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Development of Analysis Method of Caffeine and Content Survey in Commercial Foods by HPLC (HPLC를 이용한 카페인의 분석법 개발 및 시판 식품중 함유량 조사)

  • Kim, Hee-Yun;Lee, Young-Ja;Hong, Ki-Hyoung;Lee, Chul-Won;Kim, Kil-Saeng;Ha, Sang-Chul
    • Korean Journal of Food Science and Technology
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    • v.31 no.6
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    • pp.1471-1476
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    • 1999
  • A simple and practical method for determination of caffeine in foods was developed. The analysis of caffeine was performed by reverse phase high performance liquid chromatography using a ${\mu}-Bondapak\;C_{18}$ column at isocratic condition with methanol-acetic acid-water(20 : 1 : 79) on UV detector at 280 nm. The clean-up and extraction of caffeine in samples were based on a simple pretreatment using a Sep-Pak $C_{18}$ cartridge. Recovery rates obtained with this method for cider, candy, cookie, milk, ice cream and persimmon leaf tea were 99.23%, 99.50%, 99.17%, 99.37%, 98.93% and 99.10% respectively. And the detection limit of caffeine was $0.1\;{\mu}g/mL$. With this method, the range of caffeine contents extracted from coffee, green tea, black tea, Oolong tea(tea bag), soft drinks, ice cream, milk and commercial confectionery were $3.38{\sim}37.50\;mg/g,\;16.30{\sim}26.10\;mg/g,\;10.80{\sim}16.65\;mg/g,\;11.25\;mg/g,\;0.06{\sim}0.11\;mg/g,\;0.04{\sim}0.44\;mg/g,\;0.04{\sim}0.39\;mg/g\;and\;0.10{\sim}1.80\;mg/g$, respectively. But caffeine was not detected in the other tea such as Acanthopanax sessiliflorum tea, Angelica gigas tea, Angelica tea, Arrow root tea, Duchu'ng tea, Dunggulle tea, Ganoerma lucidum tea, Ginger tea powder, Persimmon leaf tea, Ssanghwa tea and Cocoa mix powder.

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Melanogenesis regulatory constituents from Premna serratifolia wood collected in Myanmar

  • WOO, SO-YEUN
    • Proceedings of the Plant Resources Society of Korea Conference
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    • 2019.04a
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    • pp.21-22
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    • 2019
  • Melanin is a mixture of pigmented biopolymers synthesized by epidermal melanocytes that determine the skin, eye, and hair colors. Melanocytes produce two different kinds of melanin, eumelanin (dark brown/black insoluble pigments found in dark skin and dark hair and pheomelanin (lighter red/yellow). The biological role of melanin is to prevent skin damage by ultraviolet (UV) radiation. However, the overproduction or deficiency of melanin synthesis could lead to serious dermatological problems, which include melasma, melanoderma, lentigo, and vitiligo. Therefore, regulating melanin production is important to prevent the pigmentation disorders. Myanmar has a rich in natural resources. However, the chemical constituents of these natural resources in Myanmar have not been fully investigated. In the effort to search for compounds with anti-melanin deposition activity from Myanmar natural resources, five plants were collected in Myanmar. Extracts of these collected five plants were tested for anti-melanin deposition activity against a mouse melanoma cell line (B16-F10) induced with ${\alpha}$-melanocyte-stimulating hormone (${\alpha}$-MSH) and 3-isobutyl-1-methylxanthine (IBMX), and their anti-melanin deposition activities were compared with the positive control, arbutin. Among the tested extracts, the CHCl3 extracts of the Premna serratifolia (syn: P. integrifolia) wood showed anti-melanin deposition activities with IC50 values of $81.3{\mu}g/mL$. Hence, this study aims to identify secondary metabolites with anti-melanin deposition activity from P. serratifolia wood of Myanmar. P. serratifolia belongs to the Verbenaceae family and is widely distributed in near western sea coast from South Asia to South East Asia, which include India, Malaysia, Vietnam, Cambodia, and Sri Lanka. People in Tanintharyi region located in the southern part of Myanmar utilize the P. serratifolia, Sperethusa crenulata, Naringi crenulata, and Limonia acidissima as Thanaka, traditional cosmetics in Myanmar. Thanaka is applied in the form of paste onto skins to make it smooth and clear, as well as to prevent wrinkles, skin aging, excessive facial oil, pimples, blackheads, and whiteheads. However, the chemical constituents responsible for their cosmetic properties are yet to be identified. Moreover, the chemical constituents of P. serratifolia was almost uncharacterized. Investigation of the P. serratifolia chemical constituents is thus an attractive endeavor to discover new anti-melanin deposition active compounds. The investigation of the chemical constituents of the active CHCl3 extract of P. serratifolia led to isolation of four new lignoids, premnan A (1), premnan B (2), taungtangyiol C (3), and 7,9-dihydroxydolichanthin B (4), together with premnan C (5) (assumed to be an artifact), one natural newlignoid,(3R,4S)-4-(1,3-benzodioxol-5-ylcarbonyl)-3-[(R)-1-(1,3-benzo dioxol-5-yl)-1-hydroxy methyl]tetrahydro-2-furanone (6), and five known compounds (7-11)1,2). The structures of all isolated compounds were determined on the basis of their spectroscopic data and by comparison with the reported literatures. The absolute configurations of 1-3 and 5 were also determined by optical rotation and circular dichroism (CD) data analyses1). The anti-melanin deposition activities of all the isolated compounds were evaluated against B16-F10 cell line. 7,9-Dihydroxydolichanthin B (4) and ($2{\alpha},3{\alpha}$)-olean-12-en-28-oic acid (11) showed strong anti-melanin deposition activities with IC50 values of 18.4 and $11.2{\mu}M$, respectively, without cytotoxicity2). On the other hand, compounds 1-3, 5, and 7 showed melanogenesis enhancing activities1). To better understand their anti-melanin deposition mechanism, the effects of 4 and 11 on tyrosinase activities were investigated. The assay indicated that compounds 4 and 11 did not inhibit tyrosinase. Furthermore, we also examined the mRNA expression of microphthalmia-associated transcription factor (MITF), tyrosinase (TYR), tyrosinase-related protein-1 (TRP-1), and tyrosinase-related protein-2 (TRP-2). Compounds 4 and 11 down-regulated the expression of Tyr and Mitf mRNAs, respectively. Although the P. serratifolia wood has been used as traditional cosmetics in Myanmar for centuries, there are no scientific evidences to support its effectiveness as cosmetics. Investigation of the anti-melanin deposition activity of the chemical constituents of P. serratifolia thus provided insight into the effectiveness of the P. serratifolia wood as a cosmetic agent.

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Development and Validation of an Analytical Method for Quinoxyfen in Agricultural Products using QuEChERS and LC-MS/MS (QuEChERS법 및 LC-MS/MS를 이용한 농산물 중 살균제 Quinoxyfen의 잔류시험법 개발 및 검증)

  • Cho, Sung Min;Do, Jung-Ah;Lee, Han Sol;Park, Ji-Su;Shin, Hye-Sun;Jang, Dong Eun;Choi, Young-Nae;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.140-147
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    • 2019
  • An analytical method was developed for the determination of quinoxyfen in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with 1% acetic acid in acetonitrile and water was removed by liquid-liquid partitioning with $MgSO_4$ (anhydrous magnesium sulfate) and sodium acetate. Dispersive solid-phase extraction (d-SPE) cleanup was carried out using $MgSO_4$, PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed by using LC-MS/MS in positive mode with MRM (multiple reaction monitoring). The matrix-matched calibration curves were constructed using six levels ($0.001-0.25{\mu}g/mL$) and the coefficient of determination ($R^2$) was above 0.99. Recovery results at three concentrations (LOQ, 10 LOQ, and 50 LOQ, n=5) were in the range of 73.5-86.7% with RSDs (relative standard deviations) of less than 8.9%. For inter-laboratory validation, the average recovery was 77.2-95.4% and the CV (coefficient of variation) was below 14.5%. All results were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for quinoxyfen determination in agricultural commodities. This study could be useful for the safe management of quinoxyfen residues in agricultural products.

Evaluation of Manganese Removal from Acid Mine Drainage by Oxidation and Neutralization Method (산화법과 중화법을 이용한 산성광산배수 내 망간 제거 평가)

  • Kim, Bum-Jun;Ji, Won-Hyun;Ko, Myoung-Soo
    • Economic and Environmental Geology
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    • v.53 no.6
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    • pp.687-694
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    • 2020
  • Two oxidizing agents (KMnO4, H2O2), and one neutralizing agent (NaOH) were applied to evaluate Mn removal in mine drainage. A Mn2+ solution and artificial mine drainage were prepared to identify the Fe2+ influence on Mn2+ removal. The initial concentrations of Mn2+ and Fe2+ were 0.1 mM and 1.0 mM, respectively. The injection amount of oxidizing and neutralizing agents were set to ratios of 0.1, 0.67, 1.0, and 2.0 with respect to the Mn2+ mole concentration. KMnO4 exhibited a higher removal efficiency of Mn2+ than did H2O2 and NaOH, where approximately 90% of Mn2+ was removed by KMnO4. A black MnO2 was precipitated that indicated the oxidation of Mn2+ to Mn4+ after an oxidizing agent was added. In addition, MnO2 (pyrolusite) is a stable precipitate under pH-Eh conditions in the solution. However, relatively low removal ratios (6%) of Mn2+ were observed in the artificial mine drainage that included 1.0 mM of Fe2+. The rapid oxidation tendency of Fe2+ as compared to that of Mn2+ was determined to be the main reason for the low removal ratios of Mn2+. The oxidation of Fe2+ showed a decrease of Fe concentration in solution after injection of the oxidizing and neutralizing agents. In addition, Mn7+ of KMnO4 was reduced to Mn2+ by Fe2+ oxidation. Thus, the concentrations of Mn increased in artificial mine drainage. These results revealed that the oxidation method is more effective than the neutralization method for Mn removal in solution. It should also be mentioned that to achieve the Mn removal in mine drainage, Fe2+ removal must be conducted prior to Mn2+ oxidation.

Determination and Validation of an Analytical Method for Spiropidion and Its Metabolite Spiropidion-enol (SYN547305) in Agricultural Products with LC-MS/MS (LC-MS/MS를 이용한 농산물 중 Spiropidion 및 대사산물 Spiropidion-enol (SYN547305) 시험법 개발 및 검증)

  • Gu, Sun Young;Lee, Su Jung;Shin, Hye-Sun;Kang, Sung Eun;Chung, Yun Mi;Lee, Jung Mi;Jung, Yong-hyun;Moon, Guiim
    • Korean Journal of Environmental Agriculture
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    • v.41 no.2
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    • pp.82-94
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    • 2022
  • BACKGROUND: Spiropidion and its metabolite are tetramic acid insecticide and require the establishment of an official analysis method for the safety management because they are newly registered in Korea. Therefore, this study was to determine the analysis method of residual spiropidion and its metabolite for the five representative agricultural products. METHODS AND RESULTS: Three QuEChERS methods (original, AOAC, and EN method) were applied to optimize the extraction method, and the EN method was finally selected by comparing the recovery test and matrix effect results. Various adsorbent agents were applied to establish the clean up method. As a result, the recovery of spiropidion was reduced when using the dispersive-SPE method with MgSO4, primary secondary amine (PSA), graphitized carbon black (GCB) and octadecyl (C18) in soybean. Color interference was minimized by selecting the case including GCB and C18 in addition to MgSO4. This method was established as the final analysis method. LC-MS/MS was used for the analysis by considering the selectivity and sensitivity of the target pesticide and the analysis was performed in MRM mode. The results of the recovery test using the established analysis method and inter laboratory validation showed a valid range of 79.4-108.4%, with relative standard deviation and coefficient of variation were less than 7.2% and 14.4%, respectively. CONCLUSION(S): Spiropidion and its metabolite could be analyzed with a modified QuEChERS method, and the established method would be widely available to ensure the safety of residual insecticides in Korea.

Effect of Planting Date and Hybrid on the Agronomic Characteristics, Forage Production and Feed Value of Corn for Silage (파종시기 및 품종이 사일리지용 옥수수의 생육특성, 사초생산성 및 사료가치에 미치는 영향)

  • Bae, Myeong Jin;Chung, Sung Heon;Kim, Jong Duk
    • Journal of The Korean Society of Grassland and Forage Science
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    • v.42 no.1
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    • pp.54-60
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    • 2022
  • The planting date of corn for silage has been delayed because of spring drought and double cropping system in Korea. This experiment was conducted to evaluate agronomic characteristics, forage production and feed value of corn at April and May in 2019. Experimental design was a split-plot with three replications. Planting dates (12 April and 10 May) were designated to the main plot, and corn hybrids ('P0928', 'P1543' and 'P2088') to the subplot. The silking days of the early planting date (12 April) was 79 days and that of the late planting date (10 May) was 66 days (p<0.0001), however, there were no significant differences among the corn hybrids. Ear height of the late planting date was higher than that of the early planting (p<0.05), while there were no significant differences in plant height of corn. Insect resistance at the early planting was lower than that of late planting (p<0.05), however, lodging resistance was no significant difference at planting date. The rice black streaked virus (RBSDV) infection of early planting was 3.7% and that of late planting was 0.3% (p<0.001). Dry matter (DM) contents of stover, ear and whole plant had significant difference at planting date (p<0.05). And differences in ear percentages were observed among the corn hybrids (p<0.01). And ear percentages of early maturing corn ('P0928') was higher than for other hybrids. Ear percentage at the early planting date was higher than that at the late planting date (p<0.01). DM and total digestible nutrients (TDN) yields had significant difference at planting date, however, there were no significant differences among the corn hybrids. DM and TDN yields at the late planting (21,678 kg/ha and 14,878 kg/ha) were higher than those of the early planting (13,732 kg/ha and 9,830 kg/ha). Crude protein content at the early planting date was higher than that of the late planting. Acid detergent fiber content of the late planting was lower than that of the early planting date (p<0.01), while there were no significant neutral detergent fiber content difference among the corn tested. Calculated net energy for lactation (NEL) and TDN at the early planting were higher than those of at the late planting (p<0.01). Results of this our study indicate that the late planting date (May) is better than early planting date (April) in forage yield and feed value of corn. Therefore, the delay of planting date by May was more suitable for use in cropping system.

A Study on Nutritive Values and Salt Contents of Commercially Prepared Take-Out Boxed-Lunch In Korea (한국형 시판 도시락의 영양가 및 식염함량)

  • Kim, Bok-Hee;Lee, Eun-Wha;Kim, Won-Kyung;Lee, Yoon-Na;Kwak, Chung-Shil;Mo, Sumi
    • Journal of Nutrition and Health
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    • v.24 no.3
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    • pp.230-242
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    • 1991
  • This research was conducted on the 10 take-out boxed-lunches commercially prepared in the department stores. chain stores. and the public railroad trains in Korea. Sampling was conducted from February 1990 to March 1990. Nutritive values and sodium contents of the 10 boxed-lunch samples are summarized as follows : 1) The average weight(percentage) of the cooked rice and the side dishes were 304.6g(49.4) and 312.4(506%), respectively. The weight of these samples were significantly heavier than that of Japanese style boxed-lunches. 2) The average number of the side dishes was 12. The average numbers of food items classified by the five food groups were 6.1 in protein food group, 0.3 in calcium food group. 6.0 in vitamin and mineral food group. 1.5 in carbohydrate food group, and 1.5 in oil and fat food group. 3) They contained on the average 840.7kcal of energy, 38.9g of protein, 22.7g of fat, 120.4g of carbohydrate. 300.8mg of calcium. 410.8mg of phosphours, 6.61 mg of iron. 219.8 R.E. of vitamin A, 0.46mg of thiamin, 0.67mg of riboflavin, 10.5mg of niacin, 27.5mg of ascorbic acid. Thus. except vitamin t the content of all the nutrients were higher than the value of 1/3 of the RDA for adults. 4) The high priced group(group 2) had more protein, calcuim. iron and niacin contents than the cheaper group(group 1). Probably, it's because the group 2 had more animal foods than the group 1. 5) The average energy content per unit price(100 won) was 37.3kcal and the average protein content per unit price(100 won) was 1.64g. Korena style boxed-lunches had higher energy and protein contents per unit price than Japanese style, and the group 1 higher than the group 2. 6) The average energy Proportions of Protein, carbohydrate. and fat were 18.3%, 57.4%, and 24.3%, respectively. These proportions are good enough. 7) Frequency of cooking methods for the side dishes were found in the decreasing order : pan-frying, frying, braising, seasoning, kimchi, grilling, pickling, stir-frying, steaming and fermenting. Generally simple cooking methods were used, thus the menus were lack or varieties. 8) Frequency of colors for the side dishes were found in the decreasing order : red, brown. yellow, green, black, white. Too much red pepper was used. 9) The average capacity of the containers for the staples and the side dishes were 468.1ml and 590.6ml, respectively. And the containers could not keep the food items well seperated. 10) The average contensts of sodium and salt were 2.287mg and 5.76g, in the range of 1, 398mg to 3, 489mg and 3.53g to 8.80g, respectively. These are much higher values than the recommended amount of salt.

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Development and Validation of the Analytical Method for Oxytetracycline in Agricultural Products using QuEChERS and LC-MS/MS (QuEChERS법 및 LC-MS/MS를 이용한 농산물 중 Oxytetracycline의 잔류시험법 개발 및 검증)

  • Cho, Sung Min;Do, Jung-Ah;Lee, Han Sol;Park, Ji-Su;Shin, Hye-Sun;Jang, Dong Eun;Cho, Myong-Shik;Jung, ong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.3
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    • pp.227-234
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    • 2019
  • An analytical method was developed for the determination of oxytetracycline in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). After the samples were extracted with methanol, the extracts were adjusted to pH 4 by formic acid and sodium chloride was added to remove water. Dispersive solid phase extraction (d-SPE) cleanup was carried out using $MgSO_4$ (anhydrous magnesium sulfate), PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed with LC-MS/MS using ESI (electrospray ionization) in positive ion MRM (multiple reaction monitoring) mode. The matrix-matched calibration curves were constructed using six levels ($0.001{\sim}0.25{\mu}g/mL$) and coefficient of determination ($r^2$) was above 0.99. Recovery results at three concentrations (LOQ, $10{\times}LOQ$, and $50{\times}LOQ$, n=5) were from 80.0 to 108.2% with relative standard deviations (RSDs) less than of 11.4%. For inter-laboratory validation, the average recovery was in the range of 83.5~103.2% and the coefficient of variation (CV) was below 14.1%. All results satisfied the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for oxytetracycline determination in agricultural commodities. This study could be useful for safety management of oxytetracycline residues in agricultural products.