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Chromatography 2016
September 21-23, 2016
Volume 7, Issue 5(Suppl) J Chromatogr Sep Tech 2016
ISSN: 2157-7064 JCGST, an open access journal
conferenceseries .com
September 21-23, 2016 Amsterdam, Netherlands
World Congress on Chromatography
J Chromatogr Sep Tech 2016, 7:5(Suppl)
Gas chromatographic and gas chromatographic-mass spectrometric analysis of high-purity
monoisotopic hydrides of silicon and germanium
Valentin A Krylov and A J Sozin
N I Lobachevskii Nizhny Novgorod State University, Russia
At present time, there is a great interest to simple substances, including isotopically enriched ones, with the ultimately
low content of impurities. A suitable method for production and ultra purification of the initial substances is their use
in the form of volatile hydrides. Gas chromatography-mass spectrometry is the most promising method of analysis of high-
purity substances which make it possible to reliably detect the impurities with high sensitivity. It is for the first time that the
method of gas chromatography-mass spectrometry was used to determine the impurity composition monoisotopic silanes
28SiH4, 29 SiH 4, 30SiH4 and germanes 72GeH4, 74GeH4, 76 GeН4. Introducing of gaseous samples into gas chromatograph was carried
out by automatic two-position valve “Valco EH2C6WEZPH-CER5”, connected with the developed sampling vacuum system.
56 impurity components have been determined including the permanent gases, arsine, phosphine, the homologs of silane,
disiloxane, sulfur hexafluoride, carbon bisulfide, hydrocarbons, chloro- and fluoroorganic substances. The positive chemical
ionization method was used to identify impurities missing in the individual state and thus, not included in the library of mass
spectra. It is the first found that monoisotopic hydrides contain an increased concentration of substances that have displaced
isotopic composition. The quantitative analysis has been conducted by the method of absolute calibration. The determination
of substances missing in the individual state was based upon the dependence of analysis sensitivity on their ionization cross
section. The limits of detection for impurities are 2x10-6 – 1x10 -9 mol. %, which are by 8-20 times lower than those given in
literature.
Handling time misalignment and rank deficiency in liquid chromatography by multivariate curve
resolution: Quantitation of five biogenic amines in fish
José Licarion Pinto Segundo Neto
Laboratório de Automação e Instrumentação em Química Analítica e Quimiometria, Brazil
Biogenic amines are used for identifying spoilage in food. The most common are tryptamine, 2-phenylethylamine,
putrescine, cadaverine and histamine. Due to lack of chromophores, chemical derivatization with dansyl was employed
to analyze these amines using HPLC-DAD. However, the derivatization reaction occurs with any primary or secondary
amine, leading to co-elution of analytes and interferents with identical spectral profiles, and thus causing rank deficiency.
When the spectral profile is the same and peak misalignment is present on the chromatographic runs, it is not possible to
handle the data only with MCR-ALS, by augmenting on the time, or the spectral mode. To overcome both problems, this
paper proposes a new analytical methodology for fast quantitation of these BAs in fish with HPLC-DAD by using the icoshift
algorithm for temporal misalignment correction before MCR-ALS spectral mode augmented treatment. Limits of detection,
REP and average recoveries, ranging from 0.14 to 0.50 µg mL-1, 3.5 o 8.8% and 88.08% to 99.68%, respectively. These results
reaches quantification limits for the five BAs much lower than those established by FAO/WHO, and EFSA, all without any
pre-concentration steps. The concentrations of BAs in fish samples ranged from 7.82 to 29.41 µg g-1 , 8.68 to 25.95 µg g-1, 4.76
to 28.54 µg g-1 , 5.18 to 39.95 µg g-1 and 1.45 to 52.62 µg g-1 for TRY, PHE, PUT, CAD, and HIS, respectively. In addition, the
proposed method spends less than 4 minutes in an isocratic run, consuming less solvent in accordance with the principles of
green analytical chemistry.