• Title/Summary/Keyword: chromatogram

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Quantitative Analsysis of Flavanone Glycosides and Peroxynitrite Scavenging Effect of the Five Oriental Medicinal Drugs (Aurantii nobilis Pericarpium, Citrii unshiu Pericarpium, Citrii unshiu Semen, Aurantii Fructus, Poncirii Fructus) (5종 생약(진피, 청피, 귤핵, 지실, 지각)의 Flavanone Glycoside 함량분석과 Peroxynitrite 소거효과)

  • Nugroho, Agung;Park, Myung-Gon;Jin, Seong-Eun;Choi, Jae-Sue;Park, Hee-Juhn
    • Korean Journal of Pharmacognosy
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    • v.40 no.4
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    • pp.370-375
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    • 2009
  • Overproduction of peroxynitrite ($ONOO^-$) causes a variety of disease such as atherosclerosis, hypercholesterolemia, diabetes mellitus or obesity. Peroxynitrite scavenging activities and HPLC analysis on the five Oriental medicinal drugs belonging to the genus Citrus, Aurantium or Poncirus (Rutaceae family) and HPLC analysis were taken to evaluate flavanone glycosides with peroxynitrite scavenging activity. The $IC_{50}s$ of the five crude drugs were shown as follows: Aurantii nobilis Pericarpium (Jinpi, 18.3 ${\mu}g$/ml), Citrii unshiu Pericarpium (Chungpi, 7.50${\mu}g$/ml), Citrii unshiu Semen (Gyulhaek, >50.0${\mu}g$/ml), Aurantii Fructus (Jigak, 18.3${\mu}g$/ml), and Poncirii Fructus (Jisil, >50.0${\mu}g$/ml) where Korean crude drug's names are noted in the parenthesis. Peroxynitrite scavenging effect of flavanones or their glycosides usually contained in Citrus species were observed as follows: hesperetin (1.89 ${\mu}g$/ml), naringenin (7.77 ${\mu}g$/ml), hesperidin (8.44 ${\mu}g$/ml), poncirin (>50.0 ${\mu}g$/ml)and ponciretin(>50.0 ${\mu}g$/ml). The activities of naringin and poncirin with ${\alpha}$-L-rhamnopyranosyl($1{\rightarrow}2$)-${\beta}$-D-glucopyranosyl moiety were weak. HPLC analytical data revealed that Jinpi (the peels of mature fruits of Citrus unshiu) and Chungpi (the peels of immature fruits of C. unshiu) had high quantities of hesperidin as the value of 142.1${\pm}$0.21 and 104.51${\pm}$1.10 mg/g dried weight, respectively. Poncirin was clearly detected in only Jisil and naringenin and naringin were not observed on the HPLC chromatogram of the five crude drugs.

Variation of Glucosinolate Contents among Domestic Broccoli (Brassica oleracea L. var. italica) Accessions (국내 브로콜리(Brassica oleracea L. var. italica) 유전자원 내 Glucosinolate 함량 변이)

  • Lee, Jun Gu;Kwak, Jung-Ho;Um, Yeong Cheol;Lee, Sang Gyu;Jang, Yoon-Ah;Choi, Chang Sun
    • Horticultural Science & Technology
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    • v.30 no.6
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    • pp.743-750
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    • 2012
  • A total of 95 broccoli (Brassica oleracea L. var. italica) accessions were evaluated for the identification of desulfo-glucosinolates and their content variation in the flower head using ultra performance liquid chromatography, to select the potentially functional broccoli breeding lines. The six individual desulfo-glucosinolates, including progoitrin, glucoraphanin, sinigrin, gluconapin, glucobrassicanapin, and glucobrassicin, were commonly identified, based on the chromatogram peak comparison with those of the nine individual glucosinolate standards. The total glucosinolate contents varied from 4.2 to $29.0{\mu}mol{\cdot}g^{-1}$ DW and the glucoraphanin (1.6 to $13.9{\mu}mol{\cdot}g^{-1}$ DW) was confirmed as a major constituent in the total glucosinolate profile among the six identified individual glucosinolate species, whereas the progoitrin, which was only detected in 13 accessions, showed accession-specific variation and negative correlation with glucoraphanin content. It was also revealed that the four major glucosinolates, such as glucobrassicanapin, glucoraphanin, glucobrassicin, and gluconapin, affected major content variation and showed higher positive inter-correlation. These results might be used for the selection of potential breeding materials as functional broccoli germplasm through the further evaluation on the stability and reproducibility of glucosinolate profile depending on environmental factors or cultural managements using the selected accessions.

Chromatographic Determination of Amino Acids in Nonprotein and Protein Fraction Of Undaria Pinnatifida

  • Kwon, Tai-Wan;Lee, Tae-Young
    • Applied Biological Chemistry
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    • v.1
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    • pp.55-61
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    • 1960
  • The amino acid compositions of the protein and the nonprotein fractions obtained from a marine brown alga, 'Undaria pinnatifida' were determined by use of Ion Exchange Column Chromatography. The protein nitrogen in the alga was about ten times of the nonprotein nitrogen. Nonprotein fraction obtained from the extraction with 80 percent ethanol contains considerable amount of tree citrulline. Alanine content in the alga was the highest (about 1 per cent in dry weight) and one third of which was found in free state. The amino acid composition of the alga was well balanced and the content of the essential amino acids were relatively higher, than soybean protein. In addition, several peptide like substances were fractionated from nonprotein fraction, in which one way identified as a naturally occurring new tripeptide composed of alanine, glutamic acid and aspartic acid, and the remaining unknown substances are under investigation for the further information.

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Analysis of Mint Essential Oils from Jeju Island, Korea by Gas Chromatography-mass Spectrometry and Headspace-Gas Chromatography-mass Spectrometry (Gas Chromatography-mass Spectrometry와 Headspace-Gas Chromatography-mass Spectrometry를 이용한 제주산 민트 에센셜오일 성분 분석)

  • Hyun, Ho Bong;Boo, Kyung Hwan;Kang, Hye Rim;Kim Cho, Somi
    • Journal of Applied Biological Chemistry
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    • v.58 no.2
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    • pp.175-181
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    • 2015
  • Compositions of essential oils extracted from mint herb such as Mentha piperita, Mentha spicata, and Mentha ${\times}$ piperita var. citrate produced in Jeju were analyzed using gas chromatography-mass spectrometry (GC-MS) and headspace-GC-MS (HS-GC-MS). By the GC-MS analysis, 13 compounds were tentatively identified in Mentha piperita, Mentha spicata, and Mentha ${\times}$ piperita var. citrate, respectively. Peperitenone oxide, carvone, and linalool were detected as major compounds in Mentha piperita, in Mentha spicata, in Mentha ${\times}$ piperita var. citrate, respectively, based on the ratio of peak intensity in the total ion chromatogram. The greater number of compounds, including volatile alcohols and acetates were identified by HS-GC-MsS than by GC-MS in these all three essential oils. Similar patterns of composition were detected in both Mentha spicata and Mentha ${\times}$ piperita var. citrate by either one of GC-MS methods. However, in case of Mentha piperita, $\small{L}$-(-)-menthol, which was identified as the major compound by HS-GC-MS was detected in dramatically reduced quantity by GC-MS. Interestingly, we found that both linalyl acetate and linalool were identified as the dominant compounds in the essential oil of Mentha ${\times}$ piperita var. citrate.

Separation Characteristics of Alkali and Alkaline Earth Metal Ions Using Novel HDBPDA Ion Exchanger (새로운 HDBPDA 이온교환체를 사용한 알칼리 및 알칼리 토금속 이온들의 분리특성)

  • Kim, Dong Won;Kim, Chang Suk;Choi, Ki Young;Jeon, Young Shin;Hong, Choon Pyo
    • Analytical Science and Technology
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    • v.6 no.5
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    • pp.471-477
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    • 1993
  • The novel macrocylic ligand {(4, 5):(13, 14)-dibenzo-6, 9, 12-trioxa-3, 15, 21, -triazabicyclo [15. 3. 1]heneicosa-(1, 17, 19)(18, 20, 21) triene: HDBPDA} was synthesized, and protonable constants of the ligand and the complex stability constants with alkali metals alkaline earth metals were determined. We evaluated the resolution factor(${\Delta}$) from equation that inducing from stability constants(pK). Also, this ligand was grafted on chloromethylated styrene-divinyl benzene(Merrifield resin) for HDBPDA, ion exchanger. Alkali and alkaline earth metal ions were separated using water by the column chromatography with this ion exchanger. Selectivity(${\alpha}$) and resolution(Rs) of alkali and alkaline earth metal ions were measured from the elution curves chromatogram. The selectivity and resolution values of the various ions calculated from the elution curves were compared with those abtained from pK values. The results were in a good agreement between tow methods. Ion exchange capacity of the resin were determined using the alkali and alkaline earth metal ions and pH dependence of capacity was also discussed.

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Effect of H2O2 Injection and Temperature Changing on the Organic Carbon Fraction in Chromatogram Dissolved Organic Carbon (CDOC) from Thermal Pretreatment (H2O2 주입과 온도변화가 열적 전처리 후 발생 슬러리의 CDOC 유기탄소분율에 미치는 영향평가)

  • Kim, Hee-Joong;Kim, Tae-Kyoung;Kim, Youn-Kwon
    • Journal of Korean Society of Environmental Engineers
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    • v.38 no.3
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    • pp.110-116
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    • 2016
  • Biogas yields point of view, the possibility of reusing excess sludge treated by thermal pretreatment for the purpose of improving the efficiency of the anaerobic digestion process has been investigated in recent year. Thermal pretreatment technology was considered as a pretreatment technique to improve excess sludge properties because of the solubilization of particulate organics. As a view point of sludge reduction and recycle, however, many researchers focused on the ability of particulate hydrolysis and COD solubilization under a high temperature, and few reports have addressed on the physical/chemical characteristics changing. This research was performed to evaluate the effects of a various temperature and chemical additives on carbon formation and fractionation in treated slurry from thermal pretreatment. Based on the results, it was revealed that oxidants injection and temperature changing have significantly caused the change of carbon fractions in slurry from thermal pretreament. Especially, it was considered that the efficiencies of particle hydrolysis increased with the increase of the reaction temperature. Low molecular weight(Mw < 350 g/mol) organic carbon formation increased with the increase of oxidants injection. It was expected that results of this research will provide an overview of the characteristics of thermal pretreatement for excess sludge reduction and recycle.

Development of an Alternative Analytical Method without Related Substance Reference Standards for Fenofibrate in Korean Pharmacopoeia (페노피브레이트 유연물질 표준품 대체시험법 개발)

  • Kim, Jung Hyun;Kim, Min Young;Kwon, Eun Kyung;Lee, Kwang Moon;Choi, Don Woong
    • YAKHAK HOEJI
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    • v.59 no.3
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    • pp.98-106
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    • 2015
  • Analytical method for related substances can be categorized into two methods depending on the necessity of reference standard (RS). The analytical method of related substances with RS is fast and accurate, but it's very expensive and technically difficult to synthesize RS due to their complicated structure. Another method is using relative retention time (RRT) and relative response factor (RRF) which are already validated with RS. Validation of this method is not easy and time consuming, but once it has been developed, it can save cost and time. In this study, we developed the analytical method for related substances of fenofibrate using RRT and RRF. We validated the method by evaluating specificity, linearity, accuracy and precision according to the "Manual for Guideline Application for Validation of Analytical Procedures" of MFDS. Also, we calculated RRT and RRF between fenofibrate and fenofibrate related substances. The results of this study showed high specificity for fenofibrate and fenofibrate related substances. Correlation coefficient(r) of all substances were more than 0.99, and the recovery of fenofibrate, fenofibrate related substance I, II and III were 99.44%, 100.84%, 99.14% and 101.58%, respectively. Precision of fenofibrate and its related substances were ranged between RSD 0.29% and 0.93%. Quantification limits of fenofibrate, fenofibrate related substance I, II and III were determined to be $0.03{\mu}g/ml$, $0.05{\mu}g/ml$, $0.04{\mu}g/ml$ and $0.02{\mu}g/ml$, respectively by confirming signal to noise ratio of each chromatogram. The RRT for fenofibrate related substance I, II and III were determined to be 0.35, 0.41 and 1.34, respectively. Also, the RRF for fenofibrate related substance I, II and III were determined to be 1.28, 0.98 and 0.79, respectively. The developed method was applied to determine contents for fenofibrate related substances in commercial fenofibrate (active pharmaceutical ingredient). As a result, developed analytical methods of related substances will be used for revising the monograph of fenofibrate in Korean Pharmacopoeia revision and contribute quality control of drugs by improving cost and time consuming problem of RS.

Sinigrin content of different parts of Dolsan leaf mustard (돌산갓의 부위별 sinigrin 함량)

  • Oh, SunKyung;Kim, KiWoong;Bae, SangOk;Choi, Myeong Rak
    • Food Science and Preservation
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    • v.22 no.4
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    • pp.553-558
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    • 2015
  • The aims of this study was to optimize the extraction conditions of sinigrin from Dolsan leaf mustard. Dolsan leaf mustard (Dolsan-eup, Yeosu-si) harvested during at May 2014 was used for sinigrin extraction. After the extraction of sinigrin using 50% $CH_3CN$, 10% $NH_4Cl$, 60% $CH_2OH$, and 70% $CH_3OH$, the sinigrin content was measured by HPLC analysis. The results showed that sinigrin content was highest with 50% $CH_3CN$ solvent extraction and UV detector sensitivity was greater at 228 nm rather than at 242 nm. The sinigrin concentrations of leaf, stem and root with 50% $CH_3CN$ extraction were 345 ppm, 728 ppm, and 539 ppm, respectively. After extraction of the different parts of Dolsan leaf mustard, The standard retention time by HPLC analysis of sinigrin content was 2.054, 2.032, 2.059, and 2.035 min from the root, stalk, and leaf, respectively. On the other hand, HPLC analysis showed that the leaf extracts contained glucoraphanin, one of glucosinolates. The optimum time and extraction solvent for the sinigrin extraction from Dolsan leaf mustard was found to be 24 hr with 50% $CH_3CN$ solvent. In addition, opotimum UV detector k at 228 nm. These results showed that the optimum extraction conditions for Dolsan leaf mustard were 24 hr extraction with 50% $CH_3CN$ solvent. In addition, the optimum wavelength of UV detector was determined to be 228 nm for sinigrin analysis. Therefore, this study could provide a useful information for sinigrin extraction and its systematic analysis during the storage.

The collaborative study for verification of analytical results and assurance confidences for pesticide residue (분석결과 검증 및 신뢰성 확보를 위한 실험실간 협력 실험)

  • Park, Hye-Jin;Ko, Kwang-Yong;Han, Kook-Tak;Kim, Il-Jung;Lee, Yong-Jae;Kim, Sung-Hun;Lee, Kyu-Seung
    • Korean Journal of Agricultural Science
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    • v.32 no.2
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    • pp.215-221
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    • 2005
  • The residual study of pesticide has been used in various areas, such as food safety, environmental protection, establishment of tolerance, and explaining the pathway and reaction mode of pesticides, and its importance was expected to increase further more. The aspect of food safety, the pesticide residue survey have been practiced at many organizations, but there were no verification of analytical results at present. In this experiment, we focused on instrumental stability, including response of each instrument and the recovery ratio of each organization's method. As samples for this experiment, we prepared cucumber and sesame, and chose 4 pesticides (bifenthrin, chlorpyrifos, diazinon, and ethoprophos), which were mostly detected from pesticide residue survey and widely used for each crop. The standard deviation of peak areas in the chromatogram of each pesticide were under 1.212 %, so it showed that most instruments were stable. The relationship of recovery ratio of each organization were over 0.996 for every pesticide and each organization. Finally, the analytical results for pesticide residue from each participated organization were not statically significant and we could put confidence in the result from each organization.

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Effect of Betamethasone on Pulmonary Surfactant Activity in Unilateral Pneumonectomized Rabbits (일측폐장절제가토에 있어서 steroid가 제 II 형 폐포세포의 기능에 미치는 영향)

  • Lee, Suck-Kang;Lee, Young-Man
    • Journal of Yeungnam Medical Science
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    • v.1 no.1
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    • pp.59-66
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    • 1984
  • Although it is well established that steroid is effective for treatment of neonatal respiratory distress syndrome (NRDS), the action mechanism of steroid on NRDS is not well known. Several authors have insisted that steroid increases secretion of pulmonary surfactant from type II pneumocyte, but others have insisted that steroid does not affect the secretory function of the type II pneumocyte. And some authors have suggested that steroid may ca use compositional change of pulmonary surfactant phospholipid. From these aspects, it is desirable to confirm the effect of steroid on (he secretory function of the type II pneumocyte. In order to know the effect of steroid on pulmonary surfactant activity, phospholipid phosphorus of lung lavage was measured and composition of pulmonary surfactant phospholipid of lung lavage was analyzed by thin layer chromatography (TLC) in control (C), pneumonectomized (PN), and pneumonectomized with betamethasone treated (PNS) rabbits. And lung weight and lung weight-body weight ratio were measured in each experimental group also. In PN group, right lung pneumonectomy was performed under general anesthesia with pentobarbital sodium (30mg/kg). On the fifth day after the surgery, the left lung was excised and measured above parameters. In PNS group, pneumonectomy was performed as PN group, and one day after the surgery, betamethasone was injected for four days intramusculary (4mg/day) and rabbits were sacrificed. The experiment yielded following results. PNS group's lung weight was significantly (p<0.01) heavier than C group's, but in comparison with PN group's it showed no significant change. PNS group's L/B ratio was significantly (p<0.05) higher than C group's, but compared with PN group's it showed no significant change. The value of phospholipid phosphorus content of PNS group was significantly (p<0.01) higher than that of C group. Even if the value of phospholipid phosphorus content in PNS group was not significantly higher than that of PN group, it showed increasing tendency compared with that of PN group. And in an analysis of the thin layer chromatogram, quantity (${\mu}mol/gm$ of wet weight lung) of phosphatidylcholine in PNS group decreased significantly (p<0.05) compared with C and PN group. From these results, it may be suggested that though steroid inhibits cellular hyperplasia in the compensatory growing lung, it auguments the secretory function of type II pneumocyte and causes compositional change of pulmonary surfactant phospholipid.

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