• Title/Summary/Keyword: MS-10

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Bioassay-coupled LC-QTOF MS/MS to Characterize Constituents Inhibiting Nitric Oxide Production of Thuja orientalis

  • Park, Dawon;Shin, Hyeji;Byun, Youngjoo;Lee, Ki Yong
    • Natural Product Sciences
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    • v.27 no.4
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    • pp.293-299
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    • 2021
  • The ethyl acetate fractions prepared from the leaves of Thuja orientalis significantly inhibited nitric oxide (NO) production in lipopolysaccharide-stimulated BV2 microglial cells. According to bioassay-coupled LC-QTOF MS/MS, the components near 22 and 25 mins in the mass chromatogram highly inhibited NO production and were expected to be labdane diterpenes, and the active components were characterized via further isolation. The results of the NO production inhibitory assay of the isolated compounds correlated well with the results of bioassay-coupled LC-QTOF MS/MS. Among the identified constituents, NO production inhibitory activities of 16-hydroxy-labda-8(17),13-diene-15,19-dioic acid butenolide (2) and 15-hydroxypinusolidic acid (3) were newly reported. Taken together, these results demonstrated that LC-QTOF MS/MS coupled with NO production inhibition assay was a powerful tool for accurately predicting new anti-inflammatory constituents in the extracts from natural products. Moreover, it provided a potential basis for broadening the application of bioassay-coupled LC-QTOF MS/MS in natural product research.

Seedling Growth and Yield of Rice as Applying Slow Release Nitrogen Fertilizers Mixed with Seed Bed Soil in Seedling Box

  • Lee, Suk-Soon;Lee, Dong-Wook
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.46 no.4
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    • pp.289-295
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    • 2001
  • Experiments were conducted to find out the optimum level of slow release N fertilizers when total amounts of nitrogen required throughout the growing season in paddy were applied in the soil of seedling box. To evaluate the emergence rate and growth of rice seedlings, five levels of Meister (MS) 10, MS S10, and latex coated urea (LCU) which are equivalent to 0, 40, 60, 80, and 100kg N h $a^{-l}$ were mixed in soil of the seedling box. Emergence rate differed depending on the fertilizers and N levels; in MS 10 plots the emergence rate was 40.8% at 40kg N h $a^{-l}$ and no seedlings were emerged at the higher levels, in MS S10 plots higher than 80% at all the N levels, and decreased with the N levels from 70.0% at 40 kg N h $a^{-l}$ to 59.5% at 100kg N h $a^{-l}$ of LCU. Seedling started to wilt at 40 kg N h $a^{-l}$ of MS 10 and 80 and 100 kg N h $a^{-l}$ N of LCU on the 8th day after sowing, while seedling growth was normal at all the levels of MS S10. Field performance of rice was evaluated at the 0, 30, 60, 90, 120kg N h $a^{-l}$ of MS S10 applied in the soil of seedling box and N was not applied in paddy. Grain yield at 90 and 120kg N h $a^{-l}$ of MS S10 was similar to conventional urea split application (120 kg N h $a^{-l}$), but significantly higher compared to 30 and 60kg N h $a^{-l}$ of MS S10. Fertilizer N recovery decreased with N levels and the N recovery at 90 kg N h $a^{-l}$ of MS S10 and conventional urea split application were 62.2 % and 44.2%, respectively, with similar grain yield. The optimum level of MS S10 to be applied in seedling box seems to be about 90 kg N h $a^{-l}$ considering grain yield, price of fertilizer, labor applying fertilizer, and fertilizer N recovery.d fertilizer N recovery.

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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.

Determination of Total Aflatoxins in Foods by Parallelism of ELISA and LC/MS/MS (ELISA-LC/MS/MS 병행에 의한 식품 중 aflatoxins 분석)

  • Kim, Kyeong-Yeol;Nam, Min-Ji;Nam, Bo-Ram;Ryu, Hee-Jung;Song, Jeong-Eon;Shim, Won-Bo;Lee, Soo-Hyung;Chung, Duck-Hwa
    • Journal of Environmental Health Sciences
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    • v.36 no.1
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    • pp.52-60
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    • 2010
  • High performance liquid chromatography (HPLC) and liquid chromatography mass spectrometry (LC/MS) have been widely used to quantify aflatoxins in food, but these methods are expensive, time-consuming, unsuitable for analysis of the routine screening of large sample numbers and require derivatization and high level techniques to perform. The objective of this study is to detect aflatoxins in a large number of foods by a high efficient analytical system of combined enzyme linked immunosorbent assay (ELISA) for screening and LC/MS/MS for confirmation. The samples spiked individually with aflatoxin $B_1$ (0.5 and 1.0 ng/g) and total aflatoxins (10 ng/g) were analyzed by ELISA and LC/MS/ MS, and the recoveries for ELISA and LC/MS/MS were 71.8~119.2% and 70.8~135.3%, respectively. A total of 378 samples (grains, nuts, soybean and fermented soybean foods, pepper and fermented pepper foods) were purchased from the six major cities in Korea and analyzed by ELISA-LC/MS/MS system. Twenty two (5.8%; peanut: 11, pistachio: 2, walnut: 6, almond: 1, pepper powder: 1, pepper paste: 1) out of 378 samples were screened as aflatoxin B1 positive by ELISA, but, 4 (1.1%; peanut: 2, pistachio:1, pepper powder: 1) out of the 22 samples screened were confirmed as aflatoxins positive at levels of 1.02~52.79 ng/g by LC/MS/MS. ELISA-LC/MS/MS system provides a more rapid, accurate and cost-effective method for the detection of aflatoxins in large number of samples.

Rapid Quantitative Analysis of Vancomycin in Human Plasma and Urine Using LC-MS/MS (LC - MS/MS를 이용한 혈장과 뇨중에서 Vancomycin의 빠른정량분석)

  • Kim, Hohyun;Roh, Hyeongjin;Han, Sang-Beom
    • Analytical Science and Technology
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    • v.15 no.5
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    • pp.410-416
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    • 2002
  • In this study, a new quantitative analytical method has been developed for the rapid determination of vancomycin in human plasma and urine using liquid chromatography/tandem mass spectrometry (LC - MS/MS). Chromatography was carried out on a $C_{18}$ XTerra MS column ($2.1{\times}30mm$) with a particle size of $3.5{\mu}m$. The mobile phase was 0.25% formic acid in 10% acetonitrile and the flow rate was $250{\mu}L/min$. Vancomycin and caffeine (internal standard) were detected by MS/MS using multiple reaction monitoring (MRM). Vancomycin gives a predominant doubly protonated precursor molecule ($[M+2H]^{2+}$) at m/z 725.0 and a corresponding product ion of m/z 100.0. Detection of vancomycin was good, accurate and precise, with a limit of detection of 1 nM in plasma. The calibration curves for vancomycin in human plasma was linear in a concentration range of $0.01{\mu}M$ - $100{\mu}M$ for plasma. This method has been successfully applied to determine the concentration of vancomycin in human plasma and urine from pharmacokinetic study and relative studies.

Simultaneous determination of amphetamine derivatives and norketamine in hair by GC-MS/MS (GC-MS/MS를 이용한 모발 중 암페타민 유도체 및 노르케타민 동시분석)

  • Kim, Jin Young;Shin, Soon Ho;Ko, Beom Jun;Chung, Jae Cheol;Suh, Yong Jun;In, Moon Kyo
    • Analytical Science and Technology
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    • v.22 no.3
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    • pp.210-218
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    • 2009
  • A gas chromatography-tandem mass spectrometry (GC-MS/MS) method was developed and validated for simultaneous determination of amphetamine derivatives and norketamine in human hair. Preparation of hair involves external decontamination, mechanical pulverization, incubation and extraction prior to instrumental analysis. The samples were derivatized using heptafluorobutyric anhydride, and analyzed by GC-MS/MS. The linear ranges were 0.05-20.0 ng/mg for the analytes except for 3,4-methylenedioxyamphetamine, with good coefficients of determination ($r^2$ >0.998). The intra-day and inter-day precisions were within 10.7% and 8.5%, respectively. The intra-day and inter-day accuracies were between -1.6 and 17.0% and -2.6 and 10.5%, respectively. The limits of detections for each analyte were lower than 0.007 ng/mg, while recoveries were 75.9-100.9%. When the method was applied to hair samples obtained from suspected drug abusers, the concentrations in hair samples were 0.97-19.30 ng/mg for methamphetamine and 0.14-2.56 ng/mg for amphetamine.

A 10bit 1MS/s 0.5mW SAR ADC with Double Sampling Technique (더블 샘플링 기법을 사용한 10bit 1MS/s 0.5mW 축차 비교형 아날로그-디지털 변환기)

  • Lee, Ho-Kyu;Kim, Moo-Young;Kim, Chul-Woo
    • The Transactions of The Korean Institute of Electrical Engineers
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    • v.60 no.2
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    • pp.325-329
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    • 2011
  • This paper introduces the 10b 1MS/s SAR ADC with double sampling technique to reduce the power consumption. The SAR ADC is implemented in CMOS 1P8M 65nm technology and occupies 0.11um2. The maximum sampling rate is 1MS/s. The simulated SNDR and SFDR are 55.6dB and 62.7dB at 484kHz input frequency, respectively. The implemented data converter consumes 507uW with 1.2-V supply.

Determination of streptomycin in kiwifruit samples using LC-ESI-MS/MS (LC-ESI-MS/MS를 이용한 키위 중 streptomycin 분석)

  • Do, Jung-Ah;Lee, Mi-Young;Cho, Yoon-Jae;Chang, Moon-Ik;Hong, Jin-Hwan;Oh, Jae-Ho
    • Analytical Science and Technology
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    • v.28 no.4
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    • pp.299-307
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    • 2015
  • In May 2012, a safety hazard issue arose because some kiwifruit growers in New Zealand had sprayed streptomycin to prevent kiwifruit canker. Therefore, for food safety management, analytical methods to determine streptomycin residues in kiwifruits are required. We developed an analytical method to determine streptomycin residues in kiwifruit samples using liquid chromatograph tandem mass spectrometer (LC-ESI-MS/MS). Streptomycin residues in samples were extracted using 1% formic acid in methanol, centrifugation for 10 min, and subsequent supernatant filtration. Purified samples were subjected to LC-ESI-MS/MS to confirm presence of and quantify streptomycin residues. Average streptomycin recoveries (6 replicates each sample) were in the range of 94.8%-110.6% with relative standard deviations of <10%. The linearity of the concentration range of 0.01-5.0 mg/kg using a matrix-matched calibration gave R2 = 0.9995. The limit of quantification (LOQ) was 0.01 mg/kg. Results showed that our analytical method is rapid, simple, and sensitive, with easy sample preparation.

Comparison of the Metabolic Syndrome Risk Factors, Physical Activity, and Diet Habits between the Fifties and Sixties in Postmenopausal Women (50, 60대 폐경 여성 연령별 대사증후군 위험인자와 생활습관 비교)

  • Kim, Hee-Seung;Kim, Hye-Ryoung
    • Journal of Korean Biological Nursing Science
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    • v.15 no.3
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    • pp.133-138
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    • 2013
  • Purpose: The purpose of this study was to compare the metabolic syndrome (MS) risk factors, physical activity, and diet habits, between the fifties and sixties in postmenopausal women. Methods: Two hundred and thirty subjects were recruited from the volunteers of a tertiary care hospital located in an urban city of South Korea. MS was defined by the criteria of the American Heart Association, the National Heart, Lung, and Blood Institute, and the International Diabetes Federation, and obesity was determined by waist circumference ${\geq}85cm$. Results: During fifty and sixty years of age, the prevalence of MS was 19.7% and 30.6%, respectively. The waist circumference, triglyceride, blood pressure, and fasting serum glucose levels were significantly higher in the MS group than in the non-MS group during their fifties and sixties. For participants in their sixties, the pulse pressure and fasting serum glucose levels were significantly higher in the MS group than in the non-MS group. Physical activity was significantly lower in the MS group than in the non-MS group in their sixties. Conclusion: These results show that nurses should focus on increased physical activity for patients their sixties, especially MS patients for the improvement of MS risk factors.