\mu}g\;L^{-1}$ and $0.118{\mu}g\;L^{-1}$ and the limits of quantification (LOQs) were between $0.012{\mu}g\;L^{-1}$ and $0.354{\mu}g\;L^{-1}$. 106 groundwater wells were selected. 54 wells were from well to monitor background groundwater quality and 52 wells were from well to monitor groundwater quality in industrial or contamination source area. Eight pesticides including pentachlorobenzene, lindane (Gamma-HCH), heptachlor, chlordane (total), Endosulfan (1, 2), dieldrin, endrin, and 4,4-DDT were not detected in groundwater samples. The detection frequency for hexachlorobenzene, alachlor, carbofuran and simazine was 23.4%, 11.4%, 7.3%, and 1.0%, respectively. Atrazine was detected once in 2011. The average concentrations were $0.00423{\mu}g\;L^{-1}$ for carbofuran, $0.000243{\mu}g\;L^{-1}$ for alachlor, $0.00015{\mu}g\;L^{-1}$ for simazine, and $0.00001{\mu}g\;L^{-1}$ for hexachlorobenzene. The detection frequency of hexachlorobenzene was high, but the average concentration was low. In the contaminated groundwater, the detection frequency for hexachlorobenzene, alachlor, carbofuran, simazine and atrazine was 26.1%, 21.3%, 7.1%, 1.9% and 0.3%, respectively. In the uncontaminated groundwater, detection frequency for hexachlorobenzene, carbofuran and alachlor were 20.2%, 7.5%, and 1.9% respectively. Simazine and atrazine were not detected at uncontaminated groundwater wells. According to the purpose of groundwater use, atrazine was detected for agricultural groundwater use. Hexachlorobenzene showed high detection frequency at agricultural groundwater use area where the animal feeding area and golf course area were located. Alachlor showed more than 50% detection frequency at cropping area, pollution concern river area, and golf course area. Atrazine was detected in agricultural water use area. By land use, the maximum detection frequency of alachlor was found near an orchard. For human risk assessment, the cancer risk for the 5 pesticides was between $10^{-7}$ and $10^{-10}$, while the non-cancer risk (HQ value) was between $10^{-4}$ and $10^{-6}$. For conclusion, these monitoring study needs to continue because of the possibility of groundwater contamination based on various purpose of groundwater use.

Inhibitory Effects of Ethanolic Extracts from Aster glehni on Xanthine Oxidase and Content Determination of Bioactive Components Using HPLC-UV (섬쑥부쟁이 에탄올 추출물의 잔틴산화효소 저해 효능 및 HPLC-UV를 이용한 유효성분의 함량 분석)

  • Kang, Dong Hyeon;Han, Eun Hye;Jin, Changbae;Kim, Hyoung Ja
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.45 no.11
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    • pp.1610-1616
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    • 2016
  • This study aimed to establish an optimal extraction process and high performance liquid chromatography-ultraviolet (HPLC-UV) analytical method for determination of 3,5-dicaffeoylquinic acid (3,5-DCQA) as a part of materials standardization for the development of a xanthine oxidase inhibitor as a health functional food. The quantitative determination method of 3,5-DCQA as a marker compound was optimized by HPLC analysis using a Luna RP-18 column, and the correlation coefficient for the calibration curve showed good linearity of more than 0.9999 using a gradient eluent of water (1% acetic acid) and methanol as the mobile phase at a flow rate of 1.0 mL/min and a detection wavelength of 320 nm. The HPLC-UV method was applied successfully to quantification of the marker compound (3,5-DCQA) in Aster glehni extracts after validation of the method with linearity, accuracy, and precision. Ethanolic extracts of A. glehni (AGEs) were evaluated by reflux extraction at 70 and $80^{\circ}C$ with 30, 50, 70, and 80% ethanol for 3, 4, 5, and 6 h, respectively. Among AGEs, 70% AGE at $70^{\circ}C$ showed the highest content of 3,5-DCQA of $52.59{\pm}3.45mg/100g$ A. glehni. Furthermore, AGEs were analyzed for their inhibitory activities on uric acid production by the xanthine/xanthine oxidase system. The 70% AGE at $70^{\circ}C$ showed the most potent inhibitory activity with $IC_{50}$ values of $77.01{\pm}3.13{\sim}89.96{\pm}3.08{\mu}g/mL$. The results suggest that standardization of 3,5-DCQA in AGEs using HPLC-UV analysis would be an acceptable method for the development of health functional foods.