• Title/Summary/Keyword: Mass Spectrometry (MS)

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LC/MS-based metabolomics approach for selection of chemical markers by domestic production region of Schisandra chinensis (오미자(Schisandra chinensis)의 국내 산지별 화학적마커 선정을 위한 LC/MS 기반의 대사체학 접근법)

  • In Seon Kim;Seon Min Oh;Ha Eun Song;Doo-Young Kim;Dahye Yoon;Dae Young Lee;Hyung Won Ryu
    • Journal of Applied Biological Chemistry
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    • v.66
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    • pp.467-476
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    • 2023
  • Schisandra chinensis (S. chinensis) is a deciduous broad-leaved cave plant belonging to the Schisandraceae family and is widely distributed in East Asia including Korea, Japan, China, and Taiwan. It has been reported that the main components contained in S. chinensis include lignan compounds and triterpenoid compounds. To distinguish the characteristics of S. chinensis by production region of Korea, a discriminant was established by performing metabolite profiling and principal component analysis, a multivariate statistical analysis technique. As a result, 16 types of triterpenoids, 9 types of lignan, and 1 type each of flavonoid, phenylpropanoid, and fatty acid were identified. In addition, through multivariate statistical analysis, it was confirmed that the four groups in Danyang, Moongyeong, Geochang, and Pyeongchang were divided, by applying the s-plot model of orthogonal partial least squares discriminant analysis. Biomarkers were identified: lanostane, cycloartane, schiartane triterpenoid, and dibenzocyclo-octadiene lignan were identified as chemical markers, respectively.

An Improved Analytical Method for the Determination of Qualitative and Quantitative Characteristics of Di- and Trisaccharides in Honey using GC and GC/MS (GC 및 GC/MS에 의한 벌꿀 중의 이·삼당류 정성 및 정량 특성과 개선된 동시분석방법의 확립)

  • Kim, Jong-Bae;Jang, Eun-Suk;Kim, In-Suk;Lee, Hee-Jin;Lee, Hye-Jeong;Seo, Hyun-Sun;Park, Nam-Pyo
    • Korean Journal of Food Science and Technology
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    • v.47 no.1
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    • pp.27-36
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    • 2015
  • The improved analytical method with gas chromatography (GC) and GC-mass spectrometry was established to identify and quantify disaccharides and trisacchrides in honey. In this method, the analysis of trimethylsilyl (TMS), TMS-oxime and TMS-methoxime sugars takes into account the determination of a single peak of complete separation on the chromatogram. The number of possible peaks for the qualitative and quantitative determination of TMS, TMS-oxime, and TMS-methoxime sugars was 17, 22, and 25, respectively. This new analytical method allowed for the determination of diand trisaccharides in honey by TMS-oxime and TMS-methoxime derivatives. This study suggested that the improved method is more suitable and precise than the other analytical methods for the simultaneous determination of sugars in honey.

Monitoring of Pesticide Residues and Heavy Metals in Fermented Liquor in Ulsan (울산지역 유통 발효주의 잔류농약 및 중금속 실태조사)

  • Hee-Jung Kim;Kyoung-Jin Kim;Min-Kyung Kim;Geum-Bi Kim;Su-Hee Kim;Young-Kyung Jo;Ju-Eun Park;So-Yeon Jeong;Won-Dug Seo;Young-Sun Choi
    • Journal of Food Hygiene and Safety
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    • v.39 no.3
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    • pp.250-259
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    • 2024
  • In this study, we investigated in pesticide residues and heavy metals in fermented liquor products (wine, beer, makgeolli). Targeted analysis of 400 pesticide residues in the sample was performed using the quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction method, followed by gas chromatography-tandem mass spectrometry (MS/MS) and LC-MS/MS. The contents of heavy metals (Pb, Cd) were determined by ICP-MS using the microwave method. The mercury was measured using a mercury analyzer. From the analysis of 150 cases, 102 (68.0%) cases of fermented liquor were detected, and 35 pesticide residues (including metalaxyl, mandipropamid, azoxystrobin, and fenhexamid) were detected among the 400 pesticide residues tested. Pb, Cd, and Hg were tested in 150 samples. Lead was detected in 73 samples (48.7%), cadmium in 9 samples (6.0%), and mercury in 36 samples (24.0%). Exposure assessment was conducted to determine the safety of the detected pesticide residues and heavy metals. According to this assessment, the pesticide residues and heavy metals showed very low %ADI values (less than 1%).

Analysis of Geographical Origin of Red Ginseng Extract Using Mass Spectrometer-based Electronic Nose (홍삼 농축액의 원산지 판별을 위한 전자코 분석)

  • Kim, Ki Hwa;Dong, Hyemin;Han, Hyun Jung;Lee, Young Hyun;Moon, Ji Young;Bang, Kyong-Hwan;Noh, Bong Soo
    • Korean Journal of Food Science and Technology
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    • v.45 no.5
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    • pp.652-656
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    • 2013
  • The geographical origin of red ginseng extract (RGE) was studied using a mass spectrometry based electronic nose. Imported RGE and domestic RGE were diluted to 12oBx. The treated RGE was analyzed, and discriminant function analysis (DFA) was used for discriminating of geographical origins. The DFA plots indicated a significant separation of imported RGE and domestic RGE. The F-value of discriminant function first score (DF1) was much higher than that of discriminant function second score (DF2), indicating that discrimination was mainly affected by DF1. Based on DF1, the concentration of domestic RGE to imported RGE shifted to the left side of DFA plot, and the mixing ratio highly correlated to DF1 value. Unknown sample (#2) was closely located to the sample of mixed imported : domestic (6:4) RGE. In the bar graph, the DF1 value correlated to the mixing ratio. Unknown samples (#2) were thought to be mixed with the imported RGE. This technique could be used to efficiently differentiate the geographical origin of RGE.

Measuring in vivo Rate of Bone Collagen Synthesis in Growing Rats (성장기 흰쥐의 골조직 Collagen 생성속도 측정)

  • 김유경
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.32 no.8
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    • pp.1390-1393
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    • 2003
  • Measuring in vivo rate of bone collagen synthesis has so far been technically difficult and often subject to quite large errors. In the present study, bone collagen synthesis rate was measured using a precursor-product method, based on the exchange of $^2$$H_2O$ into amino acids. Mass isotopomer abundance in hydroxyproline from bone collagen was analyzed by gas chromatography/mass spectrometry. The $^2$$H_2O$ labeling protocol consisted of an initial intraperitoneal injection of 99.9% $^2$$H_2O$, to achieve approximately 2.5% body water enrichment followed by administration of 4% $^2$$H_2O$ in drinking water for 9 weeks. Body $^2$$H_2O$ enrichments were stable at 2.7 ∼ 3.0% over labeling Period. In growing rats, the fractional synthesis rate ( $k_{s}$) of bone collagen was 0.066 $\pm$ 0.049 w $k^{-1}$ . The unique features of stable $^2$$H_2O$ pools and label incorporation allowed the precursor-product approach to be used for measuring bone collagen synthesis rate..

Phytochemical Analysis and Anti-cancer Investigation of Boswellia Serrata Bioactive Constituents In Vitro

  • Ahmed, Hanaa H;Abd-Rabou, Ahmed A;Hassan, Amal Z;Kotob, Soheir E
    • Asian Pacific Journal of Cancer Prevention
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    • v.16 no.16
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    • pp.7179-7188
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    • 2015
  • Cancer is a major health obstacle around the world, with hepatocellular carcinoma (HCC) and colorectal cancer (CRC) as major causes of morbidity and mortality. Nowadays, there isgrowing interest in the therapeutic use of natural products for HCC and CRC, owing to the anticancer activity of their bioactive constituents. Boswellia serrata oleo gum resin has long been used in Ayurvedic and traditional Chinese medicine to alleviate a variety of health problems such as inflammatory and arthritic diseases. The current study aimed to identify and explore the in vitro anticancer effect of B. Serrata bioactive constituents on HepG2 and HCT 116 cell lines. Phytochemical analysis of volatile oils of B. Serrata oleo gum resin was carried out using gas chromatography-mass spectrometry (GC/MS). Oleo-gum-resin of B. Serrata was then successively extracted with petroleum ether (extract 1) and methanol (extract 2). Gas-liquid chromatography (GLC) analysis of the lipoidal matter was also performed. In addition, a methanol extract of B. Serrata oleo gum resin was phytochemically studied using column chromatography (CC) and thin layer chromatography (TLC) to obtain four fractions (I, II, III and IV). Sephadex columns were used to isolate ${\beta}$-boswellic acid and identification of the pure compound was done using UV, mass spectra, $^1H$ NMR and $^{13}C$ NMR analysis. Total extracts, fractions and volatile oils of B. Serrata oleo-gum resin were subsequently applied to HCC cells (HepG2 cell line) and CRC cells (HCT 116 cell line) to assess their cytotoxic effects. GLC analysis of the lipoidal matter resulted in identification of tricosane (75.32%) as a major compound with the presence of cholesterol, stigmasterol and ${\beta}$-sitosterol. Twenty two fatty acids were identified of which saturated fatty acids represented 25.6% and unsaturated fatty acids 74.4% of the total saponifiable fraction. GC/MS analysis of three chromatographic fractions (I,II and III) of B. Serrata oleo gum resin revealed the presence of pent-2-ene-1,4-dione, 2-methyl- levulinic acid methyl ester, 3,5- dimethyl- 1-hexane, methyl-1-methylpentadecanoate, 1,1- dimethoxy cyclohexane, 1-methoxy-4-(1-propenyl)benzene and 17a-hydroxy-17a-cyano, preg-4-en-3-one. GC/MS analysis of volatile oils of B. Serrata oleo gum resin revealed the presence of sabinene (19.11%), terpinen-4-ol (14.64%) and terpinyl acetate (13.01%) as major constituents. The anti-cancer effect of two extracts (1 and 2) and four fractions (I, II, III and IV) as well as volatile oils of B. Serrata oleo gum resin on HepG2 and HCT 116 cell lines was investigated using SRB assay. Regarding HepG2 cell line, extracts 1 and 2 elicited the most pronounced cytotoxic activity with $IC_{50}$ values equal 1.58 and $5.82{\mu}g/mL$ at 48 h, respectively which were comparable to doxorubicin with an $IC_{50}$ equal $4.68{\mu}g/mL$ at 48 h. With respect to HCT 116 cells, extracts 1 and 2 exhibited the most obvious cytotoxic effect; with $IC_{50}$ values equal 0.12 and $6.59{\mu}g/mL$ at 48 h, respectively which were comparable to 5-fluorouracil with an $IC_{50}$ equal $3.43{\mu}g/mL$ at 48 h. In conclusion, total extracts, fractions and volatile oils of B. Serrata oleo gum resin proved their usefulness as cytotoxic mediators against HepG2 and HCT 116 cell lines with different potentiality (extracts > fractions > volatile oil). In the two studied cell lines the cytotoxic acivity of each of extract 1 and 2 was comparable to doxorubicin and 5-fluorouracil, respectively. Extensive in vivo research is warranted to explore the precise molecular mechanisms of these bioactive natural products in cytotoxicity against HCC and CRC cells.

Analysis of ethyl glucuronide (EtG) in Hair for the diagnosis of chronic alcohol abuse of Korean (한국인의 만성 알코올 중독 진단을 위한 모발에서 Ethyl Glucuronide (EtG) 분석법 연구)

  • Gong, Bokyoung;Jo, Young-Hoon;Ju, Soyeong;Min, Ji-Sook;Kwon, Mia
    • Analytical Science and Technology
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    • v.33 no.3
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    • pp.151-158
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    • 2020
  • Alcohol, which can easily be obtained in the same way as ordinary beverages, is harmful enough to cause death due to excessive drinking and chronic alcohol intake, so it is important to maintain a proper amount of drinking and healthy drinking habits. In addition, the incidence of behavioral disturbances and impaired judgments that can be caused by chronic alcohol drinking of more than adequate amounts of alcohol is also significant. Accordingly it is very useful for forensic science to check whether the person involved is drunken or is alcoholism state in various accidents. Currently, in Korea, alcohol consumption is determined by detecting the level of alcohol or alcohol metabolism 'ethyl glucuronide (EtG)' in blood or urine samples. However, analysis of alcohol or EtG in blood or urine can only provide information about the current state of alcohol consumption because of a narrow window of detection time. Therefore, it is important to analyze the EtG as a long-term direct alcohol metabolite bio-marker in human hair and to investigate relationship between alcohol consumption and EtG concentration for the evaluation of chronic ethanol consumption. In this study, we established an analytical method for the detection of EtG in Korean hair efficiently and validated selectivity, linearity, limits of detection (LOD), limits of quantification (LOQ), matrix effect, recovery, process efficiency, accuracy and precision using liquid chromatography tandem mass spectrometry (LC-MS/MS). In addition, the assay performance was evaluated in Korean social drinker's hair and the postmortem hair of a chronic alcoholism. The results of this study can be useful in monitoring the alcohol abuse of Korean in clinical cases and legal procedures related to custody and provide a useful tool to evaluate postmortem diagnosis of alcoholic ketoacidosis in forensics.

Chemical Composition and Antiproliferative Activity of Supercritical Extract of Immature Citrus Peel in human cervical carcinoma HeLa cells (미성숙 감귤 과피 초임계 추출물의 성분 분석과 자궁암세포 성장억제효능)

  • Moon, Jeong Yong;Song, YeonWoo;Hyun, Ho Bong;KimCho, Somi
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.16 no.12
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    • pp.8836-8843
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    • 2015
  • This study was performed to investigate the antiproliferative activities of supercritical extracts from phalsak(Citrus hassaku Hort ex Tanaka) and yeagam(Citrus iyo Hort. ex Tanaka) against human cervical carcinoma HeLa cells and the chemical compositions of the extracts. The anticancer properties of supercritical extracts were demonstrated using the MTT assay and Hoechst 33342 staining and the compositional analyses were conducted by using gas chromatography-mass spectrometry(GC-MS). The peel extracts of both species exhibited similar antiproliferative effect. The antiproliferative activity of the flesh extracts was not detected up to $400{\mu}g/mL$, whereas peel extracts of phalsak and yeagam reduced cell viability with 87.16% and 92.95% at $400{\mu}g/mL$, respectively. There was a dramatic increase of the apoptotic body formation in the cell treated with peel extracts while no apoptotic body formation detected in the cell treated with flesh extracts at 100, $200{\mu}g/mL$. By GC-MS analysis, 27 and 31 kinds of compounds identified in flesh and peel of phalsak, while 27 and 29 kinds of compounds were identified in flesh and peel of yeagam, respectively. 1,1,4,4-Tetramethyl-2-tetralone(20.86%), alloimperatorin(8.15%), limonene(11.23%), and auraptene(7.29%) were major in peel of phalsak, whereas limonene(22.19%), linalool(11.23%), and ${\gamma}$-sitosterol(9.12%) were major in peel of yeagam.

Quality Standardization and Isoflavone Glycoside Research of in Buseoktae(Yeongju bean) Cheonggukjang for Business Use from Yeongju Bean (영주 부석태 청국장시료의 이소플라본 배당체 탐색과 청국장의 품질 표준화)

  • Choi, Eun-Young;Yu, Jin-Hyeon;An, Hui-Jeong
    • Culinary science and hospitality research
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    • v.22 no.2
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    • pp.13-28
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    • 2016
  • This study performed quantitative analysis of isoflavone glycoside contents on Buseoktae, Daewon, Wooram beans and cheonggukjang made of Buseoktae beans from the LC/MS/MS. Also, the experiment carried out by means of RSM(response surface methodology), which included 10 experimental points for the two independent variables addition(40, 55, 70 g) and time(2, 3, 4 min) from the beginning point to boil of cheonggukjang. These were optimized using a Face-centered central composite design. Daidzein contents were $212.16{\mu}g/mL$ in Buseoktae, $212.21{\mu}g/mL$ in daewon, $158.54{\mu}g/mL$ in wooram beans. Genistein contents were $318.84{\mu}g/mL$ in Buseoktae, $310.50{\mu}g/mL$ in daewon, $262.71{\mu}g/mL$ in wooram beans. Total isoflavone contents were $532.50{\mu}g/mL$ in Buseoktae, $524.19{\mu}g/mL$ in Daewon, $422.71{\mu}g/mL$ in Wooram beans. Isoflavone contents of Buseoktae and Daewon were quite similar, relatively contents of Wooram beans were low. Total isoflavone contents of Buseoktae cheonggukjang (for business use) was $430.10{\mu}g/mL$ in A ($32^{\circ}C$, 96 h fermentation), $460.09{\mu}g/mL$ in B ($36{\sim}40^{\circ}C$, 30 h fermentation), $417.46{\mu}g/mL$ in C cheonggukjang($36{\sim}38^{\circ}C$, 72 h fermentation), B cheonggukjang was just a bit more than A, C cheonggukjang. The estimated response surfaces confirmed that the amount and time had significant effects on taste. The optimum condition of Buseoktae cheonggukjang taste was predicted to be 55.20 g addition at 2.92 min.

Study on the Analytical Method and Monitoring of the Oxidized Polyethylene Wax in Foods (식품 중 oxidized polyethylene wax 분석법 연구 및 함유량 실태 조사)

  • Choi, Seung-Hyun;Kim, Jae-Min;Choi, Sun-il;Jung, Tae-Dong;Cho, Bong-Yeon;Lee, Jin-Ha;Lee, Gunyoung;Lim, Ho Soo;Yun, Sang Soon;Lee, Ok-Hwan
    • Journal of Food Hygiene and Safety
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    • v.32 no.4
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    • pp.284-289
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    • 2017
  • Oxidized polyethylene wax (OPEW) is, one of the food additives, used as a coating agent in citrus fruits and nuts. OPEW is authorized to quantum satis in EU, USA, and is acceptable less than 250 mg/kg in Australia and New Zealand. But OPEW is unauthorized as a food additive in Korea. This study was to establish the analytical method of OPEW and demonstrate the effective application of various food samples. We first conducted to compare the various analytical method including acid value (AV), high temperature gel permeation chromatography (HT-GPC), matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF/MS), gas chromatography flame ionization detector (GC-FID) and fourier transform infrared spectroscopy (FT-IR). This result indicated that FT-IR spectrum of OPEW treated food sample displayed absorption bands for carbonyl group (C=O, $1714cm^{-1}$), ester group (C-O, $1463cm^{-1}$), aliphatic group (C-H, $2916cm^{-1}$). Furthermore, IR spectrum of OPEW treated food sample showed similar tendency with IR spectrum of OPEW standard. Therefore, it is confirmed that analytical method using FT-IR can be detected on analysis of OPEW in food. As a result of monitoring of 111 samples using established analytical method, OPEW was not detected in the food samples.