• 제목/요약/키워드: extraction chromatography

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SPME/GC-MS를 이용한 혈액중의 호모시스테인, 메치오닌 및 시스테인의 분석 (Determination of Homocysteine, Methionine, Cysteine in Human Plasma with SPME/GC-MS)

  • 유은아;김정수;명승운
    • 분석과학
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    • 제13권6호
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    • pp.736-742
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    • 2000
  • SPME/GC-MS 방법을 이용하여 호모시스테인, 메치오닌 및 시스테인의 혈액중의 함량을 측정하고 관상동맥질환과 호모시스테인의 함량과의 관계를 조사하였다. 혈액중의 호모시스테인, 메치오닌 및 시스테인은 관상동맥질환의 위해성에 대한 생체표식인자로 알려지고 있다. 관상동맥질환자들에 대한 이들의 함량분포는 호모시스테인의 경우 $18.47-33.38{\mu}mol/L$,메치오닌피 경우는 $30.16-55.72{\mu}mol/L$ 그리고 시스테인의 경우는 $183.16-387.32{\mu}mol/L$ 범위의 함량을 보였다. 이 방법은 시간과 노력이 절약되고 또한 용매의 제한 사용으로 훨씬 환경 친화적인 방법임을 시사하였다.

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Determination of nadolol enantiomers in human plasma using a coupled achiral-chiral high-performance liquid chromatography method

  • Lee, Seung-Beom;Pham, Thuy-Vy;Mai, Xuan-Lan;Le, Thi-Anh-Tuyet;Nguyen, Thi-Ngoc-Van;Kang, Jong-Seong;Mar, Woongchon;Kim, Kyeong Ho
    • 분석과학
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    • 제33권2호
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    • pp.59-67
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    • 2020
  • Nadolol is a β-blocker drug, which effectively manages hypertension and angina pectoris. Its chemical structure allows the formation of four possible stereoisomers. A coupled column high-performance liquid chromatographic (HPLC) system with UV and fluorescence detection was investigated for simultaneously determining four nadolol enantiomers in human plasma. The plasma samples were prepared using a convenient liquid-liquid extraction process and passed through HPLC. Nadolol was initially separated from the endogenous compounds or other impurities in human plasma on a Phenomenex silica column, and its enantiomers were resolved and determined on a Chirapak AD-H column. The developed HPLC method achieved an effective chiral separation and significantly eliminated endogenous compound interference. This optimal HPLC method was validated following FDA guidelines. The results showed good selectivity, linearity, accuracy (90.50 % - 105.27 %), and precision (RSDs < 9.52 %) for each enantiomer. This method was also successfully applied to determine nadolol enantiomers in the plasma samples of a healthy male volunteer (after orally administering 80 mg racemic nadolol), proving its suitability for nadolol stereoselective pharmacokinetic studies.

채취시기에 따른 우엉 잎의 휘발성 향기성분 분석 (Analyses of the Volatile Flavor Composition of Burdock (Arctium lappa L.) Leaves according to Harvesting Season)

  • 최향숙
    • 한국식품영양학회지
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    • 제31권2호
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    • pp.220-228
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    • 2018
  • This study investigated the chemical composition of burdock (Arctium lappa L.) leaves essential oil, and the quantitative changes of the major terpene compounds according to the specific harvesting season. The essential oils obtained by the hydrodistillation extraction (HDE) method from the aerial parts of the burdock leaves were analyzed by gas chromatography (GC) and GC-mass spectrometry (GC-MS). The essential oil composition of this plant was characterized by the higher content of phytol and 6,10,14-trimethyl-2-pentadecanone. Seventy seven (98.28%) volatile flavor compounds were identified in the essential oil from the burdock leaves harvested during the spring season of 2012, and phytol (33.47%) and 6,10,14-trimethyl-2-pentadecanone (32.47%) were the most abundant compounds. Eighty eight (99.08%) compounds were identified in the essential oil from the leaves harvested during the autumn season of 2012, and in this case, phytol (37.35%) and 6,10,14-trimethyl-2-pentadecanone (34.67%) were also the most abundant compounds. These two volatile components were confirmed as the major oil components of the burdock leaves during the time of any harvest. The ratio between the two components contained in the burdock essential oils did not differ significantly by harvesting season. But overall, the essential oil harvested during the spring season contained 65.94% of the two major components, while for the essential oil harvested during the autumn season, the total amount of these two major components was 72.02%. While the main ingredients of the essential oils were found to be unchanged from one harvest time to the next, it was found to differ in content. For the burdock leaves, the quality index of the volatile constituents according to the harvest time would be more useful for utilizing the total quantity other than the proportion between phytol and 6,10,4-trimethyl-2-pentadecone.

구절초와 쑥부쟁이 정유의 휘발성 향기성분 분석 (Analyses of the Volatile Flavor Composition of Essential Oils from Chrysanthemum zawadskii var. latilobum Kitamura and Aster yomena Makino)

  • 최향숙
    • 한국식품영양학회지
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    • 제31권3호
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    • pp.378-387
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    • 2018
  • This study investigated the volatile flavor composition of essential oils from Chrysanthemum zawadskii var. latilobum Kitamura and Aster yomena Makino. The essential oils obtained by the hydrodistillation extraction method from the aerial parts of the plants were analyzed by gas chromatography (GC) and GC-mass spectrometry (GC-MS). One hundred (95.04%) volatile flavor compounds were identified in the essential oil from the C. zawadskii var. latilobum Kitamura. The major compounds were valencene (10.82%), ${\delta}$-cadinol (9.77%), hexadecanoic acid (8.70%), 2-methyl-4-(2,6,6-trimethylcyclohex-1-enyl) but-2-en-1-ol (3.67%), and 2-(2,4-hexadiynylidene)-1,6-dioxaspiro[4,4]non-3-ene (3.57%). Ninety-eight (93.83%) volatile flavor compounds were identified in the essential oil from the Aster yomena Makino. The major compounds were and 3-eicosyne (13.61%), 9,10,12-octadecatrienoic acid (7.8%), ${\alpha}$-caryophyllene alcohol (6.83%), 9-octadecynoic acid (6.03%), and ${\alpha}$-caryophyllene (5.74%). Although the two plants are apparently very similar, the chemical composition of the essential oils was significantly different in quality and quantity. In the case of C. zawadskii var. latilobum Kitamura, the sesquiterpene, valencene was found to be 10.82%, but it was not identified in A. yomena Makino. ${\delta}$-Cadinol appeared higher in C. zawadskii var. latilobum Kitamura than in A. yomena Makino. A clear characteristic of A. yomena Makino essential oil is that it has a high content of caryophyllene derivatives. The ${\alpha}$-caryophyllene alcohol contained in A. yomena Makino was relatively high at 6.83%, although the compound was not identified in C. zawadskii var. latilobum Kitamura. Also ${\alpha}$-caryophyllene was shown to be higher in A. yomena Makino than in C. zawadskii var. latilobum Kitamura.

키조개 부산물 단백질 가수분해물의 휘발성 향기성분에 관한 연구 (Volatile Flavor Compounds in Pen Shell By-product Hydrolysate)

  • 차용준;김은정
    • 한국식품과학회지
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    • 제27권6호
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    • pp.964-971
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    • 1995
  • 키조개 부산물로 부터 향미제로 응용하기 위하여 제조한 가수분해물의 유리아미노산 및 휘발성 향기성분을 분석한 결과, 유리아미노산의 경우 가수분해물이 생시료에 비해 3배 이상 증가하였으며 taurine의 함량이 가장 많았다. 그리고 생시료와 가수분해물의 휘발성 향기성분을 분석한 결과 총 109종의 화합물이 동정되었는데 이중에서 생시료는 88종, 가수분해물은 65종이 검출되었다. 그리고 이들은 주로 알데히드류(16종), 케톤류(17종), 알콜류(31종), 함질소화합물류(16종), 방향족화합물류(8종), 에스테르류(3종) 및 기타 화합물류(17종)으로 구성되어 있었다. 특히 생시료에서의 산화취 성분인 알데히드류 및 방향족화합물은 가수분해물에서 상당량 감소되었으며 반면에 고소한 향기성분인 heterocyclic 화합물이 상당량 검출되었다.

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Fatty Acid Composition and Volatile Constituents of Protaetia brevitarsis Larvae

  • Yeo, Hyelim;Youn, Kumju;Kim, Minji;Yun, Eun-Young;Hwang, Jae-Sam;Jeong, Woo-Sik;Jun, Mira
    • Preventive Nutrition and Food Science
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    • 제18권2호
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    • pp.150-156
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    • 2013
  • A total of 48 different volatile oils were identified form P. brevitarsis larvae by gas chromatography/mass spectrometry (GC/MS). Acids (48.67%) were detected as the major group in P. brevitarsis larvae comprising the largest proportion of the volatile compounds, followed by esters (19.84%), hydrocarbons (18.90%), alcohols (8.37%), miscellaneous (1.71%), aldehydes (1.35%) and terpenes (1.16%). The major volatile constituents were 9-hexadecenoic acid (16.75%), 6-octadecenoic acid (14.88%) and n-hexadecanoic acid (11.06%). The composition of fatty acid was also determined by GC analysis and 16 fatty acids were identified. The predominant fatty acids were oleic acid ($C_{18:1}$, 64.24%) followed by palmitic acid ($C_{16:0}$, 15.89%), palmitoleic acid ($C_{16:1}$, 10.43%) and linoleic acid ($C_{18:2}$, 4.69%) constituting more than 95% of total fatty acids. The distinguished characteristic of the fatty acid profile of P. brevitarsis larvae was the high proportion of unsaturated fatty acid (80.54% of total fatty acids) versus saturated fatty acids (19.46% of total fatty acids). Furthermore, small but significant amounts of linoleic, linolenic and ${\gamma}$-linolenic acids bestow P. brevitarsis larvae with considerable nutritional value. The novel findings of the present study provide a scientific basis for the comprehensive utilization of the insect as a nutritionally promising food source and a possibility for more effective utilization.

사람치아 단백질을 분리 흡착한 PVDF막의 생체반응에 관한 연구 (BIOASSAY OF HUMNA TOOTH PROTEIN BLOTTED POLYVINYLIDENE DIFLUORIDE(PVDF)MEMBRANE)

  • 강나라;홍종락;정필훈
    • Journal of the Korean Association of Oral and Maxillofacial Surgeons
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    • 제30권3호
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    • pp.186-192
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    • 2004
  • Purpose: Human tooth proteins are highly heterogeneous, comprising diverse proteins derived from a number of genes. The attempts to identify protein for activity of tooth matrix proteins have been defied by several factors. First, the amount of proteins within teeth is very small relative to many extracellular matrix proteins of other tissues. Second, the bioassay system is tedious and needed for long time. Therefore we tried to find easy techniques, which increase the product rate, and an assay of small proteins, with which amino acid sequence is possible without additional procedures. Materials and Methods: Total protein were extracted from 300 g enamel removed teeth and 600 g teeth with 4 mol/L guanidine HCl and purified by gel chromatography. Aliquot of proteins was implanted into muscle pouches in Sprague-Dawley rats for bioassay. By SDS-PAGE and membrane blotting, molecular weight of each protein was estimated and a partial amino acid sequence was obtained. Each fraction blotted on the membrane was cut out and inserted in rat ectopic model. Results: In dissociative method, total tooth proteins were obtained 1mg/ml from enamel removed teeth and 3.5 mg/ml from teeth. In SDS-PAGE, four clear bands at the sites corresponding to 66, 40, 20 and 18 kD. Especially The 66 kD band was clearly exhibited. Amino acid sequencing from tooth could be possible using PVDF membrane blotting technique. In amino acid sequencing, 66 kD protein was identified as albumin. Conclusion: Compared with conventional method for extraction of teeth protein and bioassay of proteins, the methods in this study were easy, time-saving and more productive technique. The matured tooth proteins omitting additional procedure of mechanical removal of enamel were simply analyzed using blotted PVDF membrane. This method seems to make a contribution as a technique for bioassay and amino acid sequencing of protein.

유기발광소자를 위한 해양 미세조류 유래 물질 및 광 발광 탐색 (Extracion and Photoluminescence Properties of Marine Microalgae for Organic Light Emitting Diode Applications)

  • 정상목;이한성;강슬기;이한주;손지수;전재혁;채희백;신현웅
    • 한국환경생태학회지
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    • 제29권4호
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    • pp.564-569
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    • 2015
  • 본 연구는 해양 미세조류에서 추출한 물질에 대한 광 발광(Photoluminescence) 측정 및 GC-MS 분석을 통해 유기발광다이오드 소자로 이용 가능한 물질을 탐색하고자 하였다. 국내에서 주로 서식하는 해양 미세조류 14종의 추출물을 분획으로 얻었으며 광 발광 측정 결과, Nitzschia denticula, Navicula cacellata, Nannochloropsis salina 총 3종의 추출물에서 광 발광 반응이 나타났다. 광 발광 반응을 보인 물질의 특성을 알아내기 위해 GC-MS로 분석하였으며, 그 결과 3종의 추출물이 imidazole, purine 및 quinoline기를 가진다는 것을 확인하였고, 이 계열의 물질들이 광 발광에 영향을 주는 것으로 판단된다.

Ginsenosides analysis of New Zealand-grown forest Panax ginseng by LC-QTOF-MS/MS

  • Chen, Wei;Balan, Prabhu;Popovich, David G.
    • Journal of Ginseng Research
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    • 제44권4호
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    • pp.552-562
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    • 2020
  • Background: Ginsenosides are the unique and bioactive components in ginseng. Ginsenosides are affected by the growing environment and conditions. In New Zealand (NZ), Panax ginseng Meyer (P. ginseng) is grown as a secondary crop under a pine tree canopy with an open-field forest environment. There is no thorough analysis reported about NZ-grown ginseng. Methods: Ginsenosides from NZ-grown P. ginseng in different parts (main root, fine root, rhizome, stem, and leaf) with different ages (6, 12, 13, and 14 years) were extracted by ultrasonic extraction and characterized by Liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry. Twenty-one ginsenosides in these samples were accurately quantified and relatively quantified with 13 ginsenoside standards. Results: All compounds were separated in 40 min, and a total of 102 ginsenosides were identified by matching MS spectra data with 23 standard references or published known ginsenosides from P. ginseng. The quantitative results showed that the total content of ginsenosides in various parts of P. ginseng varied, which was not obviously dependent on age. In the underground parts, the 13-year-old ginseng root contained more abundant ginsenosides among tested ginseng samples, whereas in the aboveground parts, the greatest amount of ginsenosides was from the 14-year-old sample. In addition, the amount of ginsenosides is higher in the leaf and fine root and much lower in the stem than in the other parts of P. ginseng. Conclusion: This study provides the first-ever comprehensive report on NZ-grown wild simulated P. ginseng.

Development of a Quantitative Analytical Method for Determining the Concentration of Human Urinary Paraben by LC-MS/MS

  • Lee, Seung-Youl;Son, Eunjung;Kang, Jin-Young;Lee, Hee-Seok;Shin, Min-Ki;Nam, Hye-Seon;Kim, Sang-Yub;Jang, Young-Mi;Rhee, Gyu-Seek
    • Bulletin of the Korean Chemical Society
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    • 제34권4호
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    • pp.1131-1136
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    • 2013
  • Parabens, the esters of p-hydroxybenzoic acid, have been widely used as antimicrobial preservatives in cosmetic products, drugs, and processed foods and beverages. However, some parabens have been shown to have weak estrogenic effects through in vivo and in vitro studies. Because such widespread use has raised concerns about the potential human health risks associated with exposure to parabens, we developed a simultaneous analytical method to quantify 4 parabens (methyl, ethyl, propyl, and butyl) in human urine, by using solid-phase extraction and high-performance liquid chromatography coupled with triple quadrupole mass spectrometry. This method showed good specificity, linearity ($R^2$ > 0.999), accuracy (92.2-112.4%), precision (0.9-9.6%, CV), and recovery (95.7-102.0%). The LOQs for the 4 parabens were 1.0, 0.5, 0.2, and 0.5 ng/mL, respectively. This method could be used for quick and accurate analysis of a large number of human samples in epidemiological studies to assess the prevalence of human exposure to parabens.