• Title/Summary/Keyword: 시료 전처리

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홍화유 Tocopherol 분석, Phytosterol 추출 최적화 및 CLA를 함유한 재구성지질 합성

  • 박래균;이기택
    • Proceedings of the Korean Society of Postharvest Science and Technology of Agricultural Products Conference
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    • 2003.04a
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    • pp.104.1-104
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    • 2003
  • 홍화유를 35$^{\circ}C$, 8$0^{\circ}C$ 추출조건 온도에서 각각 1, 3, 6시간 추출하여 HPLC 사용하여 $\alpha$,${\gamma}$,$\delta$-tocopherol 정량하였다. 정량결과 $\alpha$-tocopherol 함량이 ${\gamma}$-tocopherol 함량 보다 높게 나타났으며 $\delta$-tocopherol은 검출되지 않았다 총 tocopherol 함량은 35$^{\circ}C$ 추출조건에서 보다 8$0^{\circ}C$ 추출조건에서 높게 나타났으며 8$0^{\circ}C$ 6시간 추출조건에서 0.23%라는 함량을 나타났다. 또한 반응표면분석에 의하여 홍화유 추출조건에 따른 campesterol, stigmasterol, $\beta$-sitosterol 및 total sterol의 추출 최적화를 모니터링하였으며, 추출온도(35~75$^{\circ}C$, X$_1$), 추출시간(1~11시간, X$_2$), 시료의 전처리 가공 온도(60~10$0^{\circ}C$, X$_3$)를 변수로 한 중심합성계획으로 추출조건을 최적화하였다 추출온도, 추출시간 및 시료의 전처리 가공 온도가 각각 54.69$^{\circ}C$, 4.02시간, 98.37$^{\circ}C$ 이었을 때 campesterol은 0.3852% 추출율을 보였으나 stigmasterol, $\beta$-sitosterol 및 total sterol 반응표면분석 결과 유의차가 없었다. 한편, 추출된 홍화유와 conjugated linoleic acid (CLA)를 1:3 ㏖ 비율로 혼합한 후 고정화효소인 IM60 lipased와 1, 2, 3, 6, 24시간 동안 합성하여 재구성지질을 생성하고 GC에 의해 지방산 조성을 분석한 결과, 총 CLA의 함량은 각각 2.134%, 6.524%, 8.606%, 21.590%, 31.791%로 증가됨을 알 수 있었다.

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Development of Analytical Techniques for Human Serum and Urine by Using Glow Discharge (글로우 방전을 이용한 혈청과 뇨의 분석기술 개발)

  • Lee, Sang Chun;Choi, Kyung-Soo;Son, Eun-Ho;Sim, Young-Jin
    • Analytical Science and Technology
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    • v.11 no.3
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    • pp.167-173
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    • 1998
  • An electrothermal vaporization-hollow cathode glow discharge-atomic emission spectrometer(ETV-HCGD-AES) has been developed for detecting heavy metals in human serum and urine samples. Fisrt of all, we designed a glow discharge cell for atomic emission spectrometry and its analytical performance was studied with the standard reference materials(SRMs) purchased from the NIST. Practically, the ETV-HCGD-AES demonstrated better instrumental sensitivity and selectivity for detecting Hg and Pb in the SRMs, serum and urine, than ICP-OES since the ETV-HCGD-AES was not required the complicate sample digestion procedure, which improved sample transportation efficiency.

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A Rapid Method of Ginsenoside Analysis in HPLC by Pretreatment through the reverse-phase minicolumn (역상소형컬럼 전처리를 이용한 Ginsenoside의 신속정량법)

  • Lee, Mee-Kyoung;Lim, Sun-Uk;Park, Hoon
    • Journal of Ginseng Research
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    • v.12 no.2
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    • pp.164-172
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    • 1988
  • The solvent separation step in the conventional method for quantitative analysis of ginsenosides was substituted by purification through a small reverse-phase $C_18$-column resulting in the decrease of analysis time by one fourth. New method showed high recovery of total ginsenosides but low recovery in protopanaxatriol-ginsenosides. Sugars did not affect the recovery by the amount in usual root sample. Coefficient of variation in recovery of ginsenosides was lower in the rapid minicolumn method. Optimum load of ginsenosides to minicolumn was 10 to 15 mg. The rapid minicolumn method showed highly significant correlation with the solvent separation method for dried root and red ginseng. For the rapid minicolumn method a small acryl device was used for the simultaneous extraction of 8 samples. This method appeared to be beneficial in cost and for the health of analyst.

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Rapid Analysis of Major Putrefactive Metabolites by GC and GC/MSD (GC 및 GC/MSD를 이용한 주요 분변 부패산물 신속분석법)

  • 박규용;김민철;우강융;이나경;백현동
    • KSBB Journal
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    • v.18 no.1
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    • pp.74-77
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    • 2003
  • A simple, reproducible, and rapid gas chromatographic method for putrefactive metabolite determination in feces was developed. The method involves the direct injection of fecal supernatants into the gas chromatograph, without pretreatment. The mass spectra of these metabolites were obtained using an HP 5971 mass selective detector operated in electron impact (EI) ionization mode. This method produced sharp peaks and allowed the simultaneous determination of fecal putrefactive metabolites.

A study on the pretreatment of egg and dried pork for determination of selenium using ICP/MS (ICP/MS를 이용한 계란 및 건조돼지고기 중 셀렌 분석을 위한 전처리 방법 연구)

  • Park, Kyung-Su;Kim, Sun-Tae
    • Analytical Science and Technology
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    • v.14 no.6
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    • pp.465-470
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    • 2001
  • A pretreatment procedure was performed to improve recovery of selenium from enriched egg and dried pork. Samples were digested with only $HNO_3$ in beaker at $150^{\circ}C$ for 3 hrs, and Se was determined by ICP-MS. Recovery of selenium was 94.2%, and its C.V. value was 2.48%. The analytical results of Se by this method were 0.13 - 2.71 mg/kg for egg and 0.36 - 4.19 mg/kg for dried pork.

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Two-stage Biological Hydrogen Production form Organic Wastes and Waste-waters and Its Integrated System (유기성 폐기물 및 폐수로부터 2단계 생물학적 수소생산 및 통합화 시스템)

  • Kim, Mi-Sun;Yoon, Y.S.
    • Transactions of the Korean hydrogen and new energy society
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    • v.13 no.1
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    • pp.52-64
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    • 2002
  • 유기성 폐기물을 이용하여 생물학적 수소생산 통합화 시스템 연구를 수행하였다. 통합화 시스템은 유기성폐기물의 전처리, 2단계 혐기발효 및 광합성 배양으로 구성된 생물학적 수소생산 공정, 초임계수 가스화 공정, 생산된 가스의 저장, 분리 및 연료전지를 이용한 전력 생산으로 구성되었다. 실험에 사용된 유기성 폐자원은 식품공장 폐수, 과일폐기물, 하수슬러지이며, 전처리는 폐기물에 따라 열처리 및 물리적 처리를 하였으며, 전처리된 시료는 생물학적 수소생산 공정에 직접 적용되었다. Clostridium butyricum 및 메탄 생성조에서 발생하는 하수슬러지중의 미생물 복합체는 수소생산 혐기 발효공정에 사용되었으며, 광합성 수소생산 미생물인 홍색 비유황 세균은 광합성 배양에 사용되었다. 생물학적 공정에서 발생하는 미생물 슬러지는 초임계수 가스화 공정으로 수소를 발생하였으며, 슬러지 중의 COD를 저하시켰다. 생물학적 공정 및 초임계수 가스화 공정에서 발생하는 수소는 가스탱크에 가입상태로 저장한 후, 95%순도로 분리하였으며, 정제된 수소는 연료전지에 연결하여 전력 생산을 하였다.

Sample Pretreatment and HRGC/HRMS Analysis for Determination of Dioxins in Environmental Samples (환경시료 중 다이옥신류의 정량을 위한 시료전처리방법의 개선 및 고분해능 GC/MS 분석에 관한 연구 Ⅰ)

  • Kim, Jin Yeong;Jang, Yun Seok;Lee, Dae Un
    • Journal of the Korean Chemical Society
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    • v.38 no.11
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    • pp.819-826
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    • 1994
  • This study described a simple, rapid and cost effective analytical technique for the ultra-trace analysis of dioxins in environmental samples. Liquid-Liquid extraction methods were used for the initial extraction and enrichment of the analyte. Subsequent clean-up procedures were achieved by using strong cation exchanger, silica and Florisil cartridges. Extracts were analysed by HRGC/HRMS-SIM. The efficiency of these analytical methods was tested by recovery and selectivity for elimination of interferences such as phenols, pesticides and PCBs in each step. The mean recovery of 1,2,3,4-TCDD spiked at 10 ppt in sea water was about 92(${\pm}$1.6)%. This analytical method was applied to Kwangyang sea water and 4.5pg/L of 2,3,7,8-TCDD was determined.

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Revision of the Analysis of Makgeolli for Ochratoxin A (막걸리 중 ochratoxin A 분석의 개선)

  • Park, Je-Won
    • Korean Journal of Food Science and Technology
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    • v.38 no.1
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    • pp.140-142
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    • 2006
  • Because ochratoxin A recovery level of Makgeolli is lower (<50%) than those of other commodities such as rice, barley, and beer, Makgeolli was evaluated to improve the recovery and enable routine analysis. Use of 3% sodium bicarbonate instead of phosphate-buffered saline as homogenizing solution provided good recovery of ochratoxin A (>80%) spiked in Makgeolli at level of 1 ppb. To determine if this analytical method is reliable for ochratoxin A detection in Makgeolli, survey was conducted for ochratoxin A in 30 sterile Makgeolli samples retailed in Korea. Only two wheat-based Makgeolli samples contained detectable level of ochratoxin A (0.8 and 2.1 ppb) as confirmed by HPLC- electrospray ionization- mass spectrometry. Extraction of sample with 3% sodium bicarbonate for 3 min, followed by cleanup of extracts with immunoaffinity columns, and HPLC with fluorescence detection provided dependable detection of ochratoxin A in Makgeolli samples.

Pretreatment of Rice Straw by Using Ammonia Recycled Percolation Process (암모니아 재순환 침출공정을 이용한 볏짚의 전처리)

  • Kang, Choon-Hyoung
    • Korean Chemical Engineering Research
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    • v.47 no.1
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    • pp.89-95
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    • 2009
  • Because of high contents of cellulose (~37 wt%) and hemicellulose (~17%), rice straw seems to be a potential lignocellulosic biomass for production of bioethanol. In this study, Ammonia Recycled Percolation (ARP) pretreatment of rice straw was extensively investigated. In particular, the experimental study included the effects of temperature, reaction time and concentration of ammonia on compositions and enzymatic digestibility of the resulting solid residues; the ranges of pretreatment conditions were, in turn, $150{\sim}190^{\circ}C$, 10~90 min and 0~20 wt%. Through ARP pretreatment, the lignin content was reduced by as high as ~84% while 20~80% of the hemicellulose was also solubilized. The solid residue resulted from the pretreatment with 15 wt% aqueous ammonia solution at $170^{\circ}C$ for 90 mim showed as high as ~90% of digestibility with 15FPU/g of glucan enzyme loading. Supplement of xylanese to cellulase led to a notable enhancement of digestibility, indicating a discernable inhibitory role of hemicellulose. Simultaneous Saccharification and Fermentation (SSF) and Simultaneous Saccharification and Co-Fermentation (SSCF) were performed to obtain ethanol productions of 13.8 g/L (corresponding to 81% yield) and 15 g/L (corresponding to 89% yield), respectively.

Studies on the Analytical Methods of Coal Ash (석탄회 분석 방법에 관한 연구)

  • Park, Hyun Joo;Kim, Kyeong Sook;Yang, Seug Ran;Lee, Gae Ho
    • Journal of the Korean Chemical Society
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    • v.44 no.6
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    • pp.563-572
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    • 2000
  • The analysis of coal ash is very important to predict some factors, such as slagging and fouling in the boiler, and to determine optimum mixing ratios of the each coals used. In ASTM, the analysis of coal ash is clarified to use lithium metaborate (LiBO$_2$) as a fluxing agent and then to analyze the pre-treated samples using AAS. However, it takes too much time and efforts to analyze many samples by ASTM method, as a result, this method is not proper in our laboratory in charge of analyses of all power plants. So we tried to establish more convenient and accurate analytical method of coal ash by 3 different methods which are 2 different pre-treatment methods (fusion dissolution and microwave digestion) and XRF analysis method using a clear pellet. Although all 3 methods can be utilized to analyze the major elements of coal ash, each method has its own characteristics, therefore, each method should be chosen according to its own purpose.

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