• 제목/요약/키워드: HPLC-ESI/MS

검색결과 149건 처리시간 0.02초

New dammarane-type triterpenoid saponins from Panax notoginseng saponins

  • Li, Qian;Yuan, Mingrui;Li, Xiaohui;Li, Jinyu;Xu, Ming;Wei, Di;Wu, Desong;Wan, Jinfu;Mei, Shuangxi;Cui, Tao;Wang, Jingkun;Zhu, Zhaoyun
    • Journal of Ginseng Research
    • /
    • 제44권5호
    • /
    • pp.673-679
    • /
    • 2020
  • Background: Panax notoginseng saponin (PNS) is the extraction from the roots and rhizomes of Panax notoginseng (Burk.) F. H. Chen. PNS is the main bioactive component of Xuesaitong, Xueshuantong, and other Chinese patent medicines, which are all bestselling prescriptions in China to treat cardiocerebrovascular diseases. Notoginsenoside R1 and ginsenoside Rg1, Rd, Re, and Rb1 are the principal effective constituents of PNS, but a systematic research on the rare saponin compositions has not been conducted. Objective: The objective of this study was to conduct a systematic chemical study on PNS and establish the HPLC fingerprint of PNS to provide scientific evidence in quality control. In addition, the cytotoxicity of the new compounds was tested. Methods: Pure saponins from PNS were isolated by means of many chromatographic methods, and their structures were determined by extensive analyses of NMR and HR-ESI-MS studies. The fingerprint was established by HPLC-UV method. The cytotoxicity of the compounds was tested by 3-(4,5-dimethylthiazol-2-yl)-2,5 -diphenyltetrazolium bromide assay. Results and Conclusion: Three new triterpenoid saponins (1-3) together with 25 known rare saponins (4-28) were isolated from PNS, except for the five main compounds (notoginsenoside R1 and ginsenoside Rg1, Rd, Re, and Rb1). In addition, the HPLC fingerprint of PNS was established, and the peaks of the isolated compounds were marked. The study of chemical constituents and fingerprint was useful for the quality control of PNS. The study on antitumor activities showed that new Compound 2 exhibited significant inhibitory activity against the tested cell lines.

연꽃 자방으로부터 이차대사물질 분리 및 구조동정 (Isolation and Identification of Secondary Metabolites from the Ovary of Nelumbo nucifera)

  • 지승헌;이재원;이승은;이영섭;김금숙;안영섭;백남인;이이;임흥빈;이대영
    • 생명과학회지
    • /
    • 제26권10호
    • /
    • pp.1196-1201
    • /
    • 2016
  • 연꽃의 자방으로부터 80% MeOH로 추출하고, 얻어진 추출물을 n-hexane, ethyl acetate, n-butanol 및 H2O으로 용매 분획하였다. 이 중 n-hexane 분획물에 대해 silica gel과 octadecyl silica gel column chromatography 및 Prep-HPLC system을 반복 수행하여 5 종의 물질을 분리 하였다. 각 화합물의 화학구조는 NMR, GC/MS및 ESI/MS 등의 분광학적 스펙트럼을 측정하고, 해석하여 1-eicosanol (1), cycloartenol (2), trans-squalene (3), pentadecanoic acid (4) 및 β-sitosterol (5)으로 동정하였다. 이 화합물들은 연꽃 자방추출물에서 처음으로 분리하고 동정하였으며 앞으로 이 화합물들에 대한 다양한 생리적 및 약리적 활성을 검토함으로써 건강기능성 식품 또는 의약품의 소재로서의 충분한 가치가 있다고 여겨진다.

상황버섯 추출물의 항산화 및 성분분석 (Antioxidative Activity and Component Analysis of Phellinus linteus Extracts)

  • 김아름;김정은;박수남
    • 대한화장품학회지
    • /
    • 제37권4호
    • /
    • pp.309-318
    • /
    • 2011
  • 본 연구에서는 상황버섯 추출물의 항산화 및 항노화 활성 및 항균 효과, 그리고 성분분석에 관한 연구를 수행하였다. 상황버섯 추출물의 자유 라디칼(1,1-diphenyl-2- picrylhydrazyl, DPPH) 소거활성($FSC_{50}$)은 에틸아세테이트(ethylacetate) 분획($2.94\;{\mu}g/mL$)에서 가장 큰 활성을 나타내었고, 루미놀-의존성 화학발광법을 이용한 $Fe^{3+}$-EDTA/$H_2O_2$계에서 생성된 활성산소종(reactive oxygen species, ROS)에 대한 상황버섯 추출물의 총항산화능은 추출물의 에틸아세테이트 분획($0.0072\;{\mu}g/mL$)에서 가장 큰 활성을 나타내었다. 광증감제인 rose-bengal로 증감된 사람 적혈구의 광용혈에 대한 억제 효과를 측정하였을 때 농도범위($5{\sim}50\;{\mu}g/mL$)에서 50 % 에탄올 추출물과 에틸아세테이트 분획 모두 농도 의존적으로 세포 보호 효과를 나타내었다. 타이로시네이즈의 활성 저해 효과($IC_{50}$)를 측정한 결과 50 % 에탄올 추출물($IC_{50}=6.34\;{\mu}g/mL$)에서 우수한 효과를 나타내었으며, 엘라스테이즈의 활성 저해 효과($IC_{50}$)는 에틸아세테이트분획($IC_{50}=14.08\;{\mu}g/mL$)에서 큰 효과가 나타났다. TLC, HPLC 및 LC/ESI-MS를 이용하여 상황버섯 추출물 ethylacetate 분획의 주성분을 분석하였고 hispidin 유도체인 interfungin A를 확인하였다. 이상의 결과들은 상황버섯 추출물이 ROS에 대항하여 세포막을 보호함으로써 생체계, 특히 태양 자외선에 노출된 피부에서 항산화제로써 작용할 수 있으며, 특히 상황버섯 추출물의 에틸아세테이트 분획을 항산화, 항노화 및 미백 기능성 화장품 소재로써의 응용 가능성을확인하였다.

식품 포장재 중의 퍼플루오르옥탄설포네이트 분석 (The Determination of Perfluorooctane sulfonate in Food Packing Materials by HPLC-MS/MS)

  • 김일영;김애경;정보경;신영;김지영;김정헌;채영주
    • 한국식품위생안전성학회지
    • /
    • 제28권4호
    • /
    • pp.376-380
    • /
    • 2013
  • 퍼플루오르옥탄설포네이트를 LC/MS/MS를 이용하여 분석한 결과 분석 대상물질의 고유한 스팩트럼을 얻어 정량하여 머므름 시간은 4.33분이었으며 상관계수($R^2$)은 0.9998로 양호한 직선상의 그래프를 얻을 수 있었다. 퍼플루오르옥탄설포네이트에 대한 분석법의 회수율은 99.84%로 전반적으로 좋은 회수율을 보였으며 또한 이 연구에 적용되기에 충분한 정밀도와 정확도를 가지고 있음을 확인할 수 있었다. 퍼플루오르옥탄설포네이트 정량한계 및 검출한계는 0.03, 0.009 ug/L이었다. 따라서 식품 용기포장재에서의 분석에 적용이 가능하였다.

Isolation and Identification of Newly Isolated Antagonistic Streptomyces sp. Strain AP19-2 Producing Chromomycins

  • Wu, Xue-Chang;Chen, Wei-Feng;Qian, Chao-Dong;Li, Ou;Li, Ping;Wen, Yan-Ping
    • Journal of Microbiology
    • /
    • 제45권6호
    • /
    • pp.499-504
    • /
    • 2007
  • A new antagonistic strain of actinomycete, designated AP19-2, was isolated from the feces of giant pandas inhabiting the Foping National Nature Reserve in China. Cultural characteristic studies strongly suggested that this strain is a member of the genus Streptomyces. The nucleotide sequence of the 16S rRNA gene of strain AP19-2 evidenced profound similarity (97-99 %) with other Streptomyces strains. Two pure active molecules were isolated from a fermentation broth of Streptomyces sp. strain AP19-2 via extraction, concentration, silica gel G column chromatography, and HPLC. The chemical structures of the two related compounds (referred to as chromomycin $A_2$ and chromomycin $A_3$) were established on the basis of their Infrared spectra (IR), High Resolution Electrospray Ionization Mass Spectrometry (HR-ESI-MS), and Nuclear Magnetic Resonance (NMR) data, and by comparison with published data.

Mediation of Rubradirin Resistance by ABC Transporters (RubT1) from Streptomyces achromogenes var. rubradiris NRRL3061

  • Lamichhane, Janardan;Oh, Tae-Jin;Lee, Hei-Chan;Liou, Kwang-Kyoung;Kim, Chun-Gyu;Sohng, Jae-Kyung
    • Journal of Microbiology and Biotechnology
    • /
    • 제16권12호
    • /
    • pp.1928-1934
    • /
    • 2006
  • The rubradirin biosynthetic gene cluster harbors 58 ORFs within a 105.6-kb sequence, which includes all of the genes responsible for the synthesis of rubradirin, as well as the primary genes relevant to regulatory, resistance, and transport functions. This gene cluster also harbors a resistance-mediating ABC transporter, RubT1, which is located at the most upstream position in the cluster. In the present study, RubT1 was expressed heterologously in E. coli, and the resistance affinity of RubT1 was determined by an antibacterial activity test, as well as by HPLC and ESI-MS analyses. Evidence clearly demonstrates that RubTl mediates rubradirin resistance as an ABC transporter.

Degradation of oxytetracycline by nano zero valent iron under UV-A irradiation: Chemical mechanism and kinetic

  • Hassanzadeh, Parisa;Ganjidoust, Hossein;Ayati, Bita
    • Advances in environmental research
    • /
    • 제3권1호
    • /
    • pp.29-43
    • /
    • 2014
  • Pharmaceutical wastewater effluents are well known for their difficult elimination by traditional biotreatment methods and their important contribution to environmental pollution due to its fluctuating and recalcitrant nature. OTC is one of the nonbiodegradable antibiotics that makes antibiotic-resistant, so it can make be high risk for environment. NZVI can be a good choice for removal of OTC in aqueous solution. Response surface methodology (RSM) was used to optimize the amounts of NZVI and OTC to be used at pH 3 and under 200 W, UV-A irradiation. The responses were removal percent of absorption at 290 and 348 nm, TOC and COD of OTC. In the optimum condition, Linear model was performed 155 ppm of OTC were removed by 1000 ppm NZVI after 6.5 hours and the removal efficiency of absorption at 290 and 348 nm, TOC and COD were 87, 95, 85 and 89 percent, respectively. In the similar process, there is no organic compound after 14 hours. The parameters ORP, DO and pH were investigated for 6:30 hours to study the type of NZVI reaction in process. In the beginning of reaction, oxidation was the dominant reaction after 3 hours, photocatalytic reaction was remarkable. The mechanism of OTC degradation is proposed by HPLC/ESI-MS and four by products were found. Also the rate constants (first order kinetic chain reaction model) were 0.0099, 0.0021, 0.0010, 0.0049 and $0.0074min^{-1}$, respectively.

궁궁이(Angelica polymorpha MAXIM)로부터 분리한 Coumarin 계열 화합물의 Melanin 생합성 억제 활성 (Melanin Biosynthesis Inhibitory Activities of Coumarins Isolated from Angelica polymorpha MAXIM)

  • 이충환;백승화;김진희;김현아;이상명;이찬용;고영희
    • 한국미생물·생명공학회지
    • /
    • 제31권2호
    • /
    • pp.135-139
    • /
    • 2003
  • Melanin 생합성에 key enzyme인 tyrosinase 억제가 melanin색소 억제에 주된 요인으로 알려져 있지만, 생합성기작에는 여러 다른 요인들이 작용하기 때문에 일차적인 탐색 단계에서 tyrosinase 저해 활성뿐만 아니라 S. bikiniensis의 melanin생합성 억제 연구를 병행하여 천연물을 탐색하였다. 그 중 선택된 궁궁이 (Angelica poiymorpha MAXIM)에서 3가지 물질을 분리하였으며, 3가지 물질 모두가 100$\mu\textrm{g}$/$m\ell$ 이상 농도에서도 tyrosinase억제 활성이 나타나지 않는 반면, S. bikiniensis melanin 생합성 저해 효과를 보여 주었다. 동일 농도에서 S. bikinieffsis의 생장에는 영향을 미치지 않았다.

Biocontrol Traits and Antagonistic Potential of Bacillus amyloliquefaciens Strain NJZJSB3 Against Sclerotinia sclerotiorum, a Causal Agent of Canola Stem Rot

  • Wu, Yuncheng;Yuan, Jun;Raza, Waseem;Shen, Qirong;Huang, Qiwei
    • Journal of Microbiology and Biotechnology
    • /
    • 제24권10호
    • /
    • pp.1327-1336
    • /
    • 2014
  • Bacillus amyloliquefaciens strain NJZJSB3 has shown antagonism of several phytopathogens in vitro, especially Sclerotinia sclerotiorum. Both the broth culture and cell suspension of strain NJZJSB3 could completely protect the detached leaves of canola (Brassica napus) from S. sclerotiorum infection. In pot experiments, the application of strain NJZJSB3 cell suspension ($10^8CFU/ml$) decreased the disease incidence by 83.3%, a result similar to commercially available fungicide (Dimetachlone). In order to investigate the potential biocontrol mechanisms of strain NJZJSB3, the nonvolatile antifungal compounds it produces were identified as iturin homologs using HPLC-ESI-MS. Antifungal volatile organic compounds were identified by gas chromatography-mass spectrometry. The detected volatiles toluene, phenol, and benzothiazole showed antifungal effects against S. sclerotiorum in chemical control experiments. Strain NJZJSB3 also produced biofilm, siderophores and cell-wall-degrading enzymes (protease and ${\beta}$-1,3-glucanase). These results suggest that strain NJZJSB3 can be a tremendous potential agent for the biological control of sclerotinia stem rot.

홍어류(Dipturus chilensis) 껍질로부터 분리 정제된 collagenase-1 저해 펩타이드의 특성 (Characterization of a Collagenase-1 Inhibitory Peptide Purified from Skate Dipturus chilensis Skin)

  • 박성하;이정권;전중균;변희국
    • 한국수산과학회지
    • /
    • 제44권5호
    • /
    • pp.456-463
    • /
    • 2011
  • We attempted to isolate a collagenase-1 inhibitory peptide from skate Dipturus chilensis skin protein. The protein from skate skin was digested by various enzymes (alcalase, ${\alpha}$-chymotrypsin, neutrase, papain, pepsin, and trypsin) to produce a collagenase-1 inhibitory peptide. The collagenase-1 inhibitory activity of the peptides obtained was measured by gelatin digestion assay. Among the six hydrolysates, pepsin hydrolysate exhibited the highest collagenase-1 inhibitory activity. The peptide showing strong collagenase-1 inhibitory activity was purified by Sephadex G-25 gel chromatography and HPLC using an octadecylsilyls (ODS) column. The amino acid sequence of purified collagenase-1 inhibitory peptide was identified to be Asn-Leu-Asp-Val -Leu-Glu-Val-Phe (961 Da) by quadrupole time of flight (Q-TOF) and electrospray ionization mass spectrometry (ESI-MS) mass spectroscopy. The $IC_{50}$ value of purified peptide was 87.0 ${\mu}M$. Moreover, the peptide did not exhibit cytotoxic effects on human dermal fibroblast cell lines.