• Title/Summary/Keyword: MS analysis

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Analysis of Lacquer and CNSL Using Infrared Spectrometer and Pyrolysis-GC/MS (적외선분광분석과 Py-GC/MS를 이용한 옻칠 및 캐슈칠도막 분석)

  • Choi, Jaewan;Kim, Soo-Chul
    • Journal of the Korean Wood Science and Technology
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    • v.46 no.1
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    • pp.1-9
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    • 2018
  • Nowadays, synthetic resin varnish such as cashew nut shell liquid (CNSL) is being used as well as traditional lacquer. The code of ethics states that material must be identical to the original when preserving cultural heritage. Therefore, lacquer should be used. However, problem is that even experts have difficulties differentiating lacquer and CNSL as they have similar components. Therefore, this study was carried out to identify the difference between lacquer and CNSL using IR and Py-GC/MS. As a result of IR, in lacquer, $720cm^{-1}$ peak was detected and in CNSL, $750cm^{-1}$, $720cm^{-1}$ and $700cm^{-1}$ peaks were detected. The results of Py-GC/MS detect benzene compounds and alkyl chains for both varnishes. However, hexanoic acid was detected from CNSL but not lacquer. Using these analytical methods, the differences between lacquer and CNSL can be identified on the scene. This is expected to be applied to the authentic conservation and restoration of lacquerware.

Quantification Analysis and Antioxidant Activity of Leejung-tang (LC-MS/MS를 이용한 이중탕(理中湯)의 정량분석 및 항산화 활성)

  • Seo, Chang-Seob;Kim, Ohn Soon;Kim, Yeji;Shin, Hyeun-Kyoo
    • Herbal Formula Science
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    • v.21 no.1
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    • pp.177-185
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    • 2013
  • Objectives : Leejung-tang (Lizhong-tang) has been used for treatment of gastrointestinal disorders in Korea. In this study, we performed quantification analysis of five marker components, liquiritin, ginsenoside Rb1, ginsenoside Rg1, glycyrrhizin, and 6-gingerol in Leejung-tang using a ultra performance liquid chromatography- electrospray ionization-mass spectrometer (UPLC-ESI-MS). In addition, we evaluated antioxidant activity of Leejung- tang. Methods : The column for separation of five constituents used a UPLC BEH C18 ($100{\times}2.1mm$, $1.7{\mu}m$) maintained at $45^{\circ}C$. The mobile phase consisted of two solvent systems, 0.1% (v/v) formic acid in H2O (A) and CH3CN (B) by gradient flow. The flow rate was 0.3 mL/min with detection at mass spectrometer. The antioxidative activities conduct an experiment on 2,2'-azinobis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) and 2,2-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging activities of Leejung-tang. Results : Calibration curves of five marker compounds were acquired with r2 values > 0.99. The amount of the five compounds in Leejung-tang were 0.07 - 0.84 mg/g. The concentration required for 50% reduction (RC50) against ABTS radical was 119.02 ug/mL. In addition, the scavenging against DPPH radical of Leejung-tang was 11.4%, 14.5%, 19.8%, 29.6%, and 49.2% at 25 ug/mL, $50{\mu}g/mL$, $100{\mu}g/mL$, $200{\mu}g/mL$, and $400{\mu}g/mL$, respectively. Conclusions : The established LC-MS/MS method will be helpful to improve quality control of Leejung-tang. In addition, Leejung-tang is a potential antioxidant therapeutic agent.

Analysis of Pyrolysis MS Spectra in Top-down Approach and Differentiation of Gram-type Cells (Top-down 방식의 열분해질량분석 스펙트라 분석 및 Gram-type 세균 분류)

  • Kim, Ju-Hyun
    • Journal of the Korea Institute of Military Science and Technology
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    • v.14 no.4
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    • pp.719-725
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    • 2011
  • To apply TMAH-based Py-MS to a field biological detection system for real-time classification of cell-type, reproducible patterns of the TMAH-based Py-MS spectra was known as a critical factor for classification but was seriously disturbed by quantity of cells injected into pyro-tube. This factor is an exterior variable that could not be complemented by improving the performance of the TMAH-based Py-MS instrument. One of idea to solve the knotty problem has been flashed from "Top-down proteomics for identification of intact microoganisms". That is, biomarker peaks are selected from complicate Py-MS spectra for intact microoganisms by tracing out their origins, based on Py-MS spectra for the featured components of different cell-types, in Top-down approach. This idea has been tested in classification of different Gram-type microoganisms. Through the analyses of spectra for the featured components - peptidoglycan and lipoteichoic acid for Gram-positive cells and lipopolysaccharide and lipid A for Gram-negative cells - with comparing to the spectra the corresponding Gram-type cells in the Top-down approach, biomarker peaks were selected to carry out PCA(Principal Component Analysis) in order to see classification of different Gram-types, resulting in significant improvement of their classification. Furthermore, weighting biomarker peaks on intact cell's spectra, based on the data for the featured components of the Gram-types, contributed to elevate classification performance.

Method Validation for the Simultaneous Analysis of Organophosphorous Pesticides in Blood by GC/MS (GC/MS를 이용한 혈액 중 유기인제류 농약의 동시 분석에 관한 방법의 유효화)

  • Park Mee Jung;Yang Ja Youl;Kim Ki Wook;Park Yoo Shin;Chung Hee Sun;Lee Sang Ki
    • Environmental Analysis Health and Toxicology
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    • v.20 no.4 s.51
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    • pp.297-302
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    • 2005
  • The purpose of this study was to provide the standard method for the analysis of organophosphorous pesticides such as chlorpyrifos, diazinon, malathion and parathion in blood. We performed method validation for these pesticides in blood according to EURACHEM (A focus For Analytical Chemistry in Europe) guide. For the analysis of the pesticides, we used solid-phase extraction ,column (Waters Oasis $HLB^{(R)}$. After the extraction, the supernatants were evaporated to dryness under the nitrogen stream. They were analyzed by gas chromatography/mass spectrometry (GC/MS) after reconstituting with ethanol. Terbufos was used as an internal standard. To validate this method, we performed verification procedures with the following parameters: selectivity, linearity of calibration, accuracy, precision, limit of detection and quantification. Validation data according to Eurachem guide were adequate for our purpose for the analysis of chlorpyrifos, diazinon, malathion and parathion in blood.

Determination of perchlorate in the Gum-River surface water by LC-ESI-MS/MS (금강 지표수에서 LC-ESI-MS/MS에 의한 염소산이온의 극미량 분석)

  • Lee, Young Joon;Lee, Jun Bae;Hong, Seon Haw;Kim, Hyun-Ji;Shin, Ho-Sang
    • Analytical Science and Technology
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    • v.25 no.6
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    • pp.435-440
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    • 2012
  • A liquid chromatography-electrospray ionization-tandem mass spectrometry method (LC-ESI-MS/MS) was used for determining perchlorate in the Gum-River surface water. Sample was directly injected into LC-ESI-MS/MS after the filtrations using PTFE filter paper. The coefficient of variation of perchlorate was less than 3% and the limit of quantification was 0.17 ${\mu}g/L$. Water samples were collected from thirty-five basins of Gum-River on February, April and June 2012, respectively. As a result, perchlorate was detected in the concentration range of 0.23-3.73 ${\mu}g/L$ (mean 0.20 ${\mu}g/L$) in the frequency of 15% in general surface water and in the concentration range of 0.36-25.10 ${\mu}g/L$ (mean 1.69 ${\mu}g/L$) in the frequency of 36% in surface water samples near industry area.

Identification of triacylglycerols in coix seed extract by preparative thin layer chromatography and liquid chromatography atmospheric pressure chemical ionization tandem mass spectrometry

  • Sim, Hee-Jung;Lee, Seul gi;Park, Na-Hyun;Kim, Youna;Cho, Hyun-Woo;Hong, Jongki
    • Analytical Science and Technology
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    • v.30 no.2
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    • pp.102-111
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    • 2017
  • Here we reported a methodology for identification of triacylglycerols (TAGs) and diacylglycerols (DAGs) in coix seed by preparative thin layer chromatography (prep-TLC) and non-aqueous reversed-phase liquid chromatography (NARP LC)-atmospheric pressure chemical ionization (APCI) tandem mass spectrometry (MS/MS). Lipid components were extracted from coix seed by reflux extraction using n-hexane for 3 hr. TAGs and DAGs in coix seed extract were effectively purified and isolated from matrix interferences by prep-TLC and then analyzed by LC-APCI-MS and MS/MS for identification. TAGs were effectively identified taking into consideration of their LC retention behavior, APCI-MS spectra patterns, and MS/MS spectra of $[DAG]^+$ ions. In MS/MS spectra of TAGs, diacylglycerol-like fragment $[DAG]^+$ ions were useful to identify TAGs with isobaric fragment ions. Based on an established method, 27 TAGs and 8 DAGs were identified in coix seed extract. Among them, 15 TAGs and 8 DAGs were for the first time observed in coix seed. Interestingly, some of TAGs isolated by prep-TLC were partly converted into DAGs through probably photolysis process during storing in room temperature. Thus, degradation phenomenon of TAGs should be considered in the quality evaluation and nutritional property of coix seed. LC-APCI-MS/MS combined with prep-TLC will be practical method for precise TAG and DAG analysis of other herbal plants.

Analysis of Metabolic Syndrome Risk Factors among the Menopausal Women in Her Fifties (50대 폐경 여성의 대사증후군 위험인자 분석)

  • Shim, Hye-Sun;Kim, Hee-Seung;Kim, Joo-Hyun
    • Journal of Korean Biological Nursing Science
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    • v.12 no.1
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    • pp.58-62
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    • 2010
  • Purpose: The purpose of this study was to assess the difference of metabolic syndrome (MS) risk factors according to the MS diagnosis in the age of fifties women. Methods: Forty-two subjects (non metabolic syndrome 30, metabolic syndrome 12) were recruited from the health promotion center of a tertiary care hospital in an urban city. MS was defined by third report of the national cholesterol education program (NCEP) expert panel on detection, evaluation, and treatment of high blood cholesterol in adults (Adult Treatment Panel III) (ATP III), and abdominal obesity was determined by Asia-Pacific criteria in waist circumference. Results: The prevalence of MS by definition of NCEP-ATP III and Asia-Pacific criteria in waist circumference was 28.6% in the age of fifties women. The educational level and the median HDL-cholesterol were significantly lower in the MS patient group than in the Non-MS group. The median of weight, triglyceride, and fasting glucose were significantly higher in the MS patient group than in the Non-MS group. Conclusion: These results indicate that the nursing care should be focused on weight, triglyceride, HDL-cholesterol, and fasting glucose of the MS patients in the fifties women.

Metabolic Syndrome and Life Style in China

  • Wu Pei-Ying;Song Xiao-Min;Jin Qi-Lin;Wang Xin-Qiao;Wang Ai-Rong
    • Journal of Community Nutrition
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    • v.6 no.3
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    • pp.141-145
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    • 2004
  • The purpose of this study was to explore the relationship between life style and metabolic syndrome. The cross-sectional survey was conducted in Pingliang community in Shanghai in Jan 2003. The data was collected by questionnaire, and the results were analyzed by SPSS. It was found that the prevalence of Metabolic Syndrome (MS) was $13.4\%$ in the community, and the body mass index (BMI), waist-to-hip ratio (WHR), systolic blood pressure (SBP), diastolic blood pressure (DBP), serum triglyceride (TG), total cholesterol(TC), low density lipoprotein-cholesterol (LDL-C), and fast plasma glucose (FPG) in MS group were higher than that in non-MS group. Logistic regression analysis indicated that BMI and WHR were positively correlated to the prevalence of MS, and physical activity was negatively correlated to the prevalence of MS. People with higher education levels (${\geq}10y$) had lower BMI, SBP, DBP, LDL-C and FPG. The prevalence of MS in the higher education level group was significantly lower than that of the lower education level group. These results suggested that BMI, WHR and physical activity were important factors of MS, and education background played an important role in the occurrence of MS. Therefore, it is very important to build a healthy life style for preventing and controlling the incidence and developing of MS.

LC-MS/MS analysis and anti-inflammatory effects of crude extract from Coptidis Rhizoma (황련 추출물의 LC-MS/MS 분석 및 항염증 효과)

  • Min-Jung, Kim;Ye-Jin, Yang;Kwang-Youn, Kim;Hun Hwan, Kim;Jae Dong, Son;Ju-Hye, Yang;Dong bin, Lee;Woo Hyun, Kim;Hu-Jang, Lee;Seon Been, Bak;Kwang-Il, Park
    • Herbal Formula Science
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    • v.31 no.1
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    • pp.1-10
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    • 2023
  • Objectives : The main aim of this study was to examine the LC-MS/MS used to identify phenolic compounds of CRE(Coptidis Rhizoma 70% EtOH Extract). Also, we investigated antioxidative activities and Anti-inflammatory activities. Methods : LC-MS/MS Analysis HPLC and LC-MS/MS were performed on a 1260 series HPLC system (Agilent Technologies, Inc., California, USA) and 3200 QTrap tandem mass system (Sciex LLC) operated in positive ion mode (spray voltage set at -4.5 kV). The solvent used was DW and Acetonitrile containing 0.1% formic acid, a gradient system was used at a flow rate of 0.5 mL/min for analysis, and a Prontosil C18 column (length, 250 mm; inner diameter, 4.6 mm; particle size, 5 ㎛; Phenomenex Co., Ltd., California, USA, Biochoff Chromatography) was used. The solvent conditions used in the mobile phases were 0-10 min at 10-15% B, 10-20 min at 20% B, 20-30 min at 25%, 30-40 min at 40%, 40-50 min at 70%, 50-60 min at 95%, and 60-70 min at 95%. The analysis was performed at a wavelength of 284 nm and a temperature of 35℃. The cell viability was measured using a 3-(4,5-dimethyethiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay and 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging activity. We examined the effects of CRE on the lipopolysaccharide (LPS)-induced production of nitric oxide (NO) in a RAW 264.7 cells Results : The chemical analysis CRE by Liquid chromatography-tandem mass spectrometry (LC-MS/MS) confirmed that Rosmarinic acid, Ferrulic acid, 3-O-feruloylquinic acid, and 5-O-feruloylquinic acid as phenolic components. DPPH radical scavenging activity was the inhibitory activity of CRE showed at 200 ㎍/mL a statistically significant level. MTT assay demonstrated that the CRE did not have a cytotoxic effect in RAW 264.7 and LPS-induced RAW264.7 cells. Also, CRE reduced NO production in RAW 264.7 cells stimulated with LPS. Conclusions : Based on these findings, The chemical analysis 4 major components CRE such as Rosmarinic acid, Ferrulic acid, 3-O-feruloylquinic acid, and 5-O-feruloylquinic acid. Moreover, we confirmed that CRE has effects antioxidant and anti-inflammatory. The results demonstrate that CRE can be used as an antioxidant and a powerful chemopreventive ingredient against inflammatory diseases.

Simultaneous analysis of β-lactam antibiotics in surface water (하천수중 잔류 베타-락탐계 항생제의 동시분석법)

  • Huh, Min-Jeong;Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.23 no.2
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    • pp.119-127
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    • 2010
  • An effective method for the simultaneous analysis of ${\beta}$-lactams from surface water was established. After solid-phase extraction with HLB (Hydrophilic Lipohilic Balance) cartridge at pH 2, seven ${\beta}$-lactams (amoxicillin, ampicillin, penicillin G, cefaclor, cefadroxil, cefatrizine and cephradine) were determined using LC/ESI-MS/MS. In this newly established method, correlation coefficients ($r^2$) of calibration curves for seven ${\beta}$-lactams in blank surface water appeared to be 0.9911~0.9995 in the concentration range of 0.01~1.0 ng/mL. The limits of detection (LODs) and the limits of quantificaiton (LOQs) in spiked surface water were shown to be 0.0003~0.0234 ng/mL and 0.0046~0.0778 ng/mL, respectively. The developed method is believed to serve as a rapid and reliable method for the qualitative and quantitative analysis of residual ${\beta}$-lactam antibiotics from aquatic environment.