• Title/Summary/Keyword: MS0

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Simultaneous GC/MS Analyses of Organic acids and Amino acids in Urine using TMS-TFA derivative (TMS-TFA 유도체화를 이용한 소변여지 중 유기산과 아미노산의 GC/MS 동시분석)

  • Yoon, Hye-Ran
    • Analytical Science and Technology
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    • v.19 no.1
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    • pp.107-114
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    • 2006
  • Early diagnosis and medical intervention are critical for the treatment of patients with metabolic disorders. A rapid analytical method was developed for simultaneous quantification of organic acids and amino acids in urine without labor-intensive pre-extraction procedure showing high sensitivity and specificity. A new method consisted of simple two-step trimethylsilyl (TMS)-trifluoroacetyl (TFA) derivatization using GC/MS-selective ion monitoring (SIM). Filter paper urine specimens were dried under nitrogen after being fortified with internal standard (tropate) in a mixture of distilled water and methanol. Methyl orange was added to the residue as indicator reagent. Silyl derivative of carboxylic functional group was followed by trifluoroacetyl derivative for amino functional group. N-methyl-N-(trimethylsilyl-trifluoroacetamide) and N-methyl-bistrifluoroacetamide were consecutively added and heated for 15-20 min at $65^{\circ}C-70^{\circ}C$, for TMS-TFA derivative, respectively. This reactant was analyzed by GC/MS-SIM. Linear dynamic range showed 0.001-50 mg with the detection limit of (S/N=3) 10-200 ng, and the quantification limit of 80-900 ng in urine. Correlation coefficient of regression line was 0.994-0.998. When the method was applied to the patients 'urine, it clearly differentiated the normal from the patient with metabolic disorder. The study showed that the developed method could be the method of choices in rapid and sensitive screening for organic aciduria and amino acidopathy.

Efficient Procedures for Direct Shoots Regeneration from Leaf Explants of Rehmania glutinosa Lib. (지황 잎조직 절편으로부터 신초 형성)

  • Hwang, Sung-Jin
    • Korean Journal of Medicinal Crop Science
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    • v.13 no.6
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    • pp.273-277
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    • 2005
  • Adventitious shoots were directly induced from leaf explants of R. glutinosa, an important medicinal plant. Proliferating shoot cultures were obtained by culturing leaf discs on Murashige and Skoog(MS) medium alone or combination with auxins and cytokinins. MS medium supplemented with 1 $mg/{\ell}\;BA\;and\;2\;mg/{\ell}$ IAA was the most effective, providing high shoot bud formation frequency without formation of intervening callus. The effect of leaf age on adventitious shoot formation was also investigated. The maximum shoot bud production (93.4%) was achived using 3rd leaf from apex of 6 weeks old plantlets after seed germination. Plantlet were rooted on an half-strength MS (1/2MS) medium containing 0.1 $mg/{\ell}\;IBA$. This prtocol is useful for clonal propagation and Agrobacterium-mediated transforamtion in R. glutinosa.

Microstructures and Mechanical Properties of HfN Coatings Deposited by DC, Mid-Frequency, and ICP Magnetron Sputtering

  • Sung-Yong Chun
    • Corrosion Science and Technology
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    • v.22 no.6
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    • pp.393-398
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    • 2023
  • Properties of hafnium nitride (HfN) coatings are affected by deposition conditions, most often by the sputtering technique. Appropriate use of different magnetron sputtering modes allows control of the structural development of the film, thereby enabling adjustment of its properties. This study compared properties of HfN coatings deposited by direct current magnetron sputtering (dcMS), mid-frequency direct current magnetron sputtering (mfMS), and inductively coupled plasma-assisted magnetron sputtering (ICPMS) systems. The microstructure, crystalline, and mechanical properties of these HfN coatings were investigated by field emission electron microscopy, X-ray diffraction, atomic force microscopy, and nanoindentation measurements. HfN coatings deposited using ICPMS showed smooth and highly dense microstructures, whereas those deposited by dcMS showed rough and columnar structures. Crystalline structures of HfN coatings deposited using ICPMS showed a single δ-HfN phase, whereas those deposited using dcMS and mfMS showed a mixed δ-HfN and HfN0.4 phases. Their performance were increased in the order of dcMS < mfMS < ICPMS, with ICPMS achieving a value of 47.0 GPa, surpassing previously reported results.

Estimation of $T_2{^*}$ Relaxation Times for the Glandular Tissue and Fat of Breast at 3T MRI System (3테슬러 자기공명영상기기에서 유방의 유선조직과 지방조직의 $T_2{^*}$이완시간 측정)

  • Ryu, Jung Kyu;Oh, Jang-Hoon;Kim, Hyug-Gi;Rhee, Sun Jung;Seo, Mirinae;Jahng, Geon-Ho
    • Investigative Magnetic Resonance Imaging
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    • v.18 no.1
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    • pp.1-6
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    • 2014
  • Purpose : $T_2{^*}$ relaxation time which includes susceptibility information represents unique feature of tissue. The objective of this study was to investigate $T_2{^*}$ relaxation times of the normal glandular tissue and fat of breast using a 3T MRI system. Materials and Methods: Seven-echo MR Images were acquired from 52 female subjects (age $49{\pm}12 $years; range, 25 to 75) using a three-dimensional (3D) gradient-echo sequence. Echo times were between 2.28 ms to 25.72 ms in 3.91 ms steps. Voxel-based $T_2{^*}$ relaxation times and $R_2{^*}$ relaxation rate maps were calculated by using the linear curve fitting for each subject. The 3D regions-of-interest (ROI) of the normal glandular tissue and fat were drawn on the longest echo-time image to obtain $T_2{^*}$ and $R_2{^*}$ values. Mean values of those parameters were calculated over all subjects. Results: The 3D ROI sizes were $4818{\pm}4679$ voxels and $1455{\pm}785$ voxels for the normal glandular tissue and fat, respectively. The mean $T_2{^*}$ values were $22.40{\pm}5.61ms$ and $36.36{\pm}8.77ms$ for normal glandular tissue and fat, respectively. The mean $R_2{^*}$ values were $0.0524{\pm}0.0134/ms$ and $0.0297{\pm}0.0069/ms$ for the normal glandular tissue and fat, respectively. Conclusion: $T_2{^*}$ and $R_2{^*}$ values were measured from human breast tissues. $T_2{^*}$ of the normal glandular tissue was shorter than that of fat. Measurement of $T_2{^*}$ relaxation time could be important to understand susceptibility effects in the breast cancer and the normal tissue.

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
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    • v.34 no.3
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    • pp.157-165
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    • 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.

Direct Determination of Total Arsenic and Arsenic Species by Ion Chromatography Coupled with Inductively Coupled Plasma Mass Spectrometry

  • Nam, Sang-Ho;Kim, Jae-Jin;Han, Soung-Sim
    • Bulletin of the Korean Chemical Society
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    • v.24 no.12
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    • pp.1805-1808
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    • 2003
  • The simultaneous determination of As(III), As(V), and DMA has been performed by ion chromatography (IC) coupled with inductively coupled plasma-mass spectrometry (ICP-MS). The separation of the three arsenic species was achieved by an anionic separator column (AS 7) with an isocratic elution system. The separated species were directly detected by ICP-MS as an element-selective detection method. The IC-ICP-MS technique was applied for the determination of arsenic species in a NIST SRM 1643d water sample. An As(III) only was detected in the sample. The detection limits of As(III), As(V) and DMA were 0.31, 0.45, and 2.09 ng/mL, respectively. It was also applied for the determination of arsenic species in a human urine obtained by a volunteer, and three arsenic species were identified. The determination of total As in human urines that were obtained from 25 volunteers at the different age was also carried out by ICP-MS.

Study on analytical method of residual macrolide antibiotics in livestock products by LC/MS (LC/MS를 이용한 축산물 중 잔류 마크로라이드계 항생물질 분석법 연구)

  • 황래홍;윤은선;김연주;김동언;양윤모;이정학;이병동
    • Korean Journal of Veterinary Service
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    • v.25 no.3
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    • pp.221-227
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    • 2002
  • This study was carried out to confirm analytical method of residual macrolides in livestock products by LC/MS. 1. Macrolides were analyzed by LC/MS on XTerra C$\sub$18/ column with 0.1% TFA(trifluoroacetic acid)-methanol in a gradient mode as mobile phase, and that were identified by positive chemical ionization with selective ion monitoring at 50~1000 mass range. 2. Residual macrolides were extracted from tissue with acetonitrile, and the extract is purified with a Sep-pak C$\sub$18/ cartridge, and elute macrolides with 0.1M methanolic ammonium acetate. 3. The procedure confirms the presence of each macrolide at 50$\mu\textrm{g}$/kg in spiked sample.

Dynamic Rheological Properties of Hydroxypropylated Rice Starches during the Aging Process (Aging 과정 중 하드록시프로필화 쌀전분의 동적 레올로지 특성)

  • Choi, Hye-Mi;Yoo, Byoung-Seung
    • Korean Journal of Food Science and Technology
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    • v.39 no.5
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    • pp.584-587
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    • 2007
  • The effect of molar substitution (MS, 0.030-0.118) on the dynamic rheological properties of hydroxypropylated rice starch pastes (5%, w/w) was investigated by small-deformation oscillatory measurements during aging. The magnitudes of storage (G#) and loss (G") moduli measured at $4^{\circ}C$ before aging increased with an increase in MS in the range of 0.030-0.118, while those of tan ${\delta}$ (the ratio of G"/G#) decreased. The G# values of hydroxypropylated rice starches, as a function of aging time (10 hr) at $4^{\circ}C$, increased rapidly at the initial stage, and then reached a plateau region at shorter aging times. However, for the native starch, the plateau values were not observed for G# after a long aging time. Increasing the MS resulted in a decrease in plateau values. The rate constant (K) for structure development during aging was described by first-order kinetics. The K values of hydroxypropylated rice starches at 0.086 and 0.118 MS were much lower than the K value at 0.030 MS.

Simultaneous Analysis of 17 Organophosphorous Pesticides in Blood by Automated Head Space-SPME GC/MS (HS-SPME-GC/MS에 의한 혈액중 17종 유기인계 농약의 동시분석법)

  • Rhee, Jong-Sook;Jung, Jin-Mi;Lee, Han-Sun;Yeom, Hye-Sun;Lee, Sang-Ki;Park, Yoo-Sin;Chung, Hee-Sun
    • YAKHAK HOEJI
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    • v.54 no.6
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    • pp.429-440
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    • 2010
  • HS-SPME-GC/MS was studied and optimized for the determination of 17 orgarnophosphorous pesiticides (OPPs: chlorpyrifos, chlorpyrifos-methyl, demeton-s-methyl, diazinon, dimethoate, EPN, fenitrothion, fenthion, malathion, methidathion, monocrotophos, parathion, phenthoate, phosphamidon, sulfotep, terbufos, triazophos) in blood. Optimum SPME parameters were selected: choice of SPME fiber (85 ${\mu}m$ polyacrylate), pH effect (0.5 N HCl), salt effect ($Na_2SO_4$, 0.2 g; 20%), headspace incubation temperature ($80^{\circ}C$), headspace incubation time (1 min), headspace adsorption time (30 min) and GC desorption time (2 min). These parameters were optimized using HS-SPME autosampler coupled with gas chromatography-mass spectrometry (GC-MS). Method validation was carried out in terms of linearity, limit of detection (LOD), limit of quantitation (LOQ) and recovery in blood. The assay was linear over 0.5~5.0 mg/l ($r^2$=0.955~1.000). Limit of detection (LOD) and limit of quantitation (LOQ) in blood were determined 0.03~0.3 mg/l (S/N=3) and 0.1~1.1 mg/l (S/N=10), respectively. Relative recovery with 0.5, 1 and 5 mg/l (in blood) were 90.8%, 98.5% and 94.1%, respectively. This method will be applied to the determination of the orgarnophosphorous pesticides in postmortem blood. The proposed protocol can be an attractive alternative to be used in routine toxicological analysis.

Plant Regeneration from Cambium Callus of Ailanthus altissima Swingle (가중나무의 형성층(形成層) Callus에서 식물체(植物體) 재분화(再分化))

  • Lee, Sang Goo;Park, Young Goo
    • Journal of Korean Society of Forest Science
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    • v.78 no.4
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    • pp.412-418
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    • 1989
  • The stem segments of Ailanthus altissima were cultured on the Murashige & Skoog's medium(1962) supplemented with 0.1 mg/l BAP and 1.0 mg/l 2, 4-D for callus induction and proliferation, Shoot primordia were observed as greenish regions on the surface of yellow-brown calli about 8 weeks after culture. Shoot primordia were selected and transferred to the MS media containing various combination of BAP and 2, 4-D. Among these combinations the shoot primordia cell clusters on the medium added to 0.5mg/l BAP and 0.01mg/l 2, 4-D exhibited the highest number of shoot formation. These shoots were successfully transferred on the solid MS medium with no growth regulators for the rootings.

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