• Title/Summary/Keyword: high performance liquid chromatography-mass spectrometry (HPLC-MS)

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Analysis of Fatty Acyl Groups of Diacyl Galactolipid Molecular Species by HPLC/ESI-MS with In-source Fragmentation

  • Gil, Ji-Hye;Hong, Jong-Ki;Choe, Joong-Chul;Kim, Young-Hwan
    • Bulletin of the Korean Chemical Society
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    • v.24 no.8
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    • pp.1163-1168
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    • 2003
  • The structures of molecular species of galactolipids, such as monogalactosyl diacylglycerol (MGDG) and digalactosyl diacylglycerol (DGDG), isolated from wheat flour have been investigated using negative-ion electrospray ionization (ESI) mass spectrometry interfaced with high performance liquid chromatography (HPLC). According to the result of HPLC analysis, MGDG and DGDG were found to consist of mixtures of five and four molecular species, respectively. The galactolipids have been also analyzed to determine their fatty acid compositions, using HPLC/ESI-MS combined with in-source (or cone voltage) fragmentation. HPLC/ ESI-MS is very useful for one-step analysis of mixtures of galactolipids with a small sample quantity. Especially, the carboxylate anions produced in in-source fragmentations of the negative-ion of each component separated by HPLC provide valuable information on the composition of its fatty acyl chains.

Transformation of dissolved organic matter in a constructed wetland: A molecular-level composition analysis using pyrolysis-gas chromatography mass spectrometry

  • Park, Jongkwan;Choi, Mijin;Cho, Jaeweon;Chon, Kyongmi
    • Environmental Engineering Research
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    • v.23 no.4
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    • pp.390-396
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    • 2018
  • This study investigated the transformation of dissolved organic matter (DOM) in a free-water surface flow constructed wetland. Pyrolysis gas chromatography-mass spectrometry (Py-GC/MS) coupled with preparative high-performance liquid chromatography (prep-HPLC) was used to analyze the compositions of biopolymers (polysaccharides, amino sugars, proteins, polyhydroxy aromatics, lipids and lignin) in DOM according to the molecular size at three sampling points of the water flow: inflow, midflow, and outflow. The prep-HPLC results verified the decomposition of DOM through the decrease in the number of peaks from three to one in the chromatograms of the sampling points. The Py-GC/MS results for the degradable peaks indicated that biopolymers relating to polysaccharides and proteins gradually biodegraded with the water flow. On the other hand, the recalcitrant organic fraction (the remaining peak) in the outflow showed a relatively high concentration of aromatic compounds. Therefore, the ecological processes in the constructed wetland caused DOM to become more aromatic and homogeneous. This indicated that the constructed wetland can be an effective buffer area for releasing biochemically stable DOM, which has less influence on biological water quality indicators, e.g., biochemical oxygen demand, into an aquatic ecosystem.

Identification of Ceftiofur Oxidation Products by High-Performance Liquid Chromatography/Electrospray Ionization/Tandem Mass Spectrometry

  • Lim, Young-Hee;Park, Deok-Hie;Youn, Yeu-Young;Kim, Kyung-Hoon;Cho, Hye-Sung
    • Mass Spectrometry Letters
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    • v.2 no.1
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    • pp.16-19
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    • 2011
  • Oxidation products of ceftiofur were formed in hydrogen peroxide solution. The structures of the ceftiofur oxidation products were characterized by high-performance liquid chromatography/electrospray ionization/tandem mass spectrometry (HPLC/ESI/MS/MS). The products were identified as compounds oxidized at the sulfur of a cephem ring. For further analysis, experiments were performed using $O^{18}$-labeled hydrogen peroxide. In addition, density-functional calculations were carried out for six possible oxidation products to support the experimental results.

Profiling of the leaves and stems of Curcuma longa using LC-ESI-MS and HPLC analysis

  • Gia Han Tran;Hak-Dong Lee;Sun-Hyung Kim;Seok Lee;Sanghyun Lee
    • Journal of Applied Biological Chemistry
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    • v.66
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    • pp.338-344
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    • 2023
  • Curcuma longa is a plant belonging to the genus Curcuma and is distributed across various Asian regions. This plant is widely known for its rhizomes, which possess a variety of pharmacological properties. However, although the leaves and stems of this plant also contain several health-promoting secondary metabolites, very few studies have characterized these compounds. Therefore, our study sought to quantify the secondary metabolites from the leaves and stems of Curcuma longa L. (LSCL) using liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS) and high-performance liquid chromatography (HPLC). Our LC-ESI-MS analyses detected twenty-one phenolic compounds in the LSCL, among which fifteen compounds were detected via HPLC analysis. Four compounds, namely vanillic acid (0.129 mg/g), p-coumaric acid (0.431 mg/g), 4-methylcatechol (0.199 mg/g), and afzelin (0.074 mg/g) were then quantified. These findings suggest that LSCL is rich in secondary metabolites and holds potential as a valuable resource for the development of functional and nutritional supplements in the future.

Qualitative Analysis of the Major Constituents in Traditional Oriental Prescription Bang-poong-tong-sung-san by Liquid Chromatography/Ultraviolet Detector/Ion-Trap Time-of-Flight Mass Spectrometry

  • Eom, Han Young;Kim, Hyung-Seung;Han, Sang Beom
    • Mass Spectrometry Letters
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    • v.5 no.1
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    • pp.24-29
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    • 2014
  • An advanced and reliable high performance liquid chromatography (HPLC)/ultraviolet detector (UV)/ion-trap time-of-flight (IT-TOF) mass spectrometry was developed for the simultaneous quantification of 19 marker compounds in Bang-poong-tong-sung-san (BPTS), a traditional oriental prescription. Various parameters affecting HPLC separation and IT-TOF detection were investigated, and optimized conditions were identified. The separation was achieved on a Capcell PAK C18 column ($1.5mm{\times}250mm$, $5{\mu}m$ particle size) using a gradient elution of acetonitrile and water containing 0.1% formic acid at a flow rate of 0.1 mL/min. The column temperature was maintained at $40^{\circ}C$ and the injection volume was $2{\mu}L$. IT-TOF system was equipped with an electrospray ion source (ESI) operating in positive or negative ion mode. The optimized electrospray ionization parameters were as follows: ion spray voltage, +4.5 kV (positive ion mode), or -3.5 kV (negative ion mode); drying gas ($N_2$), 1.5 L/min; heat block temperature, $200^{\circ}C$. Automatic $MS^n$ (n = 1~3) analyses were carried out to obtain structural information of analytes. Elemental compositions and their mass errors were calculated based on their accurate masses obtained from a formula predictor software. The marker compounds in BPTS were identified by comparisons between $MS^n$ spectra from standards and those from extracts. Moreover, the libraries of $MS^2$ and $MS^3$ spectra and accurate masses of parent and fragment ions for marker compounds were constructed. The developed method was successfully applied to the BPTS extracts and identified 17 out of 19 marker compounds in the BPTS extracts.

Analysis of Gingerol Compounds of Raw Ginger (Zingiber officinale Roscoe) and Its Paste by High Performance Liquid Chromatograph-Mass Spectrometry (LC/MS) (LC/MS에 의한 원료생강 및 생강 페이스트 중의 Gingerol 화합물 분석)

  • 조길석
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.29 no.5
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    • pp.747-751
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    • 2000
  • This study was carried out to improve the analysis method of gingerol compounds from ginger (Zingiber officinale Roscoe). Pungent components of ginger were extracted by acetone and lisolated by thin layer chromatography (TLC) and high performance liquid chromatography (HPLC) with LiChrosorb RP-18 column. Three homologues of gingerols were identified by HPLC-mass spectrometry (LC/MS) and nuclear magnetic resonance (NMR). The contents of [6]-, [8]- and [10]-gingerols in three homologues identified were 635.3 mg%, 206.6 mg% and 145.7 mg% in raw ginger, and were 418.2 mg%, 142.6 mg% and 103.3 mg% in ginger paste, respectively.

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Simultaneous analysis of sulfonamides in beef and pork by high performance liquid chromatography and electrospray ionization mass spectrometry (HPLC와 LC/MS에 의한 식육내 잔류 설파제의 동시 분석법)

  • 정봉수;박준조;금모래;김인경;박병옥;한정희
    • Korean Journal of Veterinary Service
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    • v.27 no.1
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    • pp.17-29
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    • 2004
  • A multiresidual analysis was performed to determine 12 sulfonamides(sulfacetamide, sulfadiazine, sulfisomidine, sulfathiazole, sulfapyridine, sulfamerazine, sulfamethazine, sulfamonomethoxine, sulfisoxazole, sulfamethoxazole, sulfaquinoxaline, and sulfadimethoxine) in beef and pork simultaneously. The multiresidual analysis for the sulfonamides currently used was able to analyze 5 kinds of sulfonamides at the same time. The method of this 12 sulfonamides multiresidual analysis in this study was matrix solid-phase dispersion(MSPD) by high performance liquid chromatography (HPLC) and liquid chromatography mass spectrometry (LC/MS). The recovery rate of the materials was measured by MSPD method with 3 different extraction solvents; Dichloromethane, DCM: Ethylacetate(3:1), DCM:EA(9:1). Also, samples (84 beef and 205 pork samples) which were positive by EEC-4 plate test from 2001 to 2003 were tested to investigate the kinds of sulfonamides using HPLC. The results from the study were as follows; 1. The recovery rate of the materials was measured by MSPD method with 3 different extraction solvents; Dichloromethane, DCM:Ethylacetate(3:1), DCM:EA(9:1). The method of extraction solvent with DCM:ethyl acetate(9:1) was the most excellent(87.7∼99.3%) in separation and reappearance. 2. In the LC/MS analysis. of sulfonamides, signal to noise ratio was showed relatively high in the positive mode and special ion in the quality analysis was determined via [M+H]$\^$+/ and m/z 156. A spectrum of sulfonamides was showed from all 12 sulfonamides. 3. The samples positive by the EEC-4 plate, a screening test method, were categorized by sulfonamides through Charm II and confirmed the kinds of sulfonamides through HPLC. 1) Among 84 beef samples positive by EEC-4 plate, 20 samples were positive by Charm II and identified as 7 sulfamethazine, 9 sulfadimethoxine, 1 sulfamonomethoxine and 3 unknown status. 2) Among 205 pork samples positive by EEC-4 plate, 42 samples were positive by Charm II and identified as 19 sulfamethazine, 1 sulfadimethoxine, 4 sulfamonomethoxine and 5 unknown status.

Determination of thyroid hormones by solid-phase extraction using high performance liquid chromatograph/diode array detector/electro-spray ionization mass spectrometry in urine samples (HPLC/DAD/ESI-MS 및 고체상 추출법을 이용한 뇨시료중 갑상선 호르몬 분석)

  • Kwak, Sun Young;Moon, Myeong Hee;Pyo, Heesoo
    • Analytical Science and Technology
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    • v.19 no.6
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    • pp.519-528
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    • 2006
  • An analytical method for the determination of thyroid hormones in urine samples has been studied by using solid-phase extraction and high-performance liquid chromatography/diode array detector/electro-spray mass spectrometry. Seven thyroid hormones were successfully separated by gradient elution on the reverse phase Hypersil ODS column (4.6 mm I.D., 100 mm length, particle size $5{\mu}m$) with ammonium formate buffer and acetonitrile, and UV spectra and mass fragment could be confirmed. The extraction recoveries of thyroid hormones in the urine samples (pH 3) were in the range of 89.0-113.1% with solid-phase extraction by C18, followed by elution with 4 ml of methanol/ammonium hydroxide (9 : 1). The calibration curves showed good linearity with the correlation coefficients ($r^2$) varying from 0.992 to 0.998 and the detection limits of all analytes were obtained in the range of 2-4 ng/ml (3.8-13.0 pmol/ml).

Structural determination of triterpenic acids in Prunellae Spica by fast atom bombardment tandem mass spectrometry (하고초의 생리활성 성분 Triterpenic Acids의 FAB-MS를 이용한 구조 규명)

  • Ahn, Young Min;Lee, Kang Ro;Hong, Jongki
    • Analytical Science and Technology
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    • v.21 no.4
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    • pp.245-258
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    • 2008
  • Five triterpenic acids as marker compounds were extracted and isolated from Prunellae Spica by column chromatography and reversed-phase high-performance liquid chromatography (HPLC), and their purity was determinated by HPLC (purity ${\geq}90%$). Molecular weight and elemental compositions of the five marker compounds were determined by fast atom bombardment high-resolution mass spectrometry (FAB-HRMS). The structural determination of the five marker compounds was carried out fast atom bombardment collision-induced dissociation tandem mass spectrometry (FAB-CID-MS/MS). The collision-induced dissociation (CID) of protonated molecules $[M+H]^+$ and deprotonated molecules $[M-H]^-$ produced diverse product ions due mainly to retro Diels-Alder reaction (RDA), dehydration and decarboxylation. Moreover, the CID-MS/MS spectra of the $[M-H]^-$ ions were observed charge-remote fragmentation (CRF) patterns. On the basis of interpretation of CID-MS/MS spectra, structural elucidation of triterpenic acids isolated from Prunellae Spica was clearly performed.

Polyphenolic Profile of Fermented Houttuynia cordata Thunb. and Overall Contribution to Antioxidant and Lipolytic Activities

  • Lee, Soo Jung;Hu, Wensi;Lee, Eun Jung;Choi, Jin Young;Koo, Ok Kyung
    • Food Engineering Progress
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    • v.22 no.4
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    • pp.295-303
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    • 2018
  • Polyphenol profiles, physicochemical properties, antioxidant activities, and inhibitory effect of adipocyte differentiation of Houttuynia cordata fermented with Lactobacillus brevis B84 were evaluated. Six polyphenols were characterized for this plant by using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), and the results were compared with total phenolic content by a spectrophotometric method. The total amount of the identified polyphenols was lower than that determined by the spectrophotometric method. However, the fermentation process influenced polyphenol composition such as content of vanillic acid and caffeic acid. The phytochemical profiles were evaluated by high-performance liquid chromatography with UV and electrospray ionization mass spectrometry detection ($HPLC-DAD-ESI-MS^n$). Total sugar and reducing sugar contents decreased after fermentation. Antioxidant activities such as DPPH, ABTS, and superoxide anion radical scavenging and reducing power were evaluated to compare the beneficial effect after fermentation. Fermented H. cordata increased the lipolytic effect in 3T3-L1 adipocytes. Overall, the results indicate that the fermentation of H. cordata with L. brevis B84 produces changes of phenolic compounds, antioxidant activity, and lipolytic effect.