Papers by Wojciech Filipiak
Anticancer research, 2009
AIM The aim of this work was to confirm the existence of volatile organic compounds (VOCs) specif... more AIM The aim of this work was to confirm the existence of volatile organic compounds (VOCs) specifically released by lung cancer cells. MATERIALS AND METHODS NCI-H2087 cells were trypsinized and 100 x 10(6) cells were incubated in a sealed fermenter overnight. Samples from the headspace of the culture vessel were collected with simultaneous preconcentration by adsorption on solid sorbents and subsequently thermodesorbed for analysis by gas chromatography mass spectrometry (GC-MS). RESULTS The results showed a significant increase in the concentration of 2-ethyl-1-hexanol and 2-methylpentane in the headspace as compared with medium controls. 2-Methylpentane is also found in exhaled breath of lung cancer patients in contrast to that from healthy volunteers. Statistically significantly lower abundances of acetaldehyde, 2-methylpropanal, 3-methylbutanal, 2-methylbutanal and butyl acetate were found. CONCLUSION Our findings demonstrate that certain compounds can be cancer cell derived and...
Monatshefte fĂ¼r Chemie - Chemical Monthly
This work is focused on the detection of butter adulteration by sunflower and rapeseed oils using... more This work is focused on the detection of butter adulteration by sunflower and rapeseed oils using low pressure gas chromatography mass spectrometry (LPGC-MS). The method is based on simple dissolution of triglycerides from butter samples in chloroform and their direct analysis with LPGC-MS. The method allows the detection of characteristic triglycerides as butter adulteration markers and their quantification in different samples, with the possibility to quantify plant oil addition to butter at 0.45% level (using m/z = 600.4 for rapeseed oil) and 0.15% for sunflower oil (using m/z = 598.4). Ten different commercial butters were tested for the presence of sunflower and rapeseed oil. Interestingly, the addition of rapeseed oil up to 1.2% was recorded in one butter brand.Graphical abstract
Analytical Methods
Continuous research on metabolomics is of utmost importance in the field of anti-doping control, ... more Continuous research on metabolomics is of utmost importance in the field of anti-doping control, including updating the selection of the most appropriate markers of prohibited substances, testing specimens and analytical...
Journal of Pharmaceutical and Biomedical Analysis
Gamma-oryzanol (GO) has gained special attention in the equine sports industry in recent years du... more Gamma-oryzanol (GO) has gained special attention in the equine sports industry in recent years due to its touted properties, including the fact that it may cause anabolic effects on muscle growth and reduce fatigue. Many manufactures offer supplements containing GO as a naturally occurring anabolic substance; however, some producers do not declare its presence in product compositions. Taking into consideration the touted properties of GO, its ambiguous effectiveness and the open character of the Prohibited Substances List established by the FĂ©dĂ©ration Equestre Internationale, there is an urgent need to elaborate procedures for the estimation of horse exposure to GO during supplementation, as well as during routine analysis of supplements. This work describes the development and validation of the method for determination of the four main GO components, i.e., cycloartenyl ferulate, 24-methylenecycloartanyl ferulate, campesteryl ferulate and β-sitosteryl ferulate, in equestrian supplements based on LC-MS/MS after a simple ultrasound-assisted extraction (Eco-Scale score value of 76). The analytical performance achieved satisfactory results in terms of linearity (R2 > 0.9910), sensitivity (LODs ranged from 0.4 to 1.9 ng/mL), intra- and interday accuracy (from 90.4-115.8%), precision (CV < 9.6%) and recovery (from 87.6-108.6%) for all of the investigated compounds. The method was successfully applied to the analysis of thirty equestrian supplements.
TrAC Trends in Analytical Chemistry
Abstract Growing threats in modern medicine, e.g., antibiotic resistance, along with urgent need ... more Abstract Growing threats in modern medicine, e.g., antibiotic resistance, along with urgent need for rapid diagnostic techniques and introduction of new drugs, induced intensive clinical and basic research. Model in vitro experiments with bacteria cultures and human cell lines, ex vivo experiments with tissues and in vivo animal or human study put more light into mechanism of cellular processes and biomarkers discovery. Particular aims may require unique approaches to the specific conditions. Solid Phase Microextraction proved to be a very versatile technique for collection and preparation of medically important samples. The review compiles the most recent reports applying SPME in the clinical, biotechnological and pharmaceutical studies. Current achievements but also limitations in development of novel SPME assays and their application in biomedical research and drug discovery are discussed. Existing challenges and further perspectives are outlined for studies on human metabolome and its application in clinical practice and pharmaceutical or biotechnological industry.
Journal of Breath Research
Chronic obstructive pulmonary disease (COPD) is a major cause of death worldwide. Acute exacerbat... more Chronic obstructive pulmonary disease (COPD) is a major cause of death worldwide. Acute exacerbations COPD (AECOPD), caused by infectious and non-infectious agents, contribute to an increase in mortality. The diagnostic procedure of AECOPD is mainly based on clinical features. The aim of this pilot study was to identify whether volatile organic compounds (VOCs) in breath could be used to discriminate for acute exacerbated COPD. Three patient groups were included in this controlled study: AECOPD patients (n = 14, age mean ± SD: 71.4 ± 7.46), stable COPD patients (n = 16, age mean ± SD: 66.9 ± 9.05) and healthy volunteers (n = 24, age mean ± SD: 28 ± 6.08). Breath samples were collected by optimizing a sampling strategy developed by us. These samples were then analyzed using a thermal desorption-gas chromatography-time of flight-mass spectrometer (TD-GC-ToF-MS). A total of 105 VOCs were identified in the breath samples. Relevant substances were subsequently selected by overall occurrence rate, the frequency of positive alveolar gradient (AG) (i.e. the difference in exhaled and inhaled VOCs concentration), exclusion of 'smoking related' VOCs and significant differences in AGs between the three groups. These steps dramatically reduced the number of relevant analytes and resulted in 12 key VOCs having discriminative values. The performance of patients' classification described by the Receiver Operating Characteristic (ROC) curve using all 12 substances delineates an area under the curve (AUC) of 0.97. A further reduction to four VOCs (AGs only different between AECOPD and COPD) delineates an AUC of 0.92. These results indicate that breath analysis with TD-GC-ToF-MS holds promise for an accurate and easy to perform differential diagnosis between AECOPD and COPD. In this regard, ketones were observed at the highest levels in exhaled breath of AECOPD, some of which are also related to potential bacterial pathogens. Using a set of VOCs that can discriminate for AECOPD, the calculated AUCs in ROC curve analysis show far superior results in comparison to serum AECOPD biomarkers, such as C-reactive protein. The identified VOCs should be further investigated in translational studies addressing their potential for developing highly specific nanosensors for breath gas analysis which would give clinicians a tool for non-invasive diagnosis of AECOPD at the point of care.
Journal of separation science, Jan 30, 2017
AÂ simple method for the simultaneous derivatization of carbohydrates, polyols, amines and amino a... more AÂ simple method for the simultaneous derivatization of carbohydrates, polyols, amines and amino acids using hexamethyldisilazane and N,O-bis(trimethylsilyl)trifluoroacetamide was developed. This method allows the direct derivatization of urine samples without sample pretreatment before derivatization. The method was successfully used for analysis of the selected metabolites in urine samples of healthy individuals and neonates suffering from galactosemia. The limits of detection by positive chemical ionization gas chromatography with tandem mass spectrometry analysis were in the range of 1.0 mgL-1 for mannitol to 4.7 mg/L for glucose.
The European respiratory journal, 2017
We read with great interest the editorial by AGUSTI [1] which reflected on past advances in techn... more We read with great interest the editorial by AGUSTI [1] which reflected on past advances in technology in general, in respiratory medicine more specifically, and which tried to predict potential future advances. Among the latter, the use of exhaled biomarkers for detection of lung cancer caught our attention and we want to bring the editor's and readers' attention to a rapidly advancing related field of respiratory medicine, namely the analysis of volatile biomarkers of bacterial infections in exhaled breath. Like all living cells, bacteria produce numerous volatile organic compounds (VOCs), of which some may be species-specific and thus provide a biological fingerprint of pathogen presence. Detection of such bacteria-derived metabolites in exhaled breath is completely non-invasive and can be performed repeatedly without any burden to the patient. It is increasingly recognised as an innovative and promising diagnostic technique for early detection of emerging pulmonary infections [2]. Furthermore, breath analysis has high potential to advance precision diagnosis of pathogens as it reflects individual susceptibility to disease causing agents and also to therapeutic agents. Apart from this, the potential for non-invasive "real-time" analysis of exhaled biomarkers and the application of portable, point-of-care, sensor-based devices for personalised monitoring of disease state and therapy progress is a clear advancement beyond the current state-of-the-art in clinical practice. Ultimately such methodology could lead to more timely and hence more effective antibiotic use. Translation of this approach into the clinical setting was recently achieved by us in a prospective pilot clinical study where volatile metabolites produced by Staphylococcus aureus and Candida albicans under in vitro @ERSpublications Volatile organic compounds (VOCs) for the detection of respiratory infections http://ow.ly/rdhy30aEGQt
Journal of breath research, Jan 16, 2017
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Current Medicinal Chemistry, 2016
Volatile organic compounds (VOCs) offer unique insights into ongoing biochemical processes in hea... more Volatile organic compounds (VOCs) offer unique insights into ongoing biochemical processes in healthy and diseased humans. Yet, their diagnostic use is hampered by the limited understanding of their biochemical or cellular origin and their frequently unclear link to the underlying diseases. Major advancements are expected from the analyses of human primary cells, cell lines and cultures of microorganisms. In this review, a database of 125 reliably identified VOCs previously reported for human healthy and diseased cells was assembled and their potential origin is discussed. The majority of them have also been observed in studies with other human matrices (breath, urine, saliva, feces, blood, skin emanations). Moreover, continuing improvements of qualitative and quantitative analyses, based on the recommendations of the ISO-11843 guidelines, are suggested for the necessary standardization of analytical procedures and better comparability of results. The data provided contribute to arriving at a more complete human volatilome and suggest potential volatile biomarkers for future validation. Dedication:This review is dedicated to the memory of Prof. Dr. Anton Amann, who sadly passed away on January 6, 2015. He was motivator and motor for the field of breath research.
Metabolites
Volatile organic compounds (VOCs) have been proposed in the last two decades as biomarkers for di... more Volatile organic compounds (VOCs) have been proposed in the last two decades as biomarkers for disease detection and therapeutic monitoring. Model in vitro experiments with established cell lines are fundamental to clarify whether given VOCs originate from normal human cells or pathogens, including transformed cancer cells. Due to the trace concentrations of target metabolites, adsorptive enrichment is needed before gas chromatography-mass spectrometry (GC-MS) analysis, with solid-phase microextraction (SPME) being perfectly suited for this purpose. Here, a modification of SPME, the thin-film microextraction (TFME) technique, is proposed for analysis of cellular VOCs, which utilizes a planar mesh coated with stationary phase to increase the extraction phase volume and active surface area. In this study, four different adsorbents were compared: carboxen, divinylbenzene, hydrophobic−lipophilic balanced and polydimethylsiloxane. Amongst them, HLB sheets using poly(divinylbenzene-co-N-v...
memo - Magazine of European Medical Oncology, 2010
Volatile Biomarkers, 2013
Journal of breath research, 2009
Breath gas samples from 27 patients with epilepsy (17 male and 10 female patients; mean age: 9.7 ... more Breath gas samples from 27 patients with epilepsy (17 male and 10 female patients; mean age: 9.7 years, median age: 8.2 years, SD: ±4.2 years) were screened via proton transfer reaction mass spectrometry. The patients were treated with valproic acid (VPA) therapy, and blood samples for determination of VPA concentrations were surveyed. All patients showed significantly elevated concentrations of 3-heptanone (C(7)H(14)O) in exhaled breath gas (mean: 14.7 ppb, median: 13.8 ppb SD: ±5.7 ppb). In human breath, several hundred different volatile organic compounds can be detected. In breath of patients with valproic acid monotherapy, an increased concentration of 3-heptanone was measured. The objective of this study was to investigate if serum VPA concentrations correlate with 3-heptanone concentrations in exhaled breath. In conclusion, 3-heptanone in breath gas is significantly elevated in patients treated with the valproic acid, but does not correlate significantly with the VPA concentr...
Cancer biomarkers : section A of Disease markers, 2010
Analysis of volatile organic compounds (VOCs) provides an elegant approach for cancer screening a... more Analysis of volatile organic compounds (VOCs) provides an elegant approach for cancer screening and disease monitoring, whose use is currently limited by a lack of validated cancer-derived metabolites, which may serve as biomarkers. The aim of the experiments presented here was to investigate the release and consumption of VOCs from the non small cell lung cancer cell line NCI-H1666, which was originally derived from a bronchoalveolar carcinoma.Following detachment by trypsinization suspended cells were incubated in a sealed fermenter for 21 hours. 200 ml of headspace from the cell culture were sampled, diluted with dry, highly purified air and preconcentrated by adsorption on three different solid sorbents with increasing adsorption strength. VOC-analysis was performed by thermodesorption-gas chromatography mass spectrometry (TD-GC-MS). In contrast to our previous studies experiments with NCI-H1666 cells only confirmed the consumption of several aldehydes, n-butyl acetate and the e...
Anticancer research, 2009
The aim of this work was to confirm the existence of volatile organic compounds (VOCs) specifical... more The aim of this work was to confirm the existence of volatile organic compounds (VOCs) specifically released by lung cancer cells. NCI-H2087 cells were trypsinized and 100 x 10(6) cells were incubated in a sealed fermenter overnight. Samples from the headspace of the culture vessel were collected with simultaneous preconcentration by adsorption on solid sorbents and subsequently thermodesorbed for analysis by gas chromatography mass spectrometry (GC-MS). The results showed a significant increase in the concentration of 2-ethyl-1-hexanol and 2-methylpentane in the headspace as compared with medium controls. 2-Methylpentane is also found in exhaled breath of lung cancer patients in contrast to that from healthy volunteers. Statistically significantly lower abundances of acetaldehyde, 2-methylpropanal, 3-methylbutanal, 2-methylbutanal and butyl acetate were found. Our findings demonstrate that certain compounds can be cancer cell derived and thus may be indicative of the presence of a ...
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Papers by Wojciech Filipiak