scholarly journals ANALISIS, IDENTIFIKASI PRECURSOR DAN HASIL DEGRADASI SENYAWA SENJATA KIMIA MENGGUNAKAN TEKNIK GAS CHROMATOGRAPHY MASS SPECTROMETRY– ELECTRON IONISASI (GCMS-EI)

2014 ◽  
Vol 16 (1) ◽  
pp. 1-9
Author(s):  
Evita Boes
Keyword(s):  
Mass Spectrometry ◽  
Phosphonic Acid ◽  
Retention Time ◽  
Soil Samples ◽  
Gas Chromatography Mass Spectrometry ◽  
Identification System ◽  
Chemical Weapon ◽  
Base Peak ◽  
Mass Spectral ◽  
Chromatographic Mass

Telah dilakukan analisis, identifikasi precursor dan hasil degradasi senyawa senjata kimia  diethyl methylphosphonat (DEMP), methyl phosphonic acid (MPA) dalam sampel air dan  dimethyl methyl phosphonat (DMMP), ethyl phosphonic acid (EPA) dalam sampel tanah. Contoh yang dianalisa merupakan contoh senyawa tributilphosphat  (TBP)  40 ug/mL dan poliethilene glycol  56,24 ug/mL ditambahkan sebagai background dan sampel tanah kering yang berpasir. Identifikasi dilakukan dengan  metode  kromatografi gas spektrometri massa - elektron ionisani (GCMS-EI). Ekstraksi fasa organik  pada pH netral, sililasi dari fasa air yang diuapkan,  di mana triethylamine/methanol-sililasi dan  kation exchange-sililasi digunakan untuk ekstraksi senyawa - senyawa precursor dan hasil degradasi sebelum diinjeksikan ke GCMS. Dari hasil analisis diperoleh  waktu retensi  8,9 dan 10,97  menit  masing - masing untuk  diethyl methylphosphonat dan bis(trimethylsilyl) methylphosphonate dalam sampel air sedangkan dalam sampel tanah  6,62 dan 12,06 menit untuk dimethyl methylphosphonat  dan bis(trimethylsilyl) ethylphosphonate. Total Ion Chromatography (TIC) yang dihasilkan dari GCMS dievaluasi dengan menggunakan    Library Data Base NIST (National Institute of Standards and Technology), dan AMDIS (Automated Mass Spectral Deconvolution and Identification System). Spektrum yang dihasilkan memberikan nilai base peak pada m/z = 97  untuk  diethyl methylphosphonate , m/z = 225 untuk  bis(trimethylsilyl) methylphosphonate, m/z = 94 untukdimethyl methylphosphonate dan m/z = 239 untuk bis(trimethylsilyl) ethylphosphonate sedangkan  retention index (RI) yang dihitung digunakan untuk  mengonfirmasi masing-masing senyawa precursorKata kunci : precursor, degradsi senyawa senjata kimia, base peak , waktu retensi,  Total Ion KromatografiAnalysis, precursoridentification have been done and  degradation compoundsof chemical weapon diethyl methylphosphonat , methyl phosphonic acid in water matrices, dimethyl methylphosphonat and ethyl phosphonic acidin soil samples. Water used for extracting those  compounds was an example of simulation that contain tributilphosphat  (TBP)  40 ug/mL and poliethylene glycol  56,24 ug/mL which added as a background and  dry sandy soil samples. Identification was done  by using Gas Chromatographic Mass Spectrometry – Electron Ionization (GCMS-EI) method. Neutral organic extraction, evaporated water - silylation, triethylamine/methanol-silylation and cation exchanged-silylation were performed to extract the precursor’s compounds from the samples, before being analyzed by gas chromatography mass spectrometry .The result of the analysis by  Gas Chromatographic  Mass Spectrometry  method showed that the retention time (in min) was 8,9 and 10,97 for diethyl methylphosphonat and bis(trimethylsilyl) methylphosphonate in the water sample , while the retention time in soil sample was 6,62 and  12,06 for dimethyl methylphosphonat and bis(trimethylsilyl) ethylphosphonate . The result of Total Ion Chromatography (TIC) from GCMS was evaluated using NIST (National Institute of Standards and Technology) database library and AMDIS (Automated Mass Spectral Deconvolution and Identification System). The spectrum’s result gave the value of base peak, which are m/z = 97for diethyl methylphosphonat, m/z= 225 for bis(trimethylsilyl) methylphosphonate , m/z = 94 for dimethyl methylphosphonat and m/z = 239 for bis(trimethylsilyl) ethylphosphonate. On the other hand, the retention indice (RI) calculation was used to get the confirmation of each compounds of precursors. Key word : precursor, degradation of chemical weapon,  base peak, retention time, totalion chromatography.

Gas Chromatographic-Mass Spectrometric Detection and Quantitation of Lincomycin in Animal Feedingstuffs

1984 ◽  
Vol 67 (3) ◽  
pp. 582-588
Author(s):  
Cecil H McMurray ◽  
W John Blanchflower ◽  
Desmond A Rice
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Retention Time ◽  
Coefficient Of Variation ◽  
Chemical Ionization ◽  
Mass Spectrometric ◽  
Gas Chromatography Mass Spectrometry ◽  
Ionization Mode ◽  
Main Fragment ◽  
Chromatographic Mass

Abstract A substantially Improved assay was developed for lincomycin A in animal feedingstuffs. The assay allows unambiguous quantitation of at least 0.1 ppm in feed. Lincomycin B did not interfere because of differences in both retention time and mass of the main fragment ion in electron impact (EI) spectra. The assay using single ion monitoring with EI detection would not discriminate between lincomycin A and clindamycin. The presence of the latter was easily confirmed by using gas chromatography-mass spectrometry in the chemical ionization mode. The assay for lincomycin A was linear in the range 0–40 ng applied to the gas chromatographic column. The recovery was 93.4 ± 4.2% at 1 and 5 ppm and 86.2 ± 5.5% at 0.1 ppm in feed. The coefficient of variation of the assay was 4.8% at both 1 and 5 ppm, and was 6.43% at 0.1 ppm.

Characterization of drug interferences caused by coelution of substances in gas chromatography/mass spectrometry confirmation of targeted drugs in full-scan and selected-ion monitoring modes

1994 ◽  
Vol 40 (2) ◽  
pp. 216-220 ◽  
Author(s):  
A H Wu ◽  
D Ostheimer ◽  
M Cremese ◽  
E Forte ◽  
D Hill
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography Mass Spectrometry ◽  
Spectrometric Analysis ◽  
Targeted Drugs ◽  
Selected Ion Monitoring ◽  
Internal Standards ◽  
Target Drug ◽  
Full Scan ◽  
Chromatographic Mass

Abstract Interference by substances coeluting with targeted drugs is a general problem for gas chromatographic/mass spectrometric analysis of urine. To characterize these interferences, we examined human urine samples containing benzoylecgonine and fluconazole, and other drug combinations including deuterated internal standards that coelute (ISd,c) with target drugs, by selected-ion monitoring (SIM) and full-scan mass spectrometry. We show that, by SIM analysis, detecting the presence of an interferent is dependent on the specific IS used for the assay. When an ISd,c is used, the presence of another coeluting substance (interferent) suggests that the intensity of IS ions is substantially diminished, because the interferent affects both the ISd,c and target drug. When a noncoeluting IS (ISnc) is used, the interferent cannot be discerned unless it coincidently contains one or more of the ions monitored for either the target drug or ISnc. Under full-scan analysis, a coeluting interferent is directly discernable by examining the total ion gas chromatogram.

Degradation of bacteria mass spectral signals via hydrothermal processing and UV irradiation: relevance to life detection on icy moons

2021 ◽  
Author(s):  
Tara Salter ◽  
Hunter Waite ◽  
Mark Sephton
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Uv Irradiation ◽  
Gas Chromatography Mass Spectrometry ◽  
Xenon Lamp ◽  
Hydrothermal Processing ◽  
Mass Spectral ◽  
Icy Moons ◽  
Chromatography Mass Spectrometry ◽  
Life Detection

<p>The inferred subsurface oceans of the icy moons of Jupiter and Saturn, in particular Europa and Enceladus, may contain conditions suitable for life. Plumes of material have been detected from Enceladus and may also be present on Europa. These plumes could contain molecular signs of habitability that could be detected by mass spectrometers on orbiting spacecrafts, such as the upcoming Europa Clipper mission. However, these molecular markers may have degraded between their production and detection, for example by possible hydrothermalism in the subsurface ocean or by UV irradiation once carried into space by the plume. It is important to look at how the biosignatures degrade under different conditions as degradation processes need to be taken into account when analysing the data from life detection missions. We investigate how these two processes affect the mass spectral signals of terrestrial bacteria.</p> <p>Two cyanobacteria samples, <em>Spirulina</em> and <em>Chlorella</em>, were subjected to hydrothermal processing and UV irradiation. Hydrous pyrolysis was used to simulate hydrothermal degradation. Experiments were carried out for 24 or 72 hours at temperatures between 200 and 300 °C. The pyrolyzed contents were subsequently extracted and analysed with gas chromatography-mass spectrometry (GC-MS). UV irradiation was carried out in a vacuum chamber (10<sup>-2</sup> mbar), using a 300 W short arc xenon lamp at UV to near infrared wavelengths (~250 – 800 nm). After UV irradiation, samples were analysed using pyrolysis-gas chromatography-mass spectrometry (Py-GC-MS).</p> <p>Our results show that hydrothermal processing of cyanobacteria affects the compound classes in different ways. Carbohydrate and protein components from the cyanobacteria were significantly affected, with phenol and indole derivatives detected. However, some of the biological fingerprint, such as straight-chain even numbered saturated fatty acids from lipid fragments, remain even at the harshest experimental conditions used in our study. This provides confidence that these diagnostic molecules could be used as fingerprints of biological materials on icy moons.</p>

scholarly journals Analysis of electrocautery generated smoke by chromatographic-mass spectrometry

2016 ◽  
Vol 43 (2) ◽  
pp. 124-128 ◽  
Author(s):  
JEFFERSON KALIL ◽  
FRANCISCO B. T. PESSINE ◽  
CARLOS H. V. FIDELIS ◽  
FABIO H. MENEZES ◽  
PAULO CESAR RODRIGUES PALMA
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography Mass Spectrometry ◽  
Chemical Components ◽  
Qualitative And Quantitative Analysis ◽  
Porcine Tissue ◽  
Qualitative And Quantitative ◽  
Hyphenated Technique ◽  
Muscular Tissues ◽  
Chromatographic Mass ◽  
Liver Tissues

ABSTRACT Objective: to analyze the chemical components of the smoke from electrocautery from coagulating muscle and liver tissues of pigs. Methods: we collected smoke produced by electrocautery applied to porcine tissue in previously evacuated bottles, with qualitative and quantitative analysis of the compounds present through the hyphenated technique gas chromatography / mass spectrometry. Results: there was a majority of decanal aldehyde in the fumes from the subcutaneous, muscle and liver tissues. Fumes of subcutaneous and muscular tissues also showed the presence of hexanal and phenol. In the fumes of subcutaneous and liver tissues we also found toluene and limonene and, finally, nonanal smoke was present in the muscle and liver tissues. Conclusion: there is increasing evidence showing that smoke from electrocautery used in subcutaneous, muscle and liver tissue is harmful to human health. Thus, there is need to reduce exposure to it or wear masks with filters capable of retaining these particles.

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