• Title/Summary/Keyword: MS analysis

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GC-MS/Ms Analysis of Benzo(a)pyrene by Ion Trap Tandem Mass Spectrometry

  • Nam, Jae-Jak;Lee, Sang-Hak
    • Bulletin of the Korean Chemical Society
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    • v.23 no.8
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    • pp.1097-1102
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    • 2002
  • The mass spectrometry using an ion trap tandem mass spectrometer has been investigated to find optimum conditions for the analysis of benzo(a)pyrene (3,4-benzpyrene). The applicability to a real soil sample was also investigated to verify the usef ulness of the MS/MS (or collision induced dissociation, CID) analysis. The optimum CID condition was 1.5 and 0.45 for the RF excitation voltage and the q value, respectively. For comparison, CID and EI were applied to the analysis of a soil sample. CID analysis was more sensitive than EI analysis of the soil sample. The limit of detection (LOD) of benzo(a)pyrene was 3.18 ng mL-1 and 0.85 ng mL,-1 for EI and MS/MS analysis, respectively. The precision at the soil sample for EI and CID showed relative standard deviations of 6.1% and 4.1%, respectively, and the concentrations were 168 ㎍ kg-1 and 162 ㎍ kg-1 , respectively.

Educational Peptide Mapping of Protein-based Biopharmaceuticals by using LC-MS/MS (LC-MS/MS를 이용한 단백질 의약품 맵핑 교수법)

  • Kim, Junseok
    • Journal of Practical Engineering Education
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    • v.14 no.2
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    • pp.327-332
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    • 2022
  • This experiment presents a precise analysis method using a mass spectrometer in the biopharmaceutical market, where utility is expanding. Among various techniques for analyzing the protein drug, somatotropin, the peptide fragments through biochemical sample preparation was analyzed by LC-MS/MS characterization. The analysis process was performed by separation analysis using nanoUPLC and MS/MS analysis using Orbitrap. In the case of somatotropin with 21 tryptic peptides, 13 of them were consistent with theoretical predictions within an average of 1 ppm error.

Forgery Detection Mechanism with Abnormal Structure Analysis on Office Open XML based MS-Word File

  • Lee, HanSeong;Lee, Hyung-Woo
    • International journal of advanced smart convergence
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    • v.8 no.4
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    • pp.47-57
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    • 2019
  • We examine the weaknesses of the existing OOXML-based MS-Word file structure, and analyze how data concealment and forgery are performed in MS-Word digital documents. In case of forgery by including hidden information in MS-Word digital document, there is no difference in opening the file with the MS-Word Processor. However, the computer system may be malfunctioned by malware or shell code hidden in the digital document. If a malicious image file or ZIP file is hidden in the document by using the structural vulnerability of the MS-Word document, it may be infected by ransomware that encrypts the entire file on the disk even if the MS-Word file is normally executed. Therefore, it is necessary to analyze forgery and alteration of digital document through internal structure analysis of MS-Word file. In this paper, we designed and implemented a mechanism to detect this efficiently and automatic detection software, and presented a method to proactively respond to attacks such as ransomware exploiting MS-Word security vulnerabilities.

A study on the determination of lead in whole blood by ICP/MS (ICP/MS에 의한 전혈 중 납의 분석방법 연구)

  • Park, Kyung Su;Kim, Sun Tae
    • Analytical Science and Technology
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    • v.10 no.4
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    • pp.240-245
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    • 1997
  • An accurate analysis method for the determination of lead in whole blood by ICP/MS was developed. Whole blood samples were decomposed in microwave digestion system without any contamination and loss of lead. The 96 samples were analyzed by ICP/MS using mass$^{208}$ isotope of lead. Lead concentrations of human whole blood were ranged of $2.50{\sim}22.8{\mu}g/dL$. The accuracy of this analysis method was verified by analyzing of NIST SRM 955a series(lead in blood).

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Comparative analysis of glycerin in cosmetics by LC/MS and 1H NMR (LC/MS와 1H NMR을 이용한 화장품속의 글리세린 비교분석)

  • Park, Gyo-Beom;Park, Chan Jo;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.20 no.5
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    • pp.400-405
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    • 2007
  • The comparative analysis of glycerin in cosmetic samples was carried out by LC/MS and $^1H$ NMR spectrometry. For the LC/MS analysis, aqueous solution was controlled in strong basic condition with sodium hydroxide, and benzoyl chloride was added to the solution for the derivatization of glycerin. The derivative was extracted using pentane and analyzed by the LC/MS. For the $^1H$ NMR analysis, sample was directly dissolved in $D_2O$ solvent without pretreatment. The quantitative analysis of glycerin was done by $^1H$ NMR ERETIC method. The analysis results of LC/MS and $^1H$ NMR showed that the calibration curves were a good linearity with $r^2=0.9991$ in the range of 0.1 to $10{\mu}g/mL$ and $r^2=1$ in the range of 25 to $500{\mu}g/mL$, respectively.

Paralytic Shellfish Poisoning (PSP) Analysis using Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS를 이용한 마비성패류독소 분석조건 검토)

  • Song, Ki Cheol;Lee, Ka Jeong;Yu, Hong Sik;Mok, Jong Soo;Kim, Ji Hoe;Lim, Keun Sik;Lee, Mi Ae
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.46 no.2
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    • pp.154-159
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    • 2013
  • The AOAC Mouse Bioassay method (MBA) has been widely used for routine monitoring of paralytic shellfish poisoning (PSP) for more than 50 years. However, this method has low sensitivity and experiences interference from other components in the extract. Also, ethical issues have been raised against the continued use of this live-mouse assay. To establish an alternative method for PSP analysis, we attempted to develop PSP analysis conditions using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The LC-MS/MS analysis of reference material showed very reasonable accuracy, and the analysis time was just 15 min. However, the recovery rate of toxin spike samples using the LC-MS/MS analysis was 59.4-91.0%. We also attempted to remove the matrix effect using shellfish extracts, but recoveries of C1 and C2 did not improve. A comparison between the results of MBA and LC-MS/MS analysis revealed good correlations, with values of 0.8878 and 0.9211 for oyster and mussel matrices, respectively.

Quantitative Analysis of the Seven Marker Components in Asarum sieboldii using the LC-MS/MS and GC-MS (LC-MS/MS와 GC-MS를 이용한 세신 추출물 중 7종 성분의 함량분석)

  • Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • Korean Journal of Pharmacognosy
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    • v.44 no.4
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    • pp.350-361
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    • 2013
  • Asarum sieboldii has been used for treatment of fever, pain, common cold, and chronic sinusitis in Korea. In this study, we performed quantification analysis of seven major constituents including aristolochic acid I, aristolochic acid II, ${\alpha}$-asarone, ${\beta}$-asarone, elemicin, methyl eugenol, and safrole in the 70% ethanol extract of Asarum sieboldii and its solvent fractions, n-hexane, ethylacetate, n-butanol, and water ones using a ultra-performance liquid chromatography-electrospray ionization-mass spectrometer(UPLC-ESI-MS) and gas chromatography-mass spectrometer(GC-MS). Regression equations of seven components were acquired with $r^2$ values >0.99. The values of limit of detection(LOD) and quantification(LOQ) were 0.1-3.9 ng/mL and 0.3-11.7 mg/mL, respectively. The amount of the seven compounds in Asarum sieboldii were not detected -143.66 mg/g. The established LC-MS/MS and GC-MS methods will be helpful to improve quality control of Asarum sieboldii.

Development of Multi-residue Analysis of 320 Pesticides in Apple and Rice Using LC-MS/MS and GC-MS/MS (LC-MS/MS와 GC-MS/MS를 이용한 사과와 쌀 시료에서 320종 농약의 다성분 분석)

  • Kim, Jong-Hwan;Kim, Yeong-Jin;Kwon, Young-Sang;Seo, Jong-Su
    • The Korean Journal of Pesticide Science
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    • v.20 no.2
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    • pp.104-127
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    • 2016
  • A new analytical method has been developed to determine 320 pesticides in apple and rice. The extraction of pesticides was carried out based on QuEChERS sample extraction, and determination was performed using LC-MS/MS and GC-MS/MS. 320 pesticides were selected for experiments. 251 and 110 pesticides among them were analysed by LC-MS/MS and GC-MS/MS, respectively. 41 pesticides of them were analyzed by both GC-MS/MS and LC-MS/MS. Among pesticides analysed by LC, 242 pesticides (96% of total number) in apple and 237 pesticides (94% of total number) in rice showed recoveries in the range of 70~120% with RSD ${\leq}20%$. In case of pesticides analyzed by GC-MS/MS, 103 pesticides (94% of total number) in apple and 83 pesticides (76% of total number) in rice were successfully validated. These results indicated that LC-MS/MS and GC-MS/MS analysis with the QuEChERS sample preparation can be partly applied to multi-residue pesticides in agricultural products.

Sex Determination Using a Discriminant Analysis of Maxillary Sinuses and Three-Dimensional Technology

  • Jeong-Hyun Lee;Hee-Jeung Jee;Eun-Seo Park;Seok-Ho Kim;Sung-Suk Bae
    • Journal of dental hygiene science
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    • v.22 no.4
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    • pp.249-255
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    • 2022
  • Background: Sexual dimorphism is important for sex determination in the field of forensics. However, sexual dimorphism is commonly assessed using cone beam computed tomography (CBCT) rather than three-dimensional (3D) modeling software; therefore, studies using a more accurate measurement approach are necessary. This study assessed the sexual dimorphism of the MS using a 3D modeling program to obtain information that could contribute to the fields of surgery and forensics. Methods: The CBCT data of 60 patients (age, 20~29 y; 30 males and 30 females) admitted to the Department of Orthodontics at the Dankook University School of Dentistry were provided in Digital Imaging and Communications in Medicine (DICOM) format. The left MS and right MS were modeled based on the DICOM files using the Mimics (version 22; Materialise, Leuven, Belgium) 3D program and converted to stereolithography (STL) files used to measure the width, length, and height of the MS, infraorbital foramen (IOF), right MS, and left MS. The average of three repeated measurements was calculated, and a reliability test was performed to ensure data reliability (Cronbach's α=0.618). A canonical discriminant analysis was performed using a standard approach (left: Box's M=0.096; right: Box's M=0.115). Results: Males had greater values for all parameters (MS width, MS length, MS height, IOF, right MS, left MS) than females. The discriminant analysis identified six independent variables (MS width, MS height, MS length, IOF, right MS, left MS) that could identify sex. The left MS and right MS correctly identified the sex of 81.7% and 71.7% of the patients, respectively, with the left MS having higher accuracy. Conclusion: This study confirmed that, for Korean individuals, the left MS has a better ability to identify sex than the right MS. These results may contribute to sex identification in the fields of surgery and forensics.

Characteristic Effects of Dangnyo-hwan for Diabetes Control Studied Using LC-MS/MS and ICP (LC-MS/MS 및 ICP를 이용한 당뇨환의 화학적 특성 분석)

  • In, Jeong-do;Im, Dai-sig;Moon, Seung-ho;Ki, Won-ill
    • The Journal of Internal Korean Medicine
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    • v.36 no.3
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    • pp.217-227
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    • 2015
  • Objectives: The primary aim of this study was to identify bioactive compounds in Dangnyo-hwan, a Korean herbal medicine, through instrumental analysis using LC-MS/MS and ICP, and investigate its potential use in diabetes treatment. Methods: The extract of Dangnyo-hwan has 12 medicinal herbs; these were compared with 18 marker substances selected from literature survey. Results: LC-MS/MS analysis could detect 9 of the 18 bioactive compounds: citruline, catalpol, berberine, ginsenoside Rb1, ginsenoside Rg1, oleanolic acid, β-sitosterol, mangiferin, and schizandrin. While harmful heavy metals such as As, Pb, Cd, Hg, Ni, and Cu were not present in high concentrations, Zn concentration was 4.2 mg in 100 g Dangnyo-hwan. Conclusions: Instrumental analysis such as LC-MS/MS and ICP was successfully used to identify bioactive compounds in Dangnyo-hwan. Detection of 9 bioactive substances and Zn from the herb medicine is a valuable finding, and suggests that Dangnyo-hwan is a candidate medicine for diabetes. Further investigations like in vitro assay, percent GPR 119 activity, and percent human DGAT-1 inhibition are underway.