• Title/Summary/Keyword: LC/MS/Ms

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The survey of exposure level for PFOS and PFOA in human plasma from several residential areas in Korea (주거지역별, 연령별 및 성별 인체 혈장중의 PFOS, PFOA 함유량 조사)

  • Chung, Jaeyeon;Yoon, Hae-Seong;Ryu, Hee-Young;Won, Jong Uk;Paeng, Ki-Jung;Kim, Yunje
    • Analytical Science and Technology
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    • v.21 no.3
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    • pp.183-190
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    • 2008
  • PFOS (Perfluorooctane sulfonate) and PFOA (Perfluorooctanoic acid) are environmental hormones which belong to potential future persistent organic pollutants (POPs), and it is easy to exposure to human because they are used in a wide variety of consumer products. We studied exposure route and the relativity through determining and monitoring of PFOS and PFOA in Korean plasma of metropolis, small town, rural area and industrial area. And we monitored the concentration of PFOS and PFOA regarding the gender and age. The older age is, the higher concentration of PFOS is. The mean concentration of PFOS and PFOA in men (4.74 ng/mL, 2.20 ng/mL) was higher than that in women (3.53 ng/mL, 1.17 ng/mL). In the comparison of residential areas, the mean concentration of PFOS and PFOA was the lowest in metropolitan plasma (2.47 ng/mL, 0.79 ng/mL) whereas it was the highest in the industrial area (6.57 ng/mL, 2.19 ng/mL).

A Study on the Saponin Contents and Antioxidant Activity of the Ginseng and Extruded Ginseng by Using Different Solvents for Extraction (추출 용매에 따른 인삼과 압출 성형 인삼의 사포닌 함량 및 항산화 활성 연구)

  • Kim, Sung-Hwan
    • The Korean Journal of Food And Nutrition
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    • v.24 no.4
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    • pp.528-534
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    • 2011
  • This study was conducted to investigate the changes in saponin content and antioxidant activity of crude ginseng and extruded ginseng by using different solvent extraction methods. Each of the fractions was first extracted by 80% ethanol followed by ether treatment to remove the lipid components. Water soluble components were separated by ethylacetate and water saturated butanol. Four fraction, including 80% ethanol, ethylacetate, butanol and water were obtained from crude and extruded ginsengs to analyze saponin content and antioxidant activity. Saponin content and antioxidant capacity of each of the four fractions were measured by LC/MS analysis and ORAC(Oxygen Radical Absorbance Capacity) assay, respectively. It was found that a major portion of saponin was present in ethyl acetate and water saturated butanol fractions. When extracted by 80% ethanol, ginsenoside Rb1 and Rg1 were mostly found in crude ginseng, while ginsenoside Re and Rb1 were detected in extruded ginseng. Even though Rh1 and Rg3 were found in a very small quantity in crude ginseng, there was a significant quantity of both in extruded ginseng when extracted by 80% ethanol. Similar tendency was also observed in extruded ginseng fraction when extracted with ethyl acetate and butanol. In crude ginseng, the level of Rg1 was the highest among other ginsenosides upon extraction by ethyl acetate, while Rh1 and Rg3 were predominantly found by employing similar solvent extraction in the extruded ginseng. Also, Rg1, Re and Rb1 were also found in the extruded ginseng with small quantity. Rg1, Re and Rb1 were found in crude ginseng by butanol extraction, while Rb1 and Re were extracted from the extruded ginseng. Overall, there was no difference in the saponin content between crude ginseng and extruded ginseng when extracted by butanol and water, but twice as much of saponin was obtained by 80% ethanol extraction and 6 times more saponin were obtained in ethyl acetate fraction in the extruded ginseng. Antioxidant capacity of crude ginseng as determined by ORAC assay was higher in 80% ethanol(high in many different kinds of biological compounds) and water saturated butanol(high in polar saponin) fractions than the ethyl acetate and water fractions. No difference in antioxidant capacity was observed between crude and extruded ginseng. However, antioxidant capacity of ethyl acetate and water fractions in extruded ginseng was significantly higher than crude ginseng($P$ >0.05). All the fractions in both, crude and extruded ginseng possessed antioxidant capacity and even water fractions that contained almost no saponin had some antioxidant capacity. While determining correlation coefficient between fractions in extruded ginseng by Pearson correlation, it was observed that 80% ethanol fraction was in correlation with ethyl acetate($P$ >0.01) and ethanol($P$ >0.001) and in the case of ethylacetate, correlation was observed only with butanol fraction($P$ >0.05).

Antioxidative, and Inhibitory Activities on Melanogenesis of Vitex negundo L. Leaf Extract (목형 잎 추출물의 항산화 활성과 멜라닌 생합성에 대한 저해활성)

  • Kim, A Reum;Park, Su Ah;Ha, Ji Hoon;Park, Soo Nam
    • Microbiology and Biotechnology Letters
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    • v.41 no.1
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    • pp.135-144
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    • 2013
  • The aim of this study was to evaluate various aspects of Vitex negundo L. leaf extract, such as the antioxidative activity, tyrosinase inhibitory effects, and inhibitory activities on ${\alpha}$-MSH induced melanogenesis, and active component analysis. The DPPH (1, 1-diphenyl-2-picrylhydrazyl) scavenging activities ($FSC_{50}$) of the ethyl acetate fraction and aglycone fraction of V. negundo L. leaf extract were $14.51{\mu}g/ml$ and $13.96{\mu}g/ml$, respectively. A luminol-dependent chemiluminescence assay revealed that the reactive oxygen species (ROS) scavenging activity ($OSC_{50}$) of the aglycone fraction of V. negundo L. leaf extract on ROS generated in an $Fe^{3+}$-$EDTA/H_2O_2$ system was the most prominent at $0.22{\mu}g/ml$. The protective effects of the extracts fractions of V. negundo L. leaf against the rose-bengal sensitized photohemolysis of human erythrocytes were increased in a concentration dependent manner ($1{\sim}50{\mu}g/ml$). In particular, there were greater protective effects of the aglycone fraction on the cellular membrane than that of the fat-soluble antioxidant (+)-${\alpha}$-tocopherol. The inhibitory effects ($IC_{50}$) on mushroom tyrosinase were the highest for the ethyl acetate fraction ($IC_{50}$ = $48.58{\mu}g/ml$). The inhibitory effect on ${\alpha}$-MSH induced melanogenesis in B16 melanoma cells was 41.80% at $50{\mu}g/ml$ of ethyl acetate fraction. Active component analyses by TLC, HPLC and LC/ESI-MS revealed luteolin and isoorientin. These results indicate that V. negundo L. leaf extract can be used as an antioxidant for ROS scavenging. Particularly, the luteolin and isoorientin of the ethyl acetate fraction may be applicable to new whitening cosmetics because of its inhibitory effect on mushroom tyrosinase and ${\alpha}$-MSH induced melanogenesis in B16 melanoma cells.

Development and Validation of an Analytical Method for Ametoctradin Residue Determination in Domestic Agricultural Commodities by HPLC-PDA (HPLC-PDA를 이용한 국내 유통 농산물 중 ametoctradin 잔류량 분석법 개발 및 검증)

  • Do, Jung-Ah;Kwon, Ji-Eun;Lee, Eun-Mi;Kim, Mi-Ra;Kuk, Ju-Hee;Cho, Yoon-Jae;Kang, Il-Hyun;Kim, Hyung-Su;Kwon, Kisung;Oh, Jae-Ho
    • Korean Journal of Food Science and Technology
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    • v.45 no.3
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    • pp.285-292
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    • 2013
  • This study was carried out to validate the safety of ametoctradin residues in agricultural commodities by developing an official analysis method. An analytical method was developed and validated using HPLC-PDA detectors. The samples were extracted with methanol, subsequently partitioned with dichloromethane and purified with florisil column chromatograph using acetone/hexane (30/70, v/v) as solvent. The method was validated by using grape, hulled rice, mandarin, and potato spiked with ametoctradin at 0.05 and 5.0 mg/kg, and pepper at 0.05 and 2.0 mg/kg. Average recoveries were 76-114.8% with relative standard deviation less than 10%, and the limit of detection and limit of quantification were 0.0125 and 0.05 mg/kg, respectively. The result of recoveries and overall coefficient of variation of the laboratory results from Gwangju regional Food and Drug Administration (FDA) and Daejeon regional FDA was accorded with Codex Alimentarius Commission Guideline (CAC/GL 40). Based on these results, this method was found to be appropriate for ametoctradin residue determination and can be used as the official method of analysis.

Choline and Betaine Concentrations in Breast Milk of Korean Lactating Women and the Choline and Betaine Intakes of Their Infants (한국 수유부 유즙의 콜린과 베타인 농도 및 영아의 콜린과 베타인 섭취량)

  • Jeong, Han-Ok;Suh, Yoon-Suk;Chung, Young-Jin
    • Journal of Nutrition and Health
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    • v.43 no.6
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    • pp.588-596
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    • 2010
  • Most nutrients taken by pregnant women are secreted into their breast milk. Food contains choline together with betaine, and in human body choline is oxidized to betaine which transfer methyl group. The aim of the study was to estimate the concentrations of choline and betaine in breast milk of Korean lactating women and the choline and betaine intakes of their infants. Total choline, free choline and betaine concentrations in breast milk of some lactating women living in Daejon Metropolitan city were analyzed every month by using HPLC-MS and enzymatic method during the first five months. Total choline concentrations of breast milks were 157.64 mg/L (1.52 mmol/L), 157.83 mg/L (1.52 mmol/L), 165.99 mg/L (1.60 mmol/L), 153.67 mg/L (1.48 mmol/L), 145.05 mg/L (1.39 mmol/L) by month after delivery for five months. The concentrations of total choline and free choline in breast milks were not significantly changed for the five months while the betaine concentrations gradually decreased. Daily intake of total choline of the infants appears to be adequate for the infant's requirement according to the US DRI; 124.6 mg/d, 120.9 mg/d, 126.5 mg/d 104.1 mg/d from 2nd to 5th month after birth. Free choline and betaine intakes of the infants were not significantly changed during the four months except showing decrease in betaine intake per kg body weight. Choline intakes of the infants more correlated with choline concentrations of the breast milks (r = 0.982, p = 0.000) than intake amount of the breast milk (r = 0.414, p = 0.028). These results suggest that the choline intake of Korean breast-fed infants appears to be adequate and the intake could be affected by the choline concentration of the breast milk.

Effects of Extraction Method on Anserine, Protein, and Iron Contents of Salmon (Oncorhynchus keta) Extracts (연어(Oncorhynchus keta) 추출물 중의 Anserine, 단백질 및 철분 함량에 미치는 추출방법의 영향)

  • Min, Hye-Ok;Park, In-Myoung;Song, Ho-Su
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.46 no.2
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    • pp.220-228
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    • 2017
  • Effects of extraction methods on reducing concentrations of pro-oxidants (total iron and protein) of salmon was determined. For development of the extraction process, the effectiveness of several extraction methods was determined and compared, including heat treatment (60, 80, and $100^{\circ}C$), ion exchange and carboxymethyl (CM)-cellulose column chromatography, and ultrafiltration (UF). Protein, total iron, and anserine contents of salmon extracts were 23.64 mg/mL, $16.20{\mu}g/mL$, and 5.47 mg/mL in non-heated extracts, 7.40 mg/mL, $2.32{\mu}g/mL$, and 5.20 mg/mL in heated extracts at $60^{\circ}C$, 7.64 mg/mL, $1.20{\mu}g/mL$, and 5.21 mg/mL at $80^{\circ}C$, and 7.04 mg/mL, $0.68{\mu}g/mL$, and 4.04 mg/mL at $100^{\circ}C$, respectively. Heating and UF decreased contents of protein and total iron, whereas only UF slightly decreased anserine content. Application of the primary ion exchange method increased the content of anserine up to 16%. Protein and total iron contents by the primary ion exchange method decreased by 70 and 98%, respectively. Secondary ion exchange (CM-cellulose) treatment after primary ion exchange and UF resulted in lower anserine content than the primary ion exchange method. However, the content of impurities (protein, total iron) was lower than in all other salmon extracts. Therefore, primary ion exchange, UF, and secondary ion exchange method were the best extraction processes in this study.

Establishment of an Analytical Method for Determination of Fungicide Oxathiapiprolin in Agricultural Commodities using HPLC-UV Detector (HPLC-UVD를 이용한 농산물 중 살균제 Oxathiapiprolin의 잔류분석법 확립)

  • Jang, Jin;Kim, Heejung;Do, Jung Ah;Ko, Ah-Young;Lee, Eun Hyang;Ju, Yunji;Kim, Eunju;Chang, Moon-Ik;Rhee, Gyu-Seek
    • Journal of Food Hygiene and Safety
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    • v.31 no.3
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    • pp.186-193
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    • 2016
  • An analytical method was developed for the determination of oxathiapiprolin in agricultural commodities. Oxathiapiprolin is a new oomycide (fungicide of piperidinyl thiazole isoxazoline class) which controls downy mildew in cucurbits caused by Pseudoperonospora cubensis (oomycete plant pathogen). Agricultural commodities were extracted with acetonitrile and partitioned with dichloromethane to remove the interference, adjusting pH between 9 and 10 by 1 N sodium hydroxide. After purification by silica SPE cartridge to clean up the interference of organic compounds, they were finally quantified by HPLC-UVD (high performance liquid chromatograph ultraviolet detector) using a wavelength at 260 nm and confirmed by LC-MS (liquid chromatograph mass spectrometer) in electro-spray ionization positive ion mode. The standard calibration curve was linear with coefficients of determination ($r^2$) 1.00 over the calibration ranges (0.025-2.5 mg/L). Recoveries were ranged between 86.7 to 112.7%, with relative standard deviations less than 10% at three concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates. The overall results were determined and estimated according to the CODEX guidelines (CAC/GL40). The proposed method for determination of oxathiapiprolin residues in agricultural commodities can be used as an official method.

Hypoglycemic Effect of Culture Broth of Bacillus subtilis S10 Producing 1-Deoxynojirimycin (1-Deoxynojirimycin을 생산하는 Bacillus subtilis S10 배양액의 혈당강하 효과)

  • Cho, Yong-Seok;Park, Young-Shik;Lee, Jae-Yeon;Kang, Kyung-Don;Hwang, Kyo-Yeol;Seong, Su-Il
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.37 no.11
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    • pp.1401-1407
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    • 2008
  • 1-Deoxynojirimycin (DNJ) is a strong $\alpha$-glucosidase inhibitor which inhibits hyperglycemia in animals. To select the Bacillus strains highly producing DNJ, 4,000 strains were isolated from soil and grain samples. By the inhibitory activity against $\alpha$-glucosidase, nine Bacillus strains were selected and then identified by 16S rDNA sequencing. B. subtilis S10 was finally selected as the best strain for the production of DNJ. Various carbon sources and nitrogen sources in culture medium were evaluated for the highest production of DNJ. As the results, the optimized concentration of carbon source and nitrogen source was 1.0% galactose and 1.6% polypeptone and the concentration of DNJ produced was 0.75 g/L. The effect of culture supernatant of B. subtilis S10 on lowering blood glucose level was investigated in streptozotocin (STZ)-induced diabetic mice model. Mice were randomly assigned to control group (saline) and three test groups such as acarbose group, silkworm powder group and B. subtilis S10 group. After eight-week oral feeding, blood glucose levels of the B. subtilis S10 and silkworm powder groups were respectively $209.1{\pm}19.6\;mg/dL$ (59.1%) and $208.6{\pm}39.8\;mg/dL$ (59.0%) lower than $510{\pm}10\;mg/dL$ of the control group. These results indicated that the culture supernatant of B. subtilis S10 was able to reduce the blood glucose level in STZ-induced diabetic mice.

Phytochemical Contents and Antioxidant Activities of Opuntia ficus-indica var. saboten (보검선인장의 Phytochemical 함량 분석 및 항산화 활성)

  • Jeong, Yun Sook;Lee, Sang Hoon;Song, Jin;Hwang, Kyung-A;Noh, Geon Min;Jang, Da Eun;Hwang, In Guk
    • The Korean Journal of Food And Nutrition
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    • v.29 no.5
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    • pp.767-776
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    • 2016
  • The aim of this study was to evaluate key properties of the prickly pear cactus (Opuntia ficus-indica var. saboten (OFI) ie, levels of key chemicals (carotenoids, flavonoids and polyphenolic compounds as well as phenolic acid) and its antioxidative potential, depending on where the plant had been cultivated in Korea. The levels of flavonoids and polyphenolic compounds in OFI were 55.45~65.32 mg (+)-catechin/g and 149.00~181.15 mg gallic acid/g, respectively. Protocatechuic acid was the most abundant phenolic acid in the ON1 and ON2 (161.90 and $196.25{\mu}g/g$ DW (dry weight)). Nineteen flavonoids were identified and analyzed by LC-ESI-MS in cladodes from OFI. Narcissin was the most abundant flavonoid in all of the samples ($1,241.89{\sim}1,775.10{\mu}g/g$ DW). Capxanthin and zeaxanthin were the most abundant carotenoids in OFI (64.88~128.08 and $48.10{\sim}93.82{\mu}g/g$ DW). The level of DPPH radical and ABTS radical scavenging activities in OFI were 10.78~25.35 and 16.85~34.16 mg AA eq/100 g, respectively. OFI by cultivar has different kind of phenolic acid, flavonoids, and carotenoids. Therefore, dietary intake of cladodes from OFI may be helpful for improving human health.

Protective effect on neuronal cells of Orostachys japonicus A. Berger extract against reactive oxygen species-induced neuronal cytotoxicity and active compounds (활성 산소종으로 야기된 산화스트레스에 대한 와송 추출물의 신경세포 보호효과 및 주요 생리활성물질)

  • Park, Su Bin;Lee, Du Sang;Kang, Jin Yong;Kim, Jong Min;Park, Seon Kyeong;Kang, Jeong Eun;Kwon, Bong Seok;Park, Sang Hyun;Lee, Chang Jun;Lee, Uk;Heo, Ho Jin
    • Korean Journal of Food Science and Technology
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    • v.49 no.5
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    • pp.524-531
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    • 2017
  • The study aimed to investigate the antioxidant activity and neuroprotective effect of the ethyl acetate fraction from Orostachys japonicus A. Berger extract (EFOJ) and its main constituent compounds. Among all fractions, the highest content of total phenolics was found in EFOJ. The antioxidant activity of EFOJ was confirmed through the 2,2-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid (ABTS), 1-1-diphenyl-2-picryl-hydrazyl (DPPH), ferric reducing antioxidant power (FRAP) assays and the inhibitory effect of malondialdehyde (MDA). In addition, we ascertained that EFOJ not only decreased the intracellular ROS level, but also protected the neuronal cells against $H_2O_2$-induced oxidative stress. In liquid chromatography-mass spectrometry analysis, the following were found to be the main compounds of EFOJ: quercetin-3-O-glucoside, kaempferol-3-O-rutinoside, kaempferol-3-O-glucoside, and kaempferol-3-O-rhamnoside. Consequently, these results suggested that the protective effect on neuronal cells was based on the antioxidant activities of the physiologically active compounds of Orostachys japonicus A. Berger extract, which could therefore help to mitigate neurodegenerative diseases.