• 제목/요약/키워드: gas-liquid chromatography

검색결과 498건 처리시간 0.03초

지렁이(지룡)의 해열성분에 관한 연구 (Studies of Antipyretic Component of the Earthworm)

  • 김영은;이왕규;윤희정
    • 약학회지
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    • 제25권4호
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    • pp.137-143
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    • 1981
  • In order to confirm the exact antipyretic component in the earthworm, etherial extract of American earthworm(Red Worm) was fractionated into five fractions by using silica gel column chromatography and thin layer chromatography. The fraction including free fatty acids was found to possess artipyretic response and standard arachidonic acid showed marked antipyretic response on typhoid vaccinated rabbits. Arachidonic acid was identified from the free fatty acid fraction of the earthworm by using gas liquid chromatography. Thus it was considered that the antipyretic activity of the free fatty acid may be due to the presence of arachidonic acid. Lipid-free earthworm powder was extracted with phosphate buffer (pH, 8.0, 0.1M) and all the proteins was salted out by ammonium sulfate. The crude precipitate was dialyzed and the impure proteins were eliminated at pH 5.4 and 4.6. The remaining protein solution was fractionated with various concentrations of acetone. The acetone fractions were identified by using S.D.S. polyacrylamide gel electrophoresis and disc gel electrophoresis. The precipitate at 85% acetone concentration and the remaining proteins in the supernatant did not exhibit the antipyretic activity.

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첨가제를 이용한 액체연료의 열안정성 향상 (Thermal Stability Improvement of Liquid Fuel by Using Some Additives)

  • 박선희;김중연;전병희;한정식;정병훈;김성현
    • 한국추진공학회:학술대회논문집
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    • 한국추진공학회 2010년도 제35회 추계학술대회논문집
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    • pp.294-299
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    • 2010
  • 본 연구의 목적은 열안정성을 향상시키는 첨가제 (열안정제)를 이용하여 exo-tetrahydrodicyclopentadiene (exo-THDCP, $C_{10}H_{16}$)의 열안정성을 향상시키는 것이다. 실험은 반응 진행 중 미량의 시료 추출이 가능한 회분식 반응기에서 수행되었다. 추출한 시료를 gas chromatography-mass spectrometry (GC-MS)를 이용해 성분 분석하여 첨가제 성능-exo-THDCP의 열분해성-을 확인하고, 반응시간에 따른 exo-THDCP의 분해생성물의 성분 및 조성 변화를 통해 첨가제의 작용 메커니즘을 규명하였다. 열안정제로써 수소공여체를 사용하여 실험한 결과 1,2,3,4-tetrahydroquinoline (THQ), benzyl alcohol (BnOH) 등을 첨가하였을 때 exo-THDCP의 열안정성이 향상되었다. 이러한 수소공여체 물질들은 개시반응이 진행된 exo-THDCP 라디칼에 수소원자 (hydrogen radical)를 제공함으로 라디칼의 반응성을 완화시켜 1차 생성물의 활성을 감소시키어 2차생성물질인 $C_{11}$ 이상 생성물의 발생을 감소시키는 것으로 밝혀졌다.

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Study on the Development and Functional Characteristics of Salted Egg with Liquid Smoke

  • Putri Widyanti Harlina;Tri Yuliana;Fetriyuna;Raheel Shahzad;Meihu Ma
    • 한국축산식품학회지
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    • 제43권3호
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    • pp.471-490
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    • 2023
  • In this study, the duck eggs were salted with none or 2.5% and 5.0% (v/v) of liquid smoke (LS), respectively. As a control, samples salted without LS were used. The 2-thiobarbituric acid (TBA) values, 1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging ability, and reducing power of the three groups were tested at 0, 7, 14, and 21 and 28 days to determine the effects of LS on the antioxidant activity of treated eggs. In addition, gas chromatography-mass spectrometry (GC-MS) and electronic nose (E-Nose) were used to analyze the volatile flavor components of fresh duck eggs, LS, control, and salted duck eggs enriched with 2.5% (v/v) LS after 28 days of salting. The TBA value considerably increased with an increase in salting period, and the treated egg's TBA value significantly associated with LS concentration. The TBA value decreased as the LS concentration increased. The amount of LS present was highly associated with their capacity to scavenge DPPH radicals. The reducing power of the samples was substantially correlated with the LS concentration, and the reducing power increased with increasing LS concentration. The GC-MS data revealed that phenols and ketones were the predominant chemicals present in the LS, and they were also found in the eggs added to the LS even though they were absent in the fresh eggs and control. The flavor of the control group and treated eggs with LS differed significantly, according to the principal component analysis and radar map of the E-nose. The texture study results revealed that the LS significantly impacted the hardness, cohesiveness, and chewiness of eggs.

GC-FID를 이용한 식품 중 유동파라핀 함량 분석 (Determination of Liquid Paraffins in Foods by Using GC-FID)

  • 박세종;최재천;임호수;장수진;김소희;김미혜
    • 한국식품과학회지
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    • 제45권5호
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    • pp.545-549
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    • 2013
  • 본 연구에서는 GC-FID를 이용하여 식품첨가물공전에 사용량이 정해져 있는 빵류, 캡슐류, 건조과실류 채소류 및 과실류 채소류 중 유동파라핀의 함량을 측정하였다. 시료에서 n-hexane으로 유동파라핀을 추출하고 $KMnO_4$ 산화반응을 통해 추출물 중 불포화탄화수소의 극성을 증대시킨 다음 aluminium oxide를 충진한 SPE 카트리지로 정제하여 GC-FID로 측정하였다. 검출한계와 정량한계는 각각 10 mg/kg과 20 mg/kg으로 개별 n-alkane으로 정량하는 방법이 아닌 넓은 봉우리로 나타나는 유동파라핀의 면적의 합으로 정량하는 문헌들(15,17)의 값과 유사하게 나타났다. 유동파라핀은 빵류, 건조과실류 채소류 및 캡슐류에서 이형제 등으로 사용되고 있으나 최종 완제품에서 사용기준 이하로 검출되었고, 과실류 채소류에서 모두 불검출로 나타남에 따라 안전한 수준으로 관리되고 있음을 알 수 있었다.

Rapid Determination of Ginkgolic Acids in Ginkgo biloba Leaf Using Online Column Switching High-Performance Liquid Chromatography-Diode Array Detection and Confirmation by Liquid Chromatography-tandem Mass Spectrometry

  • Lee, Hyounyoung;Lim, Heungyoul;Yang, Juhong;Hong, Jongki
    • Bulletin of the Korean Chemical Society
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    • 제34권12호
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    • pp.3629-3634
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    • 2013
  • In this study, an improved method for the quantitative analysis of ginkgolic acids (GAs) in Ginkgo biloba leaf extract was developed. The samples were extracted with a mixture of chloroform and 50 % ethanol, after which the chloroform extract was dried and reconstituted in methanol. GAs with 13:0, 15:1, and 17:1 in the extract were successfully separated within 40 min and determined with high throughput performance using an online column-switching HPLC method using an SP column C8 SG80 ($4.6{\times}150mm$, $5{\mu}m$) and a Cadenza 5CD C18 column ($4.6{\times}150mm$, $3{\mu}m$). The developed HPLC method was validated for Ginkgo biloba leaf extract. The validation parameters were specificity, linearity, precision, accuracy, and limits of detection and quantitation (LODs and LOQs, respectively). It was found that all of the calibration curves showed good linearity ($r^2$ > 0.9993) within the tested ranges. The LODs and LOQs were all lower than $0.04{\mu}g/mL$. The established method was found to be simple, rapid, and high throughput for the quantitative analysis of GAs in ten commercial Ginkgo biloba leaf extract and dietary supplements. The samples were also analyzed in LC-electrospray ionization (ESI) tandem mass spectrometry (MS/MS) - multiple-ion reaction monitoring (MRM) mode to confirm the identification results that were obtained by the column switching HPLC-DAD method. The developed method is considered to be suitable for the routine quality control and safety assurance of Ginkgo biloba leaf extract.

주곡중의 잔류농약분석에 관한 연구 (Comparative Studies on the Analysis of Pesticide Residues. in Rice, Barley and Wheat)

  • 박승희
    • 한국응용곤충학회지
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    • 제13권4호
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    • pp.235-243
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    • 1974
  • 산지별로 채취된 쌀, 보리, 밀에 함유된 잔류농약(유기수은제 및 유기감소제)을 Dithizone법과 GLC법으로 비교분석한 바 이에서 얻은 결과를 요약하면 다음과 같다. 1. Recovery는 유기수은에 있어서 TLC법$93\%$.에 비하여 GLC법$98\%$이 양호했고, 유기감소제는 GLC법으로 평균 약 $93\%$였다. 2. 시료중 유기수은의 잔류수준은 Dithizone법으로 쌀에 있어서 ND-0.053, .보리는 ND-0.051, 밀은 ND-0.033pm이었고, GLC법으로는 쌀은 trace(less than 0.002ppm)-0.036, 보리는 trace-0.030, 밀은 trace-0.025ppm으로 GLC법이 다소 낮은 수치였다. 3. 유기감소제의 잔류수준은 GLC법으로, 쌀에 있어서 BHC(trace-0.0090ppm), DDT(ND-0.0001ppm), Aldrin(trace-0.0032ppm), Heptachlor(race-0.0031ppm), Dieldrin(ND-0.0092ppm), Endrin(ND-0.0057ppm)이었는데, 수은화합물과 모두 공인최대허용량에 월등히 미달되는 안전수준이었다. 4. Column packing은 유기수은분리에는 $10\%$-DEGS/chromosorb-W,A,W., 유기감소제에는 $3\%$-DC-200/chromosorb-W,A.W.,가 적당하였는데, 유기수은제의 injection sample의 조제에 있어서 ?를 겸한 정제와 reduced glutatione에 의한 유출처리는 ghost peak의 소거와 성분 peak의 완전분리에 효과가 컸으며 검출감도도 높았다.

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한약처방의 표준화를 위한 HPTLC의 활용 (The Application of High Performance Thin Layer Chromatography for Herbal Formula Standardization)

  • 최민경;김형극;왕경화;손창규
    • 대한한의학회지
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    • 제32권4호
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    • pp.68-74
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    • 2011
  • Objective: The purpose of this study is to expatiate on high performance thin layer chromatography (HPTLC) as a simple, easy and scientific method for evaluation and standardization of herbal formulae. Methods: Through retrieving HPTLC application for herbal formulae in the literatures, the current situation of HPTLC application, and potential as well as limitation of HPTLC as a standardization method for multi-herbal drug was studied. Results: HPTLC is a speedy, inexpensive and well-operable tool for possessing multi-capability on component identification, separation, quantification and purification compared to other methods, such as high performance liquid chromatography (HPLC), gas chromatography (GC). Conclusions: HPTLC is considered as an available and convenient method for quality control and standardization of multi-herbal drugs. Thereby, this method could be recommended to widely applicate in the traditional Korean medicine.

한국(韓國) 인삼(人蔘)의 연근별(年根別) 지질(脂質) 및 유리당조성(遊離糖組成) (Lipids and Free Sugar Composition in Ginseng Classified by Years)

  • 손규목;성태수;조영제;이광승;최청
    • Applied Biological Chemistry
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    • 제31권2호
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    • pp.169-176
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    • 1988
  • 인삼의 연근별 지방질 및 지방산 조성과 유리당의 조성을 silicic acid column chromatography, thin layer chromatography, gas liquid chromatography, high performance liquid chromatography로 분리하여 정량하였고 연근별 조 지방질의 함량은 $1.07{\sim}1.67%$로써 3년근이 1.67%로 가장 많았다. 지방질 분별 조성 및 함량은 중성 지질이 $51.35{\sim}72.30%$로 점차 증가한 반면 당 지질은 $15.03{\sim}34.59%$로 거의 2 배 이상 감소하였고 인지질은 $11.83{\sim}2.72%$로 연근별에 따른 큰 변화는 없었다. 중성지질의 성분은 9종류가 확인되었으며 미확인 불질은 2종류였다. 주요 지질성분은 triglyceride가 $14.42{\sim}23.91%$로써 일반적인 동식물의 triglyceride함량 $80{\sim}80%$에 비해 상당히 적다. 지방산 조성은 linoleic acid, palmitic acid, oleic acid 및 linolenic acid가 대부분을 차지하며 linoleic acid의 함량은 총 지질과 중성 지질의 $61{\sim}65%$를 차지하는 반면 당지질과 인 지질에서는 $46{\sim}57%$로 다소 적었다. 중성 지질분획의 지방산조성은 총 지질의 지방산 조성과 거의 비슷하였으며 당 지질의 linolenic acid함량은 오래된 인삼일수록 감소하였다. 유리당을 구성하는 당으로는 rhamnose, fructose, glucose, sucrose, maltose 및 미확인물질 1종이 동정되었다. Sucrose의 함량이 $92{\sim}94%$로 거의 대부분을 차지하였으며 2년근에서 가장 많았으며 그 후에는 점차 감소하였다.

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Gas Liquid Chromatography에 의한 각종(各種) 인삼(人蔘) 제품(製品) 및 오가피(五加皮)의 유리당(遊離糖) 조성(組成)에 관(關)한 연구(硏究) (Studies on Free Sugars in Various Ginseng Products and Acanthopanax by Gas Liquid Chromatography)

  • 이성우;소궤신행;배효원;윤태헌
    • 한국식품과학회지
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    • 제11권4호
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    • pp.273-277
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    • 1979
  • 한국산(韓國産) 홍삼(紅蔘), 한국(韓國), 미국(美國) 및 캐나다산(産)의 피부(皮付) 백삼(白蔘), 홍삼(紅蔘) 및 백삼(白蔘)의 추출액(抽出液), 한국(韓國) 및 쏘련산(産)의 오가피(五加皮)에 대하여 유리당(遊離糖)의 조성(組成)을 가스 크로마토그래피에 의하여, 측정(測定)한 결과(結果)는 다음과 같다. 1. 한국(韓國) 홍삼(紅蔘)과 미국(美國) 및 한국산(韓國産)의 피부(皮付) 백삼(白蔘)에서 ${\beta}-fructose,\;{\alpha}-fructose,\;{\alpha}-glucose$, galactose, ${\beta}-glucose,\;sucrose,\;{\alpha}-maltose,\;{\beta}-maltose$를 동정(同定)할 수있었고, 캐나다산(産) 피부(皮付) 백삼(白蔘)에서 위의 유리당(遊離糖) 가운데서 ${\alpha}-maltose,\;{\beta}-maltose$을 검출(檢出) 할 수 없었다. 그리고 피부(皮付) 백삼(白蔘)에는 홍삼(紅蔘)보다 유리당(遊離糖)의 함량(含量)이 훨씬 많았다. 2. 홍삼(紅蔘) 및 백삼(白蔘) 추출액(抽出液)에서 ${\beta}-fructose,\;{\alpha}-fructose,\;{\alpha}-glucose,\;galactose,\;{\beta}-glucose,\;sucrose,\;{\alpha}-maltose,\;{\beta}-maltose$를 동정(同定)할 수 있었고, 홍삼(紅蔘) 추출물(抽出物)에는 fructose, 백삼(白蔘) 추출액(抽出液)에는 sucrose의 함량(含量)이 가장 많았다. 3. 쏘련산(産) 오가피(五加皮)에서 ${\beta}-fructose,\;{\alpha}-glucose\;galactose,\;{\beta}-glucose,\;sucrose,\;{\alpha}-maltose,\;{\beta}-maltose$를 동정(同定)할 수있어서 인삼(人蔘) 유리당(遊離糖)의 패턴과 오히려 비슷하였다. 그러나 한국산(韓國産) 오가피(五加皮)에서는 ${\beta}-fructose,\;{\alpha}-$${\beta}-glucoses$, sucrose가 동정(同定) 되었을 뿐이고 함량(含量)은 쏘련산(産) 오가피(五加皮)의 1/3에 지나지 않았다.

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A Synthesis of Optically Active cis and trans 2-(5-Hydroxypoperidin-2-yl)acetates

  • P.N. Reddy;한상수;정교현
    • Bulletin of the Korean Chemical Society
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    • 제19권6호
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    • pp.617-618
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    • 1998
  • A simple and reproducible pretreatment method was developed for the determination of dioxins in milk sample. Liquid-liquid extraction (LLE) was used for the initial extraction of the analyte from milk. For the elimination of interferences coextracted from milk, acid treatment followed by multilayer silica gel, and then alumina column clean-up were performed. The clean extract could be obtained without carbon column or high performance liquid chromatographic (HPLC) clean-up procedure. Polychlorinated biphenyles (PCBs) and dioxins were separated on neutral alumina activated at 180 ℃ for 12 hours. The final extract was analyzed by HPLC and high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS). The recovery of dioxins spiked in milk at 75-300 ppt level was 83.3-98.9% and their relative standard deviation was 4.1-14%.