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Optimization of Data Acquisition and Sample Preparation Methods for LC-MS Urine Metabolomic Analysis

100%
Skibiński R., Komsta Ł.
Open Chemistry
|
2015
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vol. 13
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issue 1
EN
Nowadays, chromatographic methods coupled with mass spectrometry are the most commonly used tools in metabolomics studies. These methods are currently being developed and various techniques and strategies are proposed for the profiling analysis of biological samples. However, the most important thing used to maximize the number of entities in the recorded profiles is the optimization of sample preparation procedure and the data acquisition method. Therefore, ultra high performance liquid chromatography coupled with accurate quadrupoletime- of-flight (Q-TOF) mass spectrometry was used for the comparison of urine metabolomic profiles obtained by the use of various spectral data acquisition methods. The most often used method of registration of metabolomics data acquisition – TOF (MS) was compared with the fast polarity switching MS and auto MS/MS methods with the use of multivariate chemometric analysis (PCA). In all the cases both ionization mode (positive and negative) were studied and the number of the identified compounds was compared. Additionally, various urine sample preparation procedures were tested and it was found that the addition of organic solvents to the sample noticeably reduces the number of entities in the registered profiles. It was also noticed that the auto MS/MS method is the least efficient way to register metabolomic profiles.
2
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A preliminary study on the effect of mineralization parameters on determination of metals in Viscum album species

71%
Blicharska E., Komsta Ł., Kocjan R., Gumieniczek A., Robak A.
Open Chemistry
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2010
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vol. 8
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issue 2
264-268
EN
An increasing interest in determination of various macro- and microelements in medicinal plants has been observed. The majority of studies are carried out using one mineralization method without any optimization. The present study demonstrates that changes in mineralization parameters can significantly affect the recovery of the elements determined. In the study, the dried plant material was mineralized in 12 ways and iron (Fe), copper (Cu), zinc (Zn), nickel (Ni) and manganese (Mn) levels were determined. The samples were mineralized in the dry or open microwave mode as well as 10 closed microwave modes. The influence of acid amounts, irradiation power and time, addition of hydrogen peroxide and perfluoric acid was examined. All parameters were shown to be critical - good efficiency was observed with larger amounts of acid. The determined content varied significantly in the same sample and were in the ranges (ug g−1): 46–136 (Fe), 1.4–11.8 (Cu), 4.0–11.3 (Ni), 15.4–53.8 (Zn) and 9.5–67.6 (Mn). Increased irradiation resulted in the loss of copper and zinc and better recovery of nickel. The results demonstrate that such determinations should include the mineralization optimization step. [...]
3
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A TLC Study of the lipophilicity of thirty-two acetylcholinesterase inhibitors - 1,2,3,4-tetrahydroacridine and 2,3-dihydro-1H-cyclopenta[b]quinoline derivatives

61%
Szymański P., Skibiński R., Liszka M., Jargieło I., Mikiciuk-Olasik E., Komsta Ł.
Open Chemistry
|
2013
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vol. 11
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issue 6
927-934
EN
The lipophilicity of thirty-two novel acetylcholinesterase (AChE) inhibitors - 1,2,3,4-tetrahydroacridine and 2,3-dihydro-1H-cyclopenta[b]quinoline derivatives was studied by thin layer chromatography. The analyzed compounds were chromatographed on RP-18, RP-8, RP-2, CN and NH2 stationary phases with dioxane - citric buffer pH 3.0 binary mobile phases containing different proportions of dioxane. RM values for pure water were extrapolated from the linear Soczewiński-Wachtmeister equation and six compounds with known literature log P values were used as reference calibration data set for computation of experimental log P values. [...] The obtained results were compared with computationally calculated partition coefficients values (AlogPs, AClogP, AlogP, MlogP, KOWWIN, XlogP2, XlogP3) by PCA and significant differences between them were observed.
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