• Title/Summary/Keyword: high performance liquid chromatography

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Chiral Separation of the Enantiomers of Metoprolol and Its Metabolites by High Performance Liquid Chromatography

  • Kim, Kyeong-Ho;Shin, Sang-Duk;Lee, Joo-Hyun;Lee, Sang-Cheal;Kang, Jong-Seong;Mar, Woong-chon;Hong, Seon-Pyo;Kim, Hyun-Ju
    • Archives of Pharmacal Research
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    • v.23 no.3
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    • pp.230-236
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    • 2000
  • (1'R, 2R)-, (1'R, 2S)-, (1'S, 2R)- and (1'S, 2S)-$\alpha$-hydroxymetoprolol; (2R)- and (2S)-O-des-methylmetoprolol; and (2R)- and (2S)-metoprolol acid are major metabolites of (2R)-and (2S)-metoprolol, $\beta$-adrenergic antagonist. The focus of most chiral separation methods until now has been on determination of the enantiomeric parent drug. However, it is just as important to be able to follow the metabolism of the enantiomers and their possible chiral metabolites. Therefore, for the study of stereoselective metabolism and pharmacokinetics of metoprolol, the chiral separation of the enantiomers of metoprolol and its metabolites has been investigated using four chiral stationary phases, i.e., Chiralcel OD, Chiral-AGP, Cyclobond I and Sumichiral OA-4900 columns. Metoprolol acid was resolved only by Sumichiral OA-4900. Chiralcel OD provided the highest separation factor and resolution value for metoprolol and O-desmethylmetoprolol and partially resolved the four stereoisomers of $\alpha$-hydroxymetoprolol. Diastereomeric $\alpha$-hydroxymetoprolols were resolved using the coupled column chromatographic system of two chiral stationary phases, Sumichiral OA-4900 column and Chiralcel OD column.

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Manufacture and Physicochemical Properties of Chitosan Oligosaccharide/A2 β-Casein Nano-Delivery System Entrapped with Resveratrol

  • Kim, Mi Young;Ha, Ho-Kyung;Ayu, Istifiani Lola;Han, Kyoung-Sik;Lee, Won-Jae;Lee, Mee-Ryung
    • Food Science of Animal Resources
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    • v.39 no.5
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    • pp.831-843
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    • 2019
  • The purposes of this research were to form chitosan oligosaccharide (CSO)/A2 ${\beta}$-casein nano-delivery systems (NDSs) and to investigate the effects of production variables, such as CSO concentration levels (0.1%, 0.2%, and 0.3%, w/v) and manufacturing temperature ($5^{\circ}C$, $20^{\circ}C$, and $35^{\circ}C$), on the production and physicochemical characteristics of CSO/A2 ${\beta}$-casein NDSs to carry resveratrol. The morphological characteristics of CSO/A2 ${\beta}$-casein NDSs were assessed by the use of transmission electron microscopy (TEM) and particle size analyzer. High-performance liquid chromatography (HPLC) was applied to determine the entrapment efficiency (EE) of resveratrol. In the TEM images, globular-shaped particles with a diameter from 126 to 266 nm were examined implying that NDSs was successfully formed. As CSO concentration level was increased, the size and zeta-potential values of NDSs were significantly (p<0.05) increased. An increase in manufacturing temperature from $5^{\circ}C$ to $35^{\circ}C$ resulted in a significant (p<0.05) increase in the size and polydispersity index of NDSs. Over 85% of resveratrol was favorably entrapped in CSO/A2 ${\beta}$-casein NDSs. The entrapment efficiency (EE) of resveratrol was significantly (p<0.05) enhanced with an increase in manufacturing temperature while CSO concentration level did not significantly affect EE of resveratrol. There were no significant (p<0.05) changes observed in the size and polydispersity index of NDSs during heat treatments and storage in model milk and yogurt indicating that CSO/A2 ${\beta}$-casein NDSs exhibited excellent physical stability. In conclusion, the CSO concentration level and manufacturing temperature were the crucial determinants affecting the physicochemical characteristics of CSO/A2 ${\beta}$-casein NDSs containing resveratrol.

Amino acids profiles of six dinoflagellate species belonging to diverse families: possible use as animal feeds in aquaculture

  • Lim, An Suk;Jeong, Hae Jin;Kim, So Jin;Ok, Jin Hee
    • ALGAE
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    • v.33 no.3
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    • pp.279-290
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    • 2018
  • Microalgae have been utilized in diverse industries including aquaculture. Among the microalgae, dinoflagellates are known to have various bioactive compounds, and thus the interest in their application to industry has increased. In order to test their potential as food materials for aquaculture animals, the crude protein contents and compositions of amino acids of six dinoflagellates Heterocapsa rotundata (family Heterocapsaceae), Ansanella granifera (Suessiaceae), Alexandrium andersonii (Ostreopsidaceae), Takayama tasmanica (Brachidiniaceae), Takayama helix, and Gymnodinium smaydae (Gymnodiniaceae) belonging to diverse families were analyzed. The percentage of the amount of the crude protein relative to dry weight of T. tasmanica was the highest (65%) and that of A. andersonii was the lowest (26%). However, the highest percentage of total detected amino acids in crude protein was found in A. andersonii (98.2%). In all six dinoflagellates, glutamic acid was the most dominant amino acid in crude protein. However, the second main amino acid was aspartic acid for H. rotundata, A. granifera, T. helix, and G. smaydae, but were arginine and leucine for A. andersonii and T. tasmanica, respectively. Furthermore, T. tasmanica and T. helix did not have taurine and gamma-aminobutyric acid, whereas the other dinoflagellates possessed them. The percentages of essential amino acid contents of the dinoflagellates met the requirement levels for juvenile shrimps. In addition, the dinoflagellates were not toxic to the brine shrimp Artemia salina. Compared with the other microalgae reported so far, H. rotundata and A. andersonii can be used for arginine-rich diets, T. tasmanica for valine and leucine-rich diets, A. granifera for histidine-rich diets, T. helix for threonine-rich diets, and G. smaydae for lysine-rich diets. Therefore, based on their biochemical composition and toxicity to Artemia, the dinoflagellates could be used as essential amino acid sources for cultivating animals in the aquaculture industry.

A comparative study of Sargassum horneri Korea and China strains collected along the coast of Jeju Island South Korea: its components and bioactive properties

  • Kim, Hyun-Soo;Sanjeewa, K.K. Asanka;Fernando, I.P. Shanura;Ryu, BoMi;Yang, Hey-Won;Ahn, Ginnae;Kang, Min Cheol;Heo, Soo-Jin;Je, Jun-Geon;Jeon, You-Jin
    • ALGAE
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    • v.33 no.4
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    • pp.341-349
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    • 2018
  • Sargassum horneri is edible brown seaweed abundant along the coasts of Jeju Island, South Korea. In addition to the native S. horneri population, a large amount of S. horneri has been found to invade Jeju Island from the east coast of China. Thus, S. horneri of both Korea (SK) and China (SC) strains now inhabits along with the shore of Jeju Island and have become a threat to the coastal biodiversity. However, they could be used in obtaining functional ingredients for industrial level applications provided an optimized cost effective strategy. In the present study, we compared SK and SC strains for the extraction efficiency, components, antioxidant, and anti-inflammatory properties of 80% methanolic extracts and their partially purified fractions. According to the results, two strains indicated similar bioactive properties such as DPPH and alkyl radical scavenging activity as well as anti-inflammatory activities on lipopolysaccharide-stimulated RAW 264.7 cells. The yield of 80% methanol extract from SC was higher than SK. However, the yields of the ethyl acetate and chloroform fractions from SK were higher than those of SC strain. The major peaks in the high-performance liquid chromatography chromatograms, which was identified as Apo-9 fucoxanthinone, indicated that both methanolic extracts of SK and SC contains major target peaks but with different amounts. This study might be useful for developing functional materials from SC and SK in future.

Discrimination of Ginseng Habitat by Using Instrumental Analysis Techniques

  • Sohn H. J.;Lee S. K.;Cho B. G.;Kim S. J.;Lee N. Y.;Choi D. S.;Jeong M. S.;Bae H. R.;Yang J. W.
    • Proceedings of the Ginseng society Conference
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    • 2002.10a
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    • pp.238-252
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    • 2002
  • In order to screen out indicators for the discrimination of ginseng habitat, some physical and chemical characteristics of Korean red ginsengs (94 kinds) and Chinese red ginsengs (50 kinds) were analyzed by using a rheometer, an electronic nose system, a combined technique of solid phase micro-extraction (SPME) and gas chromatograph equipped with an electron capture detector (GC/ECD), an X-ray fluorescence spectrometer (XRF), an inductively coupled plasma mass spectrometer (ICP/MS), a near infrared spectrometer (NIRs) and high performance liquid chromatography equipped with evaporative light scattering detector (HPLC/ELSD). The results are summarized as follows: (i) The rhizome strengths of Korean red ginsengs were significantly higher than those of Chinese red ginsengs. (ii) The electronic nose patterns of Korean red ginsengs were significantly different from those of Chinese red ginsengs. (iii) Some unidentified peaks were detected not in the headspace of Korean red ginsengs but in the headspace of Chinese red ginsengs when the headspace volatiles prepared by the SPME technique were analyzed by GC/ECD. (iv) Either the content ratios of K to Ca or Mn to Fe were significantly different between Korean red ginsengs and Chinese red ginsengs. (v) The reflectance ratios of NIRs wavenumbers such as $904\;cm^{-1}\;to\;1088\;cm^{-1}$ for Korean red ginsengs were significantly different from those for Chinese red ginsengs. (vi) The content ratios of ginsenoside-Rg to ginsenoside-Re of Korean red ginsengs were significantly higher than those of Chinese red ginsengs. These results indicate that the rhizome strength, the electronic nose pattern, the occurrence of ECD-sensitive headspace volatile components, the content ratios of K to Ca and Mn to Fe, the NIRs pattern and the content ratio of ginsenoside-Rg to -Re may be indicators for the discrimination of ginseng habitat.

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Neuroprotective Effects of Hyangsayangwi-tang in MPTP-induced Mouse Model of Parkinson's Disease (MPTP(1-methyl-4-phenyl-1,2,3,6-tetrahydropyridine)로 유도된 Parkinson's Disease 동물 모델을 이용한 향사양위탕의 신경 세포 보호 효과)

  • Go, Ga-Yeon;Kim, Yun-Hee;Ahn, Taek-Won
    • Journal of Sasang Constitutional Medicine
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    • v.26 no.2
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    • pp.165-179
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    • 2014
  • Objectives To evaluate the neuroprotective effects of Hyangsayangwi-tang (HY), a Korean traditional medicinal prescription in a Parkinson's disease mouse model. Methods Four groups(each of 10 mouse per group) were used in this study. The neuroprotective effect of HY was examined in a Parkinson's disease mouse model. C57BL/6 mouse treated with 1-methyl-4-phenyl-1,2,3,6-tetrahydropyridine (MPTP, 30mg/kg/day), intraperitoneal (i.p.) for 5 days. Slow behavioral responses and memory disorder is the major clinical symptoms of PD. In order to investigate the effect of HY on recovery of behavioral deficits and memory, we examined the motor function and memory by using Morris water maze and Forced swimming test. Ischemic mouse brain stained with TTC(2,3,5 triphenyl tetrazolium chloride) in the MPTP-induced Parkinson's disease to find out ischemia and tissue damage in mouse. The convenient, simple, and accurate high-performance liquid chromatography (HPLC) method was established for simultaneous determination of neurotransmitters in MPTP-HY group. To measure the amount of dopamine in mice brain, striatum-substantia nigra, was examined by Bradford assay. Immunohistochemistry was examined in the MPTP-induced Parkinson's disease (PD) mouse to evaluate the neuroprotective effects of Hyangsayangwi-tang on hippocampal lesion, ST and SNpc. Results and Conclusions Hyangsayangwi-tang (HY) prevents MPTP-induced loss of serotonin, hippocampus and TH-ir cell.

Enzymatic Degradation of Leucine Enkephalin and $[D-Ala^2]$-Leucine Enkephalinamide in Various Rabbit Mucosa Extracts (토끼의 수종 점막 추출액중 로이신엔케팔린 및 [D-알라$^2]$-로이신엔케팔린아미드의 효소적 분해 특성)

  • Chun, In-Koo;Park, In-Sook
    • YAKHAK HOEJI
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    • v.38 no.5
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    • pp.530-543
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    • 1994
  • To study the feasibility of transmucosal delivery of leucine enkephalin (Leu-Enk) and $[D-ala^2]$-leucine enkephalinamide (YAGFL), their degradation extents and pathways in various rabbit mucosa extracts were investigated by high performance liquid chromatography. The degradation of Leu-Enk and YAGFL was observed to follow the first-order kinetics. The degradation half-lives of Leu-Enk in the nasal, rectal and vaginal mucosal extracts were 1.62, 0.37 and 1.12 hrs and those of YAGFL were 30.55, 9.70 and 6.82 hrs, respectively, indicating Leu-Enk was degraded in a more extensive and rapid manner than YAGFL. But the mucosal and serosal extracts of the same mucosa showed the similar degradation rates for both pentapeptides. The degradation was most rapid in the neutral pH and increasing concentrations of substrates retarded the degradation rates. The maior hydrolytic fragments of Leu-Enk were Des-Tyr-Leu-Enk and tyrosine, indicating the enzymatic hydrolysis by aminopeptidases. However, the data also suggested endopeptidases such as dipeptidyl carboxypeptidase and dipeptidyl aminopeptidase could play some role in the degradation of Leu-Enk. On the other hand, the hydrolytic fragments of YAGFL in all the mucosa extracts were mainly Tyr-D-Ala-Gly and Phe-Leu-Amide, demonstrating the hydrolytic breakdown by endopeptidases. The degradation pathways were further explored by concomitantly determining the formation of smaller metabolites of primary hydrolytic fragments of Leu-Enk and YAGFL in the mucosa extracts.

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Quantification of Arsenic Species in Some Seafood by HPLC-AFS (HPLC-AFS를 이용한 해산물 중 비소 화학종 분리정량)

  • Jeong, Seung-Woo;Lee, Chae-Hyeok;Lee, Jong-Wha;Jang, Bong-Ki
    • Journal of Environmental Health Sciences
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    • v.47 no.5
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    • pp.496-503
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    • 2021
  • Background: Considering the expenses of and difficulties in arsenic speciation by high performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS), alternative measurement methods should be useful, especially for large-scale research and projects. Objectives: A measurement method was developed for arsenic speciation using HPLC-atomic fluorescence spectrometry (HPLC-AFS) as an alternative to HPLC-ICP-MS. Methods: Total arsenic and toxic arsenic species in some seafoods were determined by atomic absorption spectrometry coupled with hydride vapor generation (AAS-HVG) and HPLC-AFS, respectively. Recovery rate of arsenic species in seafood was evaluated by ultra sonication, microwave and enzyme (pepsin) for the optimal extraction method. Results: Limits of detection of HPLC-AFS for As3+, dimethylarsinate (DMA), monomethylarsonate (MMA) and As5+ were 0.39, 0.53, 0.60 and 0.64 ㎍/L, respectively. The average accuracy ranged from 97.5 to 108.7%, and the coefficient of variation was in the range of 1.2~16.7%. As3+, DMA, MMA and As5+ were detected in kelp, the sum of toxic arsenic in kelp was 40.4 mg/kg. As3+, DMA, MMA and As5+ were not detected in shrimp and squid, but total arsenic (iAS and oAS) content in shrimp and squid analyzed by AAS-HVG were 18.1 and 24.7 mg/kg, respectively. Conclusions: HPLC-AFS was recommendable for the quantitative analysis method of arsenic species. As toxic arsenic species are detected in seaweeds, further researches are needed for the contribution degree of seafood in arsenic exposure.

Variation of Caffeic acid, Rosmarinic acid, Luteolin and Apigenin Contents in Perilla Germplasm

  • Lee, Myoung-Hee;Jung, Chan-Sik;Pae, Suk-Bok;Hwang, Chung-Dong;Park, Chang-Hwan;Shim, Kang-Bo;Park, Keum-Yong;Kim, Hyun-Kyung;Park, Soon-Ki;Ha, Tae-Joung
    • Korean Journal of Breeding Science
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    • v.41 no.4
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    • pp.391-396
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    • 2009
  • Perilla frutescens, which belonging to the Labiatae family, is widely cultivated oil crop and have been used traditional herbal medicine in East Asia such as Korea, China, and Japan. Especially, the leaves and the seeds of this species are important in Korean traditional cooking, as one of the popular garnish and food colorants. Numerous studies have revealed that the beneficial health effects of perilla are due to its several phytochemicals contents, such as rosmarinic acid, caffeic acid, luteolin, and apigenin. For this reason, increasing the content of phytochemicals in perilla hasbecome a major breeding objective. The genetic diversity of the rosmarinic acid, caffeic acid, luteolin, and apigenin content in perilla seed is poorly documented. We analyzed the rosmarinic acid, caffeic acid, luteolin, and apigenin content of 203 accessions of perilla germplasm by high performance liquid chromatography (HPLC). The rosmarinic acid and luteolin contents ofgermplasms were ranged from $15.7{\mu}g/g$ to $2717.1{\mu}g/g$ and from $1.6{\mu}g/g$ to $582.4{\mu}g/g$ respectively.

Multicomponent assessment and ginsenoside conversions of Panax quinquefolium L. roots before and after steaming by HPLC-MSn

  • Huang, Xin;Liu, Yan;Zhang, Yong;Li, Shuai-Ping;Yue, Hao;Chen, Chang-Bao;Liu, Shu-Ying
    • Journal of Ginseng Research
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    • v.43 no.1
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    • pp.27-37
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    • 2019
  • Background: The structural conversions in ginsenosides induced by steaming or heating or acidic condition could improve red ginseng bioactivities significantly. In this paper, the chemical transformations of red American ginseng from fresh Panax quinquefolium L. under steaming were investigated, and the possible mechanisms were discussed. Methods: A method with reversed-phase high-performance liquid chromatography coupled with linear ion trap mass spectrometry ($HPLC-MS^n$)-equipped electrospray ionization ion source was developed for structural analysis and quantitation of ginsenosides in dried and red American ginseng. Results: In total, 59 ginsenosides of protopanaxadiol, protopanaxatriol, oleanane, and ocotillol types were identified in American ginseng before and after steaming process by matching the molecular weight and/or comparing $MS^n$ fragmentation with that of standards and/or known published compounds, and some of them were determined to be disappeared or newly generated under different steaming time and temperature. The specific fragments of each aglycone-type ginsenosides were determined as well as aglycone hydrated and dehydrated ones. The mechanisms were deduced as hydrolysis, hydration, dehydration, and isomerization of neutral and acidic ginsenosides. Furthermore, the relative peak areas of detected compounds were calculated based on peak areas ratio. Conclusion: The multicomponent assessment of American ginseng was conducted by $HPLC-MS^n$. The result is expected to provide possibility for holistic evaluation of the processing procedures of red American ginseng and a scientific basis for the usage of American ginseng in prescription.