• Title/Summary/Keyword: HPLC-MS-MS

Search Result 911, Processing Time 0.037 seconds

Chip-based microcapillary HPLC for proteomic analysis (칩 기반 미세관 HPLC를 이용한 단백체 분석)

  • Kim, Bo-Ra;Park, Jong-Moon;Lee, Hoo-Keun
    • Analytical Science and Technology
    • /
    • v.24 no.6
    • /
    • pp.407-413
    • /
    • 2011
  • Over the last decade sophisticated and powerful microcapillary HPLC for proteomic analysis have been developed increasingly and interfaced with high resolution tandem mass spectrometers. Separation prior to mass spectrometric (MS) analysis removes impurities, and concentrates analytes in the narrow elution peaks, resulting in increased sensitivity of MS analysis. This review will focus on the recent advances of on-line highperformance separation techniques based on microfluidic chips for complex proteomic analysis.

Formation of Acycloretinoic Acid by Autoxidation of Lycopene (Lycopene의 자동산화에 의한 Acycloretinoic acid의 생성)

  • Kim, Seon-Jae
    • Korean Journal of Food Science and Technology
    • /
    • v.32 no.6
    • /
    • pp.1437-1441
    • /
    • 2000
  • Acycloretinoic acid was prepared from acycloretinal by oxidation with Tollens reagent. Acycloretinoic acid was separated with Silica-HPLC and analyzed by ODS-HPLC with a photodiode array detector and by GC-MS. Lycopene was solubilized in toluene and aqueous Tween 40, and then oxidized by incubating at $37^{\circ}C$ under atmospheric oxygen. Acidic compound was produced by autoxidation of lycopene. Retention time, UV-Vis spectra and mass spectra of the acidic compound were identical to the standard acycloretinoic acid. Thus, acycloretinoic acid was confirmed to occur in vitro under oxidation condition of lycopene.

  • PDF

Evaluation of the Method for Total Homocysteine in Plasma Using LC-MS/MS (LC-MS/MS를 이용한 Homocysteine 측정과 그 유용성 평가)

  • Jun, Sun-Hee;Lim, Mi-Suk;Jung, Yong-Sun;Song, Jung-Han
    • Korean Journal of Clinical Laboratory Science
    • /
    • v.37 no.1
    • /
    • pp.22-26
    • /
    • 2005
  • Total homocysteine is now considered a risk factor for cardiovascular diseases. I increased interest has led to a multitude of studies requiring the determination of total homocysteine in conjunction with other factor. There are various methods for measuring total homocysteine, including HPLC, FPIA, GC-MS and LC-MS/MS. The most recent method for measuring total homocysteine uses a deuterium-labelled internal standard and tandem mass spectrometry. This development requires no derivatization and therefore leads to an increase in sample throughput compared to other techniques. We have evaluated the method for homocysteine by the LC-MS/MS method, and the correlation between the FPIA method and the LC-MS/MS method. The standard curve (0, 5, 10, 20, 50, 100 uM) was linear over the range examined (up to 100 uM). The lower limit of quantification (CV < 10 %) was 0.5 uM/L and the lower limit of detection (S/N >3) was 0.1 uM/L. Intra-assay variation and inter-assay variation were both <6 %. The comparision study for homocysteine concentration showed good correlation (r=0.9684) between the FPIA method and LC-MS/MS methods. Our conclusion is that the method showed relatively good precision, and was rapid and accurate.

  • PDF

Analysis of Phytochemicals in Popular Medicinal Herbs by HPLC and GC-MS (HPLC와 GC/MS를 활용한 약용식물 유래 phytochemicals 분석)

  • Cho, Hyun-Jung;Yoo, Dong-Chan;Cho, Hyun-Nam;Fan, Lu-An;Kim, Hee-Joon;Khang, Kong-Won;Jeong, Ho-Soon;Yang, Seun-Ah;Lee, In-Seon;Jhee, Kwang-Hwan
    • Korean Journal of Food Science and Technology
    • /
    • v.40 no.3
    • /
    • pp.277-282
    • /
    • 2008
  • Oriental herbs are reported as having potent functions for preventing many types of diseases. They also appear to have positive effects and potential capabilities for skin care. Among the many oriental herbs that are available, we chose to analyze four medicinal herbs, Korean red ginseng, Artemisia capillaries Thunb, Schizonepeta tenuifolia Briq, and Foeniculum vulgare Mill, because all are popular and considered as favorite medicinal plants in Korea. Extracts of the herbs were obtained by various methods such as using distilled water, ethyl ether, methanol, ethanol, benzene, 1-butanol, and chloroform. Nine phytochemicals were detected in the extracts: maltol, adenosine, b-pinene, menthone, pulegone, limonene, anethole, estragole, and fenchone, which reportedly have multi-functionalities. All phytochemicals were analyzed quantitatively by various chromatographic techniques such as HPLC and gas chromatography-mass (GC-MS) spectrometry. This article also presents the optimum conditions for extracting these 9 targeted phytochemical compounds that were derived from 4 popular oriental herbs, which could be useful for the efficient preparation of each phytochemical.

Determination of ginsenosides in Asian and American ginsengs by liquid chromatography-quadrupole/time-of-flight MS: assessing variations based on morphological characteristics

  • Chen, Yujie;Zhao, Zhongzhen;Chen, Hubiao;Brand, Eric;Yi, Tao;Qin, Minjian;Liang, Zhitao
    • Journal of Ginseng Research
    • /
    • v.41 no.1
    • /
    • pp.10-22
    • /
    • 2017
  • Background: Asian ginseng and American ginseng are functional foods that share a close genetic relationship and are well-known worldwide. This article aims to investigate the correlation between morphological characteristics and the inherent quality of Asian and American ginsengs. Methods: In this study, an ultra-HPLC-quadrupole/time-of-flight MS (UHPLC-Q/TOF-MS) method was established for the quantitative analysis of 45 ginseng samples. The method developed for determination was precise and accurate. Results: The results showed that Asian ginseng samples with the same growing time (with the same or similar number of stem scars) that had a thinner main root, a longer rhizome and more branch roots contained greater amounts of ginsenosides. For American ginseng, two tendencies were observed in the relationship between the diameter of the main root and contents of ginsenosides. One tendency was that samples with thinner main roots tended to contain higher levels of ginsenosides, which was observed in the samples sold under the commercial name pao-shen. Another tendency was that samples with thicker main roots contained higher contents of ginsenosides, which was observed in the samples sold under the commercial name pao-mian, as well as in samples of American ginseng cultivated in Jilin, China. Conclusion: An approach using ultra-HPLC-quadrupole/time-of-flight MS was successfully established to link morphology and active components for evaluating the quality of Asian and American ginsengs. Clear correlation between visible morphological features and quality of Asian and American ginsengs was found. People can see the difference; this means consumers and vendors can evaluate ginseng by themselves.

Component Analysis of Suaeda asparagoides Extracts (나문재 추출물의 성분 분석)

  • Yang, Hee-Jung;Park, Soo-Nam
    • Journal of the Society of Cosmetic Scientists of Korea
    • /
    • v.34 no.3
    • /
    • pp.157-165
    • /
    • 2008
  • In the previous study, the anti-oxidant activity of oxtract/fraction of Sueada aspparagoides(SA) and the stability test for the cream containing SA extract were investigated respectively[1,2]. In this study, the components of SA extract were analyzed by TLC, HPLC, and LC/ESI-MS/MS, $^1H$-NMR. TLC chromatogram of ethyl acetate fraction of SA extract revealed 5 bands $(SA1{\sim}SA5)$. HPLC chromatogram of aglycone fractions obtained from deglycoylation reaction of ethyl acetate fraction showed 2 bands (SAA 2 and SAA 1), which were identified as quercetin (composition ratio, 16.88%) and kaempferol (83.12%) in the order of elution time. Among 5 bands of TLC chromatogram, 4 bands $(SA2{\sim}SA5)$ also were Identified as kaempferol-3-O-glucoside (SA 2), quercetin-3-O-glucoside (SA3), kaempferol-3-O-rutinoside (SA 4), quercetin-3-O-rutinoside (SA 5) by LC/ESI-MS/MSMS/MS. respectively. The spectrum generated for SAA 1 by LC/ESI-MS/MS in the negative ion mode also gave the ion corresponding to the deprotonated aglycone $[M-H]^-$ (285m/z), the $^1H$-NMR spectrum contained signals [${\delta}$ 6.19 (1H, d, J=1.8Hz, H-6), ${\delta}$ 6.44 (1H, d, J=1.8Hz, H-8), ${\delta}$ 6.92 (2H, d, J=9.0Hz, H-3', 5'), ${\delta}$ 8.04 (2H, d, J=9.0Hz, H-2', 6', thus SAA 1 was identified as kaempferol. SAA 2 yielded the deprotonated agycone ion $[M-H]^-$ (301m/z), $^1H$-NMR spectrum showed signals [${\delta}$ 6.20 (1H, d, J=2.0Hz, H-6), ${\delta}$ 6.42 (1H, d, J=2.0Hz, H-8), ${\delta}$ 6.90 (1H, d, J=8.6Hz, H-5'), ${\delta}$ 7.55 (1H, dd, J=8.6, 2.2Hz, H-6'), ${\delta}$ 7.69 (1H, d, J=2.2Hz, H-2', thus SAA 2 was Identified as quercetin. In conclusion, with the anti-oxidant activity and the stability test reported previously, component analysis of SA extracts could be applicable to new cosmeceuticals.

Study on the Pyrolysis of Polyphenols from Tobacco by Direct Inlet/MS (Direct Inlet/MS를 이용한 잎담배중 폴리페놀 화합물의 열분해에 관한 연구)

  • 박진우
    • YAKHAK HOEJI
    • /
    • v.26 no.2
    • /
    • pp.123-128
    • /
    • 1982
  • Direct inlet/MS was used to investigate the pyrolysis pathway and the pyrolyzates of tobacco polyphenols as precursor of catechol which has been known as one of the most potent co-carcinogen from cigarette smoke. Caffeic acid, catechol and quercetin, catechol were detected from the pyrolyzates of chlorogenic acid and rutin, respectively. Interrelationship between polyphenols from tobacco leaf and catechol from cigarette smoke was investigated by using HPLC and GC. These results reveal that chlorogenic acid is the most significant precursor of catechol in cigarette smoke.

  • PDF

Analysis of Sildenafil and its Analogues by LC/MS/MS (LC/MS/MS를 이용한 sildenafil 및 그 유사체 분석)

  • Myung, Seung-Woon;Park, So-Hee;Cho, Hyun-Woo
    • Analytical Science and Technology
    • /
    • v.16 no.6
    • /
    • pp.488-498
    • /
    • 2003
  • By LC/MS/MS, the analytical method of sildenafil and its analogues (homosildenafil, vardenafil and tadalafil) used as used medical treatment of impotence was established. electrosprary ionization (ESI) and atmospheric pressure chemical ionization (APCI) as a ionization method were applied. Several parameter were varied and the sensitivity and reproducibility were compared. In LC/ESI-MS method, capillary voltage, cone voltage, extractor, entrance and RF lens to create appropriate productr ions for multiple reaction monitoring (MRM) were variable parameter, but the formation of the other product ions except the precursor ion could not detect. And the value of entrance, collision energy, exit, corona voltage, cone voltage, extractor, RF lens, cone gas, and desolvation gas in APCI mode were varied, only the creation pattern of fragment ions by the change of RF lens value were detected, and the limit of detection was decreased due to the increase of S/N. Ten millimole ammonium formate (pH 4.8):acetonitrile=70:30 by isocratic elution in HPLC system was shown the maximum sensitivity in MS, the detection limit of sildenafil, homosildenafil, vardenafil and tadalafil obtained by ESI-MRM were 0.10, 0.025, 0.025, and $0.25{\mu}g/mL$ at S/N>5, respectively.

Separating of Falcarinol from Acanthopanax senticosus (가시오가피(Acanthopanax senticosus)에서 polyacetylene계 화합물인 falcarinol의 동정)

  • Kim, Seong-Ju;Chang, Kyu-Seob
    • Korean Journal of Food Science and Technology
    • /
    • v.37 no.3
    • /
    • pp.360-363
    • /
    • 2005
  • To detect falcarinol in Acanthopanax senticosus, its stem and bark were extracted with methanol fractionated with petroleum ether and diethyl ether, and separated by silica gel column chromatography, Resulting six crude samples were compared with standard falcarinol through TLC on silica gel plates. Fraction 6 showed $R_{f}$ value of 0.46 similar to that of standard falcarinol. Through analytical reverse phase HPLC/PDA, UV spectra of standard falcarinol and traction 6 recorded between 200 and 340 nm showed identical peaks and UV spectra patterns. GC/MS revealed standard falcarinol and fraction 6 have equal retention times of 7.4 and 8.5 min before and after TMS-derivatization, respectively. Standard falcarinol and fraction 6 showed more similar spectrum patterns after TMS-derivatization than before. These results confirm presence of falcarinol in A. senticosus.