• Title/Summary/Keyword: 고상 추출법

Search Result 40, Processing Time 0.024 seconds

Analysis of alkaloids in Polygala tenuifolia by HPLC (HPLC에 의한 원지 중 알칼로이드 성분의 정량)

  • Park, Man Ki;Park, Jeong Hill;Kim, Bao-Yuan;Kim, Jong Moon;Liem, Kyung-Jin;Han, Byung Hoon
    • Analytical Science and Technology
    • /
    • v.6 no.3
    • /
    • pp.255-259
    • /
    • 1993
  • ${\beta}$-Carboline alkaloids of Polygala tenuifolia (Polygalaceae), an expectorant, tonic and sedative drude drug, were determined by HPLC. The alkaloids were separated by RP-18 column with gradient elution of 0.01M potassium phosphate buffer(pH=3.5) and acetonitrile and detected at UV 254nm. Two methods for the preparation of alkaloid fraction were compared. One was solvent extraction method using acid and base, and the other was solid phase extraction with ion exchange resin (Amberlyst 15). A more refined HPLC chromatogram was obtained using the solid phase extraction method. The alkaloidal contents in P. tenuifolia determined by this method were : harman $2.8{\times}10^{-3}%$, norharman $1.7{\times}10^{-3}%$, 1-carbomethoxy-${\beta}$-carboline $1.3{\times}10^{-3}%$, 1-carboethoxy-${\beta}$-carboline $1.4{\times}10^{-3}%$ and perlolyrine $3.3{\times}10^{-3}%$, respectively.

  • PDF

Constructing Database for Drugs and its Application to Biological Sample by HPTLC and GC/MS (HPTLC와 GC/MS를 이용한 의약품의 데이타베이스화 및 생체시료에의 응용)

  • Yoo, Young-Chan;Park, Sung-Woo;Lim, Mie-Ae;Baeck, Seung-Kyung;Park, Seh-Youn;Lee, Ju-Seon;Lho, Dong-Seok
    • Analytical Science and Technology
    • /
    • v.13 no.2
    • /
    • pp.136-150
    • /
    • 2000
  • For the identification of unknown drugs in biological samples, we attempted rapid high performance thin layer chromatographic method which is sensitive and selective chromatographic analysis of high performance thin layer chromatography (HPTLC) with automated TLC sampler and ultra-violet (UV) scanner. We constructed HPTLC database (DB) on two hundred five drugs by using the data of Rf values and UV spectra (scan 200-360 nm) as well as gas chromatography/mass spectrometry (GC/MS) DB on ninety six drugs by using the data of relative retention time (RRT) on lidocain and mass spectra. After extracting drugs in biological sample by solid phase extraction (Clean Screen ZSDAU020), we applied them to HPTLC and GC/MS DB. Drugs, especially extracted from biological samples, showed good matching ratio to HPTLC DB and these drugs were confirmed by GC/MS. In conclusion, this DB system is thought to be very useful method for the screening of unknown drugs in biological samples.

  • PDF

Analysis of Volatile Compounds in Bamboo and Wood Crude Vinegars by the Solid-Phase Microextracion(SPME) Method (SPME법에 의한 죽초 및 목초액 중의 휘발성 성분 분석)

  • Mun, Sung-Phil;Ku, Chang-Sub
    • Journal of the Korean Wood Science and Technology
    • /
    • v.30 no.4
    • /
    • pp.80-86
    • /
    • 2002
  • Volatile compounds in three different kinds of crude vinegars obtained from oak (Quercus serrata), bamboo (phyllostachys) and pine (Pinus densiflora) species were analyzed by the solid-phase microextraction (SPME) method. A total of 264 peaks were detected on the chromatograms obtained from the polar (CBP 20) and the nonpolar (CBP 1) columns, which were used for analyzing the volatile compounds in these vinegars. The major volatile compounds identified by using the polar column were 2-butanone, acetic acid, guaiacol, phenol, cresols, 4-ethyl guaiacol, 4-ethyl phenol, and syringol. Using the nonpolar column, seven compounds could be identified: 1,2-dimethoxybenzyl alcohol, 1-hydroxy-2-butanone, 1-(2-furanyl)-1-propane, ethisolide, furfuryl acetate, 1,2-dimethoxybenzene, phenyl acetate. The volatile compounds were classified into five groups: phenols, neutral compounds, organic acids, esters and others. The phenols were the main component and comprised 49~65% of the volatile compounds of these vinegars. In the case of bamboo vinegar, the proportion of the phenols in the volatile compounds was lower than that of the two wood vinegars. However, the proportions of the neutral compounds and the organic acids were higher than those of the wood vinegars. Therefore, it seems that these differences of the proportions of the volatile compounds would make a certain difference of a smoke flavor between the bamboo vinegar and the wood vinegars.

Effect of Long-term Organic Matter Application on the Fine Textured Paddy Soils of Double Cropping System in Temperate Area (난지(暖地) 2모작(毛作) 세입질(細粒質) 논에서 유기물(有機物)의 연용(連用) 효과)

  • Yoo, Chul-Hyun;So, Jae-Don;Ida, Akira;Tanaka, Fukuyo;Nishida, Mizuhiko
    • Korean Journal of Soil Science and Fertilizer
    • /
    • v.25 no.4
    • /
    • pp.325-333
    • /
    • 1992
  • An investigation was carried out to find out the effects of long-term application (14 and 28 years) of rice straw, compost and wheat straw on changes in soil chemical and physical properities, aspests of releasing potential nitrogen and nitrogen uptake by rice and maize from fine textured paddy soils with double cropping system in warm temperate area. The result obtained were summarized as follows : 1. The long-term application of organic matters improved plow layer and soil physical properties : bulk density and solid phase were decreased, while porosity and gaseous phase were decreased. 2. Average increment of total carbon per year was 0.0371% and 0.0407% for rice straw and compost, respectively, from 1 through 14 years ; it was 0.0007% and 0.0014% for the rice straw and compost, respectively, from 15 years through 28 years. The average increment of total notrogen per year was 0.0025% and 0.038% for the rice straw and compost, respectively, from 1 through 14 years ; 0.0014% and 0.0024% for the same treatments from 15 through 28 years. 3. $NH_4-N$ and amide-N were high in the soils with wheat straw application for 28 years ; the amino sugar-N in the soils with compost application for 28 years ; amino acid -N in the soils with rice straw application for 14 and 28 years ; and unidentified-N, in the control. 4. The released amount of available nitrogen with the submerged condition was higher at $30^{\circ}C$ than at $25^{\circ}C$ during the incubation. The amount of released available nitrogen at the field was aproximately same as that of $25^{\circ}C$ incubation. However, the released amounts from the incubation and the field were always lower than those extracted with reagents. 5. The amount of nitrogen uptake by rice and maize was highly correlated with available nitrogen extracted with phosphate buffer(pH 7.0). 6. The ratio of yield increase(milled rice) was 17, 12 and 7%, respectively, by application of rice straw, compost and wheat straw for 28 years, and 11% by application of rice straw for 14 years.

  • PDF

A Study on the Synthesis and the Electrochemical Properties of $LiNi_{1-y}$${Co_y}{O_2}$from $Li_2$$CO_3$, ${NiCO_3}$, and $CoCO_3$ ($Li_2$$CO_3$, ${NiCO_3}$, $CoCO_3$로부터 $LiNi_{1-y}$${Co_y}{O_2}$의 합성 및 전극특성 연구)

  • Rim, Ho;Kang, Seong-Gu;Chang, Soon-Ho;Song, Myoung-Youp
    • Journal of the Korean Ceramic Society
    • /
    • v.38 no.6
    • /
    • pp.515-521
    • /
    • 2001
  • 출발 물질로서 L $i_2$C $O_3$, NiC $O_3$, CoC $O_3$를 사용하고 조성과 합성 온도를 변화시켜, 고온 고상법에 의하여 LiN $i_{1-y}$ $Co_{y}$ $O_2$(y=0.1, 0.3, 0.5)를 합성하였다. 합성과 시료들의 결정구조, 미세구조 그리고 전기화학적 특성을 조사하였다. 80$0^{\circ}C$와 8$50^{\circ}C$에서 제조한 L $i_{x}$N $i_{1-y}$ $Co_{y}$ $O_2$는, 삼방정계(space group: R3m)의 $\alpha$-NaFe $O_2$구조로 결정화되어 있는 층상 구조를 형성하였다. LiN $i_{1-y}$ $Co_{y}$ $O_2$(y=0.1, 0.3, 0.5)는 Co의 양이 증가함에 따라 a축과 c축의 크기가 감소하였는데, 이는 코발트 이온의 크기가 니켈 이온의 크기보다 작은데 기인하는 것이다. 그러나 c축과 a축의 크기의 비(c/a)가 증가하였음은 이차원적 구조가 잘 발달됨을 보여준다. 니켈에 대한 코발트의 치환량에 따른 리튬 이온의 삽입/추출 가역성은 코발트의 치환량이 증가하면서 증가하여 y=0.3인 LiN $i_{0.9}$ $Co_{0.1}$ $O_2$에서 대체로 우수하였고 그 이상으로 y값이 증가하면 가역성이 나빠졌다. 80$0^{\circ}C$에서 합성한 LiN $i_{0.9}$ $Co_{0.1}$ $O_2$가 가장 큰 초기 방전 용량 146 mAh/g을 나타내었으며, 싸이클링 성능도 비교적 우수하였다. 8$50^{\circ}C$에서 합성한 LiN $i_{0.9}$ $Co_{0.1}$ $O_2$와 LiN $i_{0.7}$ $Co_{0.3}$ $O_2$가 우수한 싸이클링 성능을 보였다.다. 싸이클링 성능을 보였다.다.보였다.다.

  • PDF

Analysis of anatoxin-a in aqueous and cyanobacterial samples from korean lakes by liquid chromatography with fluorescence detection (액체크로마토그래피-형광검출법에 의한 호소시료의 아나톡신-a 분석)

  • Lee, In-Jung;Lee, Chul-Gu;Heo, Seong-Nam;Lee, Jae-Gwan
    • Analytical Science and Technology
    • /
    • v.24 no.3
    • /
    • pp.225-230
    • /
    • 2011
  • Anatoxin-a is a cyanobacterial neurotoxin with a high toxicity produced by Anabaena, Aphanizomenon and Oscillatoria. Water bloom, formed by Anabaena has been occurring frequently in Lake Yeongchun. It is need to develop a sensitive method for determination of anatoxin-a to control potential hazard in raw water resources. In this study, we developed a highly sensitive analytical method of anatoxin-a using solid phase extraction (SPE) and high performance liquid chromatography (HPLC) with fluorescence detection. Anatoxin-a was converted into a highly fluorescent derivative using 4-fuoro-7-nitro-2,1,3-benzoxadiazole (NBF-F). The method was evaluated in terms of linearity of calibration curve, recovery and repeatability, and the adequate values were obtained. The method detection limit was $0.034\;{\mu}g/g$ and $0.022\;{\mu}g/L$ for algal and water samples, respectively. The concentrations of anatoxin-a were measured in algal and water samples from Lake Andong, Yeongchun and Daechung and ranged from $0.135\;{\mu}g/g$ to $10.979\;{\mu}g/g$ in algal samples and not detected in water samples.

Preparation and Characterization of Tungsten Carbide Using Products of Hard Metal Sludge Recycling Process (초경합금 슬러지 재활용 공정 산물을 활용한 텅스텐 탄화물 제조 및 특성 평가)

  • Kwon, Hanjung;Shin, Jung-Min
    • Resources Recycling
    • /
    • v.31 no.4
    • /
    • pp.19-25
    • /
    • 2022
  • In this study, tungsten carbide (WC) powder was prepared using a novel recycling process for hard metal sludge that does not use ammonium paratungstate. Instead of ammonia, acid was used to remove the sodium and crystallized tungstate, resulting in the formation of tungstic acid (H2WO4). The WC powder was successfully synthesized by the carbothermal reduction of tungstic acid through H2O decomposition, reduction of WO3 to W, and formation of WC. The carbon content and holding time at the carbothermal reduction temperature were optimized to remove free carbon from the WC powder. As a result, most of the free carbon in the WC powder prepared from sludge was removed, and the content of free carbon in the synthesized WC powder was lower than that in commercial WC powder. Moreover, the crystallite size of WC prepared from H2WO4 was much smaller than that of commercial micron-sized WC powder produced from APT. The small crystallite size of WC induces grain growth during the sintering of the WC-Co composite; thus, a WC-Co composite with large WC grains was fabricated using the WC powder prepared from H2WO4. The large WC grains affected the mechanical properties of the WC-Co composite. Further, due to the large grain size, the WC-Co composite fabricated from H2WO4 exhibited a higher toughness than that of the WC-Co composite prepared from commercial WC powder.

The Exposure Status and Biomarkers of Bisphenol A in Shipyard Workers (일부 조선업 근로자들의 bisphenol A 노출실태와 생물학적 지표)

  • Kim, Cheong-Sik;Park, Jun-Ho;Cha, Bong-Suk;Park, Jong-Ku;Kim, Heon;Chang, Soung-Hoon;Koh, Sang-Baek
    • Journal of Preventive Medicine and Public Health
    • /
    • v.36 no.2
    • /
    • pp.93-100
    • /
    • 2003
  • Objectives : Because shipyard workers are involved with various manufacturing process, they are exposed to many kinds of hazardous materials. Welders especially, are exposed to bisphenol-A (BPA) during the welding and flame cutting of coated steel, This study was conducted to assess the exposure status of the endocrine disrupter based on the job-exposure matrix. The effects of the genetic polymorphism of xenobiotic enzyme metabolisms involved in the metabolism of BPA on the levels of urinary metabolite were investigated. Methods : The study population was recruited from a shipyard company in the f province. A total of 84 shipbuilding workers 47 and 37 in the exposed and control groups, respectively, were recruited for this study. The questionnaire variables included, age, sex, use of personal protective equipment, smoking, drinking and work duration. The urinary metabolite was collected in the afternoon and correction made for the urinary creatinine concentration. The of the CYP1A1, CYP2E1 and UGT1A6 genotypes were investigated using polymerase chain reaction-restriction fragment length polymorphism (PCR-RFLP) methods with the DNA extracted from venous blood. Results : The urinary BPA level in the welders group was significantly higher than in the control group (p<0.05). The urinary BPA concentration with the wild type UGT1A6 was higher than the other UGT1A6 genotypes, but with no statistical significant. From themultiple regression analysis of the urinary BPA, the regression coefficient for job grade was statistically significant (p<0.05). Conclusions : The grade of exposure to BPA affected the urinary BPA concentration was statistically significant. However, the genetic polymorphisms of xenobiotics enzyme metabolism were not statistically significant. Further investigation of the genetic polymorphisms with a larger sample size is needed.

Evaluation of Heavy Metal Contamination in Streams within Samsanjeil and Sambong Cu Mining Area (삼산제일.삼봉 동광산 주변 수계의 중금속 오염도 평가)

  • Kim, Soon-Oh;Jung, Young-Il;Cho, Hyen-Goo
    • Journal of the Mineralogical Society of Korea
    • /
    • v.19 no.3 s.49
    • /
    • pp.171-187
    • /
    • 2006
  • The status of heavy metal contamination was investigated using chemical analyses of stream waters and sediments obtained from Samsanjeil and Sambong Cu mining area in Goseong-gun, Gyeongsangnam-do. In addition, the degree and the environmental risk of heavy metal contamination in stream sediments was assessed through pollution index (Pl) and danger index (DI) based on total digestion by aqua regia and fractionation of heavy metal contaminants by sequential extraction, respectively. Not only the degree of heavy metal contamination was significantly higher in Samsanjeil area than in Sambong area, but its environmental risk was also revealed much more serious in Samsanjeil area than in Sambong area. The differences in status and level of contamination and environmental risk between both two mining areas may be attributed to existence of contamination source and geology. Acid mine drainage is continuously discharged and flows into the stream in Samsanjeil mining area, and it makes the heavy metal contamination in the stream more deteriorated than in Sambong mining area in which acid mine drainage is not produced. In addition, the geology of Samsanjeil mining area is mainly comprised of andesitic rocks including a small amount of calcite and having lower pH buffering capacity fer acid mine drainage, and it is likely that the heavy metal contamination cannot be naturally attenuated in streams. On the contrary, the main geology of Sambong mining area consists of pyroclastic sedimentary Goseong formation containing a high content of carbonates, particularly calcite, and it seems that these carbonates of high pH buffering capacity prevent the heavy metal contamination from proceeding downstream in stream within that area.

Simultaneous determinations of anthracycline antibiotics by high performance liquid chromatography coupled with radial-flow electrochemical cell (고성능 액체 크로마토그래피/방사흐름 전기화학전지를 이용한 안트라사이클린계 항생제의 동시 정량)

  • Cho, Yonghee;Hahn, Younghee
    • Analytical Science and Technology
    • /
    • v.20 no.4
    • /
    • pp.308-314
    • /
    • 2007
  • The analytical method of HPLC with the radial-flow electrochemical cell (RFEC) has been developed to determine doxorubicin, epirubicin, nogalamycin, daunorubicin and idarubicin simultaneously by employing a reversed-phase chromatography. Anthracyclines were detected at -0.74 V vs. a Ag/AgCl (0.01 M NaCl) reference electrode, a potential of diffusion current plateau in the mobile phase. At a $V_f$ of 1.0 mL/min doxorubicin, epirubicin, daunorubicin and idarubicin appeared at a retention time ($t_r$) of 6.4 min, 7.4 min, 12.7 min and 18.4 min, respectively, while at a $V_f$ of 0.6 mL/min, doxorubicin, epirubicin, nogalamycin, daunorubicin and idarubicin appeared at a $t_r$ of 9.9 min, 11.5 min, 13.5 min, 19.6 min and 28.7 min, respectively. The linearity between each anthracycline injected ($2.40{\times}10^{-7}M{\sim}1.42{\times}10^{-5}M$) and peak area (charge) was excellent with the square of the correlation coefficient ($R^2$) higher than 0.999. The detection limits were $1.0{\times}10^{-8}M{\sim}1.5{\times}10^{-7}M$ for the five anthracyclines. Within-day precision for the five anthracyclines were in reasonable relative standard deviations less than 3 % ($1.00{\times}10^{-6}M{\sim}1.42{\times}10^{-5}M$) except the lower concentrations less than $0.7{\mu}M$. Solid phase extractions of $1.00{\times}10^{-5}M$ epirubicin, $0.48{\times}10^{-5}M$ nogalamycin and $1.52{\times}10^{-5}M$ daunorubicin from human serum with a $C_{18}$ cartridge resulted in 97 %, 100 % and 90 % of recoveries, respectively.