• Title/Summary/Keyword: UV spectrometry

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Qualitative and quantitative analysis of the saponins in Panax notoginseng leaves using ultra-performance liquid chromatography coupled with time-of-flight tandem mass spectrometry and high performance liquid chromatography coupled with UV detector

  • Liu, Fang;Ma, Ni;He, Chengwei;Hu, Yuanjia;Li, Peng;Chen, Meiwan;Su, Huanxing;Wan, Jian-Bo
    • Journal of Ginseng Research
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    • v.42 no.2
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    • pp.149-157
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    • 2018
  • Background: Panax notoginseng leaves (PNL) exhibit extensive activities, but few analytical methods have been established to exclusively determine the dammarane triterpene saponins in PNL. Methods: Ultra-performance liquid chromatography coupled with time-of-flight mass spectrometry (UPLC/Q-TOF MS) and HPLC-UV methods were developed for the qualitative and quantitative analysis of ginsenosides in PNL, respectively. Results: Extraction conditions, including solvents and extraction methods, were optimized, which showed that ginsenosides Rc and Rb3, the main components of PNL, are transformed to notoginsenosides Fe and Fd, respectively, in the presence of water, by removing a glucose residue from position C-3 via possible enzymatic hydrolysis. A total of 57 saponins were identified in the methanolic extract of PNL by UPLC/Q-TOF MS. Among them, 19 components were unambiguously characterized by their reference substances. Additionally, seven saponins of PNL-ginsenosides Rb1, Rc, Rb2, and Rb3, and notoginsenosides Fc, Fe, and Fd-were quantified using the HPLC-UV method after extraction with methanol. The separation of analytes, particularly the separation of notoginsenoside Fc and ginsenoside Rc, was achieved on a Zorbax ODS C8 column at a temperature of $35^{\circ}C$. This developed HPLC-UV method provides an adequate linearity ($r^2$ > 0.999), repeatability (relative standard deviation, RSD < 2.98%), and inter- and intraday variations (RSD < 4.40%) with recovery (98.7-106.1%) of seven saponins concerned. This validated method was also conducted to determine seven components in 10 batches of PNL. Conclusion: These findings are beneficial to the quality control of PNL and its relevant products.

Analysis of High Volume Slit Type Two-Stage Virtual Impactor for Particle Size Classification (특정크기 입자농축을 위한 대유량 슬릿형 2단 가상충돌기의 성능분석)

  • 박성호;김상수;오명도
    • Transactions of the Korean Society of Mechanical Engineers
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    • v.15 no.1
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    • pp.285-291
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    • 1991
  • A two-stage slit type virtual impactor based on the concept of the single stage virtual impactor has been designed, fabricated, and evaluated for the purpose of concentrating the suspended particles in the air with the size range of 1.8-4.5 .mu.m and handling large flow volume. Monodisperse methylene blue particles have been generated with vibrating orifice aerosol generator (VOAG). The separation efficiency and concentration efficiency have been measured by the UV-visible absorption spectrometry. Previous study for a single stage virtual impactor were used to determine the design parameters such as 50% cut-off sizes and dimensions of the two stage virtual impactor. The separation efficiency curve and 50% cut-off Stokes number(cut-off sizes) are not sensitive to the nozzle Reynolds number, but sensitive to the ratio between the minor flow rate and the total flow rate, The measured concentration efficiency was compared with the maximum concentration efficiency determined by the separation efficiencies of the first and the second stages. The differences between the measured and the maximum concentration efficiencies result from the wall loss due to the deposited particles on the internal walls inside the impactor.

Extraction Characteristics of Dried Asian Lacquer by Solvents Before and After UV Degradation (자외선 열화 전후 건조 옻의 용매별 용출 특성)

  • Park, Jongseo;Schilling, Michael R.;Khanjian, Herant;Heginbotham, Arlen
    • Journal of Conservation Science
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    • v.36 no.2
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    • pp.103-111
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    • 2020
  • To compare the cleaning effect of solvents such as water and ethanol used to clean lacquer relics, the components extracted with various solvents were analyzed. A freshly dried lacquer sample and a lacquer sample exposed to ultraviolet radiation for 24 days were treated with water, ethanol, acetone, and hexane, and the dissolved material was detected by pyrolysis-gas chromatography-mass spectrometry. The amount extracted was significantly higher in acetone and ethanol than in hexane, a nonpolar solvent. Water, a highly polar solvent, was relatively efficient for extracting low-molecular-weight materials. After experiencing 24 days of ultraviolet radiation, the lacquer exhibited a significant increase of extracted materials compared with the nonexposed one. This may be due to the degradation of the urushiol chain in the form of polymers, resulting in the formation of low-molecular-weight polar substances, including dicarboxylic acids. In addition to the deterioration status of lacquer relics, such solvent extraction properties will be a crucial consideration in selecting the appropriate cleaning solvent.

The Complex Formation of Fe(III)-Salicylic acid (Fe(III)-Salicylic acid의 착물 형성에 관한 연구)

  • Cha, Ki-Won;Park, Kwang-Won
    • Analytical Science and Technology
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    • v.8 no.3
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    • pp.305-311
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    • 1995
  • The stability constant of the complex between salicylic acid($H_2A$) and Fe(III) ion has been determined using UV-Vis absorption spectrometry and pH titration method in O.1M $KNO_3$ aqueous solution at $20^{\circ}C$ and compared with reference value, $logK_f=16.48$. The $pK_{a1}$ and $pK_{a2}$ of $H_2A$ are $2.92{\pm}0.08$ and $12.90{\pm}0.13$, respectively and the $logK_f$ of 1:1 complex Fe(III)-$H_2A$ system is $11.88{\pm}0.12$ at $20^{\circ}C$.

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Determination and confirmation of the carbendazim residue in soybean sprout (콩나물중 살균제 carbendazim 잔류분의 정량 및 확인)

  • Kim, Young-Gook;Park, Jong-Tae;Hong, Suk-Soon
    • The Korean Journal of Pesticide Science
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    • v.2 no.3
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    • pp.79-84
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    • 1998
  • Tandem HPLC and atmospheric pressure chemical ionization(APcI) LC/MS method was used for the determination and confirmation of carbendazim residues in soybean sprout. Fluorescence(FL) detector was connected in tandem with the ultraviolet(UV) detector for dual detection of the carbendazim residue at the excitation and emission wavelength of 280 nm and 310 nm, respectively. The limit of detection for carbendazim was $0.1{\mu}g/kg$ sample. Recoveries of carbendazim from fortified soybean sprout at 0.5, 1.0 and 2.0 ppm were averaged 89.1%. Mass spectrometry using a APcI source confirmed the carbendazim residue in the soybean sprout sample. Fragmentation pattern on the APcI LC/MS spectrum of carbendazim was simpler than that from electron impact(EI) mass spectrum. Carbendazim produced 3 major ions including m/z 133, m/z 159 and m/z 191($M^{+}$). This method was sensitive enough to provide reliable and reproducible results for practical applications.

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A Study on Contents of Anti-impotence drug/drug-like compounds in Food (식품중 발기부전 치료제 및 유사물질 함량에 관한 조사연구)

  • Hong, Hae-Geun;Bang, Seon-Jae;Park, Kwang-Hee;Lee, In-Sook;Park, In-Jung;Park, Jeung-Hwa;Kim, Jong-Chan
    • Journal of environmental and Sanitary engineering
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    • v.22 no.3
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    • pp.89-96
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    • 2007
  • To determine 8 anti-impotence drug/drug-like compounds such as sildenafil, vardenafil, tadalafil, homosildenafil, hydroxyhomosildenafil, aminotadalafil, pseudovardenafil and hongdenafil in foods, simultaneously, high performance liquid chromatography(HPLC) and liquid chromatography-mass spectrometry (LC/MS) were used. The HPLC/UV analysis was performed on a column of capcellpak $C_{18}$ with 0.1% sodium-1-hexansulfonate in 0.2M ammonium formate/acetonitrile as a mobile phase. Mass spectra of the compounds by LC/MS were investigated with SCAN mode(Mass range and Fragment voltage) and SIM(Selected Ion Monitoring) mode (Ion target and Fragment voltage). The results follow as; 1. The HPLC/UV analysis was detected from 5 out of 63 samples. The content of sildenafil was in the range of 32.80 ppm ${\sim}$ 60.13 ppm from 4 out of 5 samples. The contents of sildenafil, vardenafil, homosildenafil were in the range 47.14 ppm from 1 out of 5 samples. 2. The conformed result of LC/MS was equal of detected from 5 out of 63 samples in HPLC/UV analysis. An easily available, simultaneous determination of 8 standards in adulterated health related foods was established by using a combination of LC/MS methods.

The Study on the Intercalation-Deintercalation of Potassium-Carbon Fiber Intercalation Compounds (칼륨-탄소섬유층간화합물의 Intercalation-Deintercalation에 관한 연구)

  • Oh, Won-Chun;Cho, Sung-Jun;Choi, Young-Jai;Ko, Young-Shin
    • Analytical Science and Technology
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    • v.7 no.2
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    • pp.193-199
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    • 1994
  • We have synthesized K-CFICs by the modified two-bulb method. These synthesized compound were analysed with X-ray diffractometer and UV/VIS spectrophotometer. According to X-ray diffraction analysis, the intercalation of potassium between the carbon layers of carbon fiber was better then other intercalants. From obtained data for this deintercalation process, we can see that a number of potassiums were presented as a residue between the carbon layers and this residue compounds had a stability for a long term. Therefore, it is appear that these compounds have a capability as new useful material. From UV/VIS spectrometry data, we can suppose that spectrum of K-CFICs synthesized at $250^{\circ}C$ had only a $R_{min}$, and spectra of any other compounds were not appeared charecteristic peaks because potassium ions were little affect the energy levels of original carbon fiber.

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Flavonoidal constituent in Korean Lactuca dentata Makino (한국산 씀바귀의 Flavonoid 성분에 관한 연구)

  • Chung, Kang-Hyun;Yoon, Kwang-Ro;Kim, Jun-Pyong
    • Journal of the Korean Society of Food Culture
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    • v.9 no.2
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    • pp.131-136
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    • 1994
  • The ethylacetate extract of Lactuca dentata Makino showed 6 flavonoidal components as detected by ferric chloride solution. The flavonoidal constituent of Lactuca dentata Makino was isolated and purified by the series of column chromatography. The chemical structure of one of the flavonoidal component named as compound E was identified by UV, IR and NMR spectrometry. The melting point range of compound E was $249.5^{\circ}C-251^{\circ}C$. The UV and IR spectra of purified compound E, and its genin were measured with the various shifting agents. The results of UV analysis showed the free state of hydroxy group at 3rd and 4th carbon and binding of sugar at the 7th carbon of compound. The sugar bound to the compound E was identified as glucose by TLC. The IR spectrum showed the presense of hydroxy group, conjugated carbonyl group and aromatic group. The analysis of NMR spectrum was done to the purified compound and its derivatives. The chemical shifts against hydrogen atom, hydroxy group, and the moiety of luteolin were observed in the NMR spectrum along with their position and number as well as type of sugar bound. The isolated and purified compound was identified as $luteolin-7-0-{\beta}-D-glucoside$.

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Improved HPLC-UV method for determination of five synthetic dyes in Typha orientalis

  • Ko, Kyung Yuk;Choi, Eun Young;Jeong, Se Hee;Paek, Ock jin;Lee, Chan;Heo, Huijin;Oh, She-Wook;Lee, Chulhyun;Kang, Juhye;Cho, Sooyeul
    • Analytical Science and Technology
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    • v.34 no.4
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    • pp.160-171
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    • 2021
  • Synthetic azo dyes are used extensively in herbal medicines to render the medicines more visually attractive to consumers. This study developed and validated a rapid high-performance liquid chromatography (HPLC) method to determine whether synthetic colorants such as Tartrazine, Auramine O, Metanil yellow, Sunset yellow, and Orange II are used extensively in Typha orientalis. To increase the recovery of the synthetic dyes, this method employed containing 50 mM ammonium acetate in 70 % methanol at first extraction and 100 mM HCl in 70 % methanol at second extraction. Five synthetic pigments in Typha orientalis were separated by gradient elution with a mobile phase consisting of acetonitrile and 50 mM ammonium acetate in distilled water at ultra-violet (UV) detection 428 nm or 500 nm. Additionally, this study established the liquid chromatography tandem mass spectrometry (LC-MS/MS) method to confirm positive samples suspected by HPLC results. The HPLC-UV method had good linearity, indicating r2> 0.999. The recoveries of the samples spiked with three different concentration ranged from 73.8~91.5 %, and relative standard deviation values indicated 0.2~5.2 %. The established LC-MS/MS could successfully identify the synthetic pigments in herbal medicine samples. The study demonstrates that Typha orientalis adulterated by yellowish synthetic dyes can be successfully distinguished when using the HPLC-UV method.

Polycrystalline silicon thin film fabricated on plastic substrates by excimer laser annealing (엑시머 레이저 어닐링을 이용하여 플라스틱 기판에 형성한 다결정 실리콘 박막의 특성)

  • 조세현;이인규;김영훈;문대규;한정인
    • Journal of the Korean Vacuum Society
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    • v.13 no.1
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    • pp.29-33
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    • 2004
  • In this paper, we investigated the ultra-low temperature(<$150^{\circ}C$) polycrystalline silicon film on plastic substrate application using RF-magnetron sputtering and excimer laser annealing. Amorphous silicon films were deposited using Ar/He mixture gas at $120^{\circ}C$ and in-film argon concentration was less than 2%, which was measured to Rutherford Backscattering Spectrometry. At energy density 320mJ/$\textrm{cm}^2$, RMS roughness was 267$\AA$ and UV crystallinity was 62%. The grain size varies from 50nm to 100nm after excimer laser irradiation.