RATIONALE: Glycolipids play important roles in many physiological processes - despite their commonly low abundance. This study summarizes selected data on the (glyco)lipid composition of sperm from different fish species. METHODS: Lipid extraction of fish sperm was performed according to the procedure by Bligh and Dyer. The lipid composition of the organic extracts was analyzed by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOFMS) and electrospray ionization ion trap (ESI-IT)MS coupled to high-performance thin-layer chromatography (HPTLC). RESULTS: It was shown that sperm from carp, northern pike, rainbow trout and burbot contain high amounts of neutral and acidic glycosphingolipids as well as sulfoglycolipids. These particular lipids are presumably involved in reproduction requirements. CONCLUSIONS: Phospholipids and glycolipids in crude lipid extracts can be analyzed in parallel by MS coupled to TLC. The direct application of tandem mass spectrometry (MS/MS) helps to elucidate the glycolipid structure. Thus, compositional analysis can be performed very rapidly.

• MeSH
• chromatografie na tenké vrstvě metody   MeSH
• glykolipidy * analýza   chemie   MeSH
• hmotnostní spektrometrie s elektrosprejovou ionizací metody   MeSH
• ryby metabolismus   MeSH
• sladká voda MeSH
• spermie chemie   MeSH
• vysokoúčinná kapalinová chromatografie MeSH
• zvířata MeSH
• Check Tag
• mužské pohlaví MeSH
• zvířata MeSH
• Publikační typ
• časopisecké články MeSH
• Názvy látek
• glykolipidy * MeSH

This study reports the development and validation of a new, simple, and accurate high-performance thin-layer chromatography (HPTLC)-densitomeric method for the determination of nandrolone decanoate in a commercially available injection formulation. Chromatographic analysis was performed on glass CN modified silica gel 60F254 plates developed using n-hexane-ethyl acetate in volume ratio 42.5:7.5 as the mobile phase. Densitometric scanning was carried out at the wavelength of 245 nm. This chromatographic system gave compact spot and a symmetrical peak of nandrolone decanoate with retardation factor (RF) value at 0.57 (±0.02). The linearity of this method with the high correlation coefficient of calibration plot ranges from 0.780 to 12.500 μg/spot. The developed method is characterized by good precision (coefficient of variation CV < 2%) and high accuracy close to 100.3% (R = 99.0%). Values of limits of detection and quantification equal to 0.231 and 0.700 μg/spot, respectively, confirm the sensitivity of the developed method. The analysis of the pharmaceutical formulation of nandrolone decanoate indicates drug content of 50.5 mg/mL and 101.0% in relation to the label claim. This is in good agreement with the recommendation of the International Council for Harmonisation (ICH) guidelines as well as the pharmacopoeial requirements. The low CV value (<1%) of nandrolone decanoate content in the tested injection formulation confirms the suitability of the proposed HPTLC-densitometric method for routine control of this compound in examined pharmaceuticals.

• Klíčová slova
• HPTLC, densitometry, nandrolone decanoate, steroids,
• MeSH
• chromatografie na tenké vrstvě * metody   normy   MeSH
• denzitometrie * metody   normy   MeSH
• léčivé přípravky analýza   MeSH
• nandrolon dekanoát analýza   MeSH
• příprava léků MeSH
• reprodukovatelnost výsledků MeSH
• senzitivita a specificita MeSH
• vysokoúčinná kapalinová chromatografie * metody   normy   MeSH
• Publikační typ
• časopisecké články MeSH
• Názvy látek
• léčivé přípravky MeSH
• nandrolon dekanoát MeSH

The rise of the mosquitoes-transmitted diseases, like dengue, zika and chikungunya in Brazil in the last years has increased concerns on protection against mosquitoes bites. However, the prohibitive prices of the commercially available repellents for the majority of the Brazilian population has provoked a search for cheaper solutions, like the use of the homemade ethanolic extract of Indian clove (Syzygium aromaticum L.) as repellent, which has been reported as quite efficient by the local press. In order to verify this, we performed here the quantification of the main components of this extract through high-performance thin-layer chromatography (HPTLC)-densitometry and evaluated its efficiency as a repellent and its acetylcholinesterase (AChE) inhibition capacity. Our results have proved HPTLC-densitometry as an efficient and appropriate method for this quantification and confirmed the repellency activity, as well as its capacity of AChE inhibition.

• Klíčová slova
• Aedes aegypti, Syzygium aromaticum L, anticholinesterase, eugenol, insect repellent,
• MeSH
• acetylcholinesterasa metabolismus   MeSH
• Aedes účinky léků   MeSH
• cholinesterasové inhibitory * analýza   chemie   farmakologie   MeSH
• chování zvířat účinky léků   MeSH
• chromatografie na tenké vrstvě metody   MeSH
• denzitometrie MeSH
• dospělí MeSH
• eugenol analýza   chemie   farmakologie   MeSH
• lidé MeSH
• limita detekce MeSH
• lineární modely MeSH
• mladý dospělý MeSH
• repelenty proti hmyzu * analýza   chemie   farmakologie   MeSH
• reprodukovatelnost výsledků MeSH
• rostlinné extrakty * analýza   chemie   farmakologie   MeSH
• Syzygium chemie   MeSH
• zvířata MeSH
• Check Tag
• dospělí MeSH
• lidé MeSH
• mladý dospělý MeSH
• mužské pohlaví MeSH
• zvířata MeSH
• Publikační typ
• časopisecké články MeSH
• Názvy látek
• acetylcholinesterasa MeSH
• cholinesterasové inhibitory * MeSH
• eugenol MeSH
• repelenty proti hmyzu * MeSH
• rostlinné extrakty * MeSH

In this study, 14 commercial products (dietary supplements) containing alga Chlorella vulgaris and cyanobacteria Spirulina platensis, originated from China and Japan, were analysed. UV-vis spectrophotometric method was applied for rapid determination of chlorophylls, carotenoids and pheophytins; as degradation products of chlorophylls. High Performance Thin-Layer Chromatography (HPTLC) was used for effective separation of these compounds, and also Atomic Absorption Spectrometry for determination of heavy metals as indicator of environmental pollution. Based on the results obtained from UV-vis spectrophotometric determination of photosynthetic pigments (chlorophylls and carotenoids), it was confirmed that Chlorella vulgaris contains more of all these pigments compared to the cyanobacteria Spirulina platensis. The fastest mobility compound identified in Chlorella vulgaris and Spirulina platensis using HPTLC method was β-carotene. Spectral analysis and standard calibration curve method were used for identification and quantification of separated substances on Thin-Layer Chromatographic plate. Quantification of copper (Cu2+, at 324.7 nm) and zinc (Zn2+, at 213.9nm) was performed using Flame Atomic Absorption Spectrometry with air-acetylene flame atomization. Quantification of cadmium (Cd2+, at 228.8 nm), nickel (Ni2+, at 232.0nm) and lead (Pb2+, at 283.3nm) by Electrothermal Graphite Furnace Atomic Absorption Spectrometry; and quantification of mercury (Hg2+, at 254nm) by Cold Vapour Atomic Absorption Spectrometry.

• Klíčová slova
• Carotenoid, Chlorella vulgaris, Chlorophyll, High Performance Thin-Layer Chromatography, Pheophytin, Spirulina platensis,
• MeSH
• Chlorella vulgaris chemie   MeSH
• chlorofyl chemie   MeSH
• chromatografie na tenké vrstvě metody   MeSH
• karotenoidy chemie   MeSH
• potravní doplňky analýza   MeSH
• spektrofotometrie atomová metody   MeSH
• Spirulina chemie   MeSH
• těžké kovy chemie   MeSH
• vysokoúčinná kapalinová chromatografie metody   MeSH
• Publikační typ
• časopisecké články MeSH
• Geografické názvy
• Čína MeSH
• Japonsko MeSH
• Názvy látek
• chlorofyl MeSH
• karotenoidy MeSH
• těžké kovy MeSH

Alzheimer's disease is an age-related, neurodegenerative disorder, characterized by cognitive impairment and restrictions in activities of daily living. This disease is the most common form of dementia with complex multifactorial pathological mechanisms. Many therapeutic approaches have been proposed. Among them, inhibition of acetylcholinesterase, butyrylcholinesterase, and prolyl oligopeptidase can be beneficial targets in the treatment of Alzheimer's disease. Roots, along with aerial parts of Argemone platyceras, were extracted with ethanol and fractionated on an alumina column using light petrol, chloroform and ethanol. Subsequently, repeated preparative thin-layer chromatography led to the isolation of (+)-laudanosine, protopine, (-)-argemonine, allocryptopine, (-)-platycerine, (-)-munitagine, and (-)-norargemonine belonging to pavine, protopine and benzyltetrahydroisoquinoline structural types. Chemical structures of the isolated alkaloids were elucidated by optical rotation, spectroscopic and spectrometric analysis (NMR, MS), and comparison with literature data. (+)-Laudanosine was isolated from A. platyceras for the first time. Isolated compounds were tested for human blood acetylcholinesterase, human plasma butyrylcholinesterase and recombinant prolyl oligopeptidase inhibitory activity. The alkaloids inhibited the enzymes in a dose-dependent manner. The most active compound (-)-munitagine, a pavine alkaloid, inhibited both acetylcholinesterase and prolyl oligopeptidase with IC50 values of 62.3 ± 5.8 µM and 277.0 ± 31.3 µM, respectively.

• Klíčová slova
• Alzheimer’s disease, Argemone platyceras, acetylcholinesterase, alkaloids, butyrylcholinesterase, prolyl oligopeptidase,
• MeSH
• alkaloidy chemie   izolace a purifikace   farmakologie   MeSH
• Alzheimerova nemoc farmakoterapie   MeSH
• Argemone chemie   MeSH
• butyrylcholinesterasa účinky léků   MeSH
• cholinesterasy účinky léků   MeSH
• chromatografie na tenké vrstvě metody   MeSH
• enzymatické testy metody   MeSH
• inhibiční koncentrace 50 MeSH
• inhibitory enzymů chemie   farmakologie   MeSH
• kořeny rostlin chemie   MeSH
• lidé MeSH
• magnetická rezonanční spektroskopie metody   MeSH
• objevování léků MeSH
• prolyloligopeptidasy MeSH
• rostlinné extrakty chemie   MeSH
• serinové endopeptidasy účinky léků   MeSH
• vztah mezi dávkou a účinkem léčiva MeSH
• Check Tag
• lidé MeSH
• Publikační typ
• časopisecké články MeSH
• Názvy látek
• alkaloidy MeSH
• butyrylcholinesterasa MeSH
• cholinesterasy MeSH
• inhibitory enzymů MeSH
• PREPL protein, human MeSH Prohlížeč
• prolyloligopeptidasy MeSH
• rostlinné extrakty MeSH
• serinové endopeptidasy MeSH

Synthetic cannabinoids have gained popularity due to their easy accessibility and psychoactive effects. Furthermore, they cannot be detected in urine by routine drug monitoring. The wide range of active ingredients in analyzed matrices hinders the development of a standard analytical method for their determination. Moreover, their possible side effects are not well known which increases the danger. This review is focused on the sample preparation and the determination of synthetic cannabinoids in different matrices (serum, urine, herbal blends, oral fluid, hair) published since 2004. The review includes separation and identification techniques, such as thin layer chromatography, gas and liquid chromatography and capillary electrophoresis, mostly coupled with mass spectrometry. The review also includes results by spectral methods like infrared spectroscopy, nuclear magnetic resonance or direct-injection mass spectrometry.

• Klíčová slova
• Biological matrices, Herbal blends, Mass spectrometry, New designer drugs, Separation methods, Synthetic cannabinoids,
• MeSH
• chemické techniky analytické přístrojové vybavení   metody   MeSH
• chromatografie kapalinová přístrojové vybavení   metody   MeSH
• chromatografie na tenké vrstvě přístrojové vybavení   metody   MeSH
• elektroforéza kapilární přístrojové vybavení   metody   MeSH
• extrakce na pevné fázi přístrojové vybavení   metody   MeSH
• hmotnostní spektrometrie přístrojové vybavení   metody   MeSH
• kanabinoidy analýza   metabolismus   farmakokinetika   farmakologie   MeSH
• lidé MeSH
• nové syntetické drogy analýza   metabolismus   farmakokinetika   farmakologie   MeSH
• zvířata MeSH
• Check Tag
• lidé MeSH
• zvířata MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH
• přehledy MeSH
• Názvy látek
• kanabinoidy MeSH
• nové syntetické drogy MeSH

In this study, direct analysis in real time-mass spectrometry (DART-MS) was assessed for the analysis of various pharmaceutical formulations with intention to summarize possible applications for the routine pharmaceutical development. As DART is an ambient ionization technique, it allows direct analysis of pharmaceutical samples in solid or liquid form without complex sample preparation, which is often the most time-consuming part of the analytical method. This makes the technique suitable for many application fields, including pharmaceutical drug development. DART mass spectra of more than twenty selected tablets and other common pharmaceutical formulations, i.e. injection solutions, ointments and suppositories developed in the pharmaceutical industry during several recent years are presented. Moreover, as thin-layer chromatography (TLC) is still very popular for the monitoring of the reactions in the synthetic chemistry, several substances were analyzed directly from the TLC plates to demonstrate the simplicity of the technique. Pure substance solutions were spotted onto a TLC plate and then analyzed with DART without separation. This was the first DART-MS study of pharmaceutical dosage forms using DART-Orbitrap combination. The duration of sample analysis by the DART-MS technique lasted several seconds, allowing enough time to collect sufficient number of data points for compound identification. The experimental setup provided excellent mass accuracy and high resolution of the mass spectra which allowed unambiguous identification of the compounds of interest. Finally, DART mass spectrometry was also used for the monitoring of the selected impurity distribution in the atorvastatin tablets. These measurements demonstrated DART to be robust ionization technique, which provided easy-to-interpret mass spectra for the broad range of compounds. DART has high-throughput potential for various types of pharmaceutical analyses and therefore eliminates the time for sample cleanup and chromatographic separation.

• Klíčová slova
• DART mass spectrometry, Impurities, Pharmaceutical formulation,
• MeSH
• chromatografie na tenké vrstvě metody   MeSH
• hmotnostní spektrometrie metody   MeSH
• léčivé přípravky analýza   chemie   MeSH
• objevování léků * MeSH
• pomocné látky chemie   MeSH
• tablety chemie   MeSH
• vysokoúčinná kapalinová chromatografie metody   MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH
• Názvy látek
• léčivé přípravky MeSH
• pomocné látky MeSH
• tablety MeSH

Here we present a novel coupling of thin-layer chromatography (TLC) to diode laser thermal vaporization inductively coupled plasma mass spectrometry (DLTV ICP MS). DLTV is a new technique of aerosol generation which uses a diode laser to induce pyrolysis of a substrate. In this case the cellulose stationary phase on aluminum-backed TLC sheets overprinted with black ink to absorb laser light. The experimental arrangement relies on economic instrumentation: an 808-nm 1.2-W continuous-wave infrared diode laser attached to a syringe pump serving as the movable stage. Using a glass tubular cell, the entire length of a TLC separation channel is scanned. The 8-cm long lanes were scanned in ∼35 s. The TLC - DLTV ICP MS coupling is demonstrated on the separation of four cobalamins (hydroxo-; adenosyl-; cyano-; and methylcobalamin) with limits of detection ∼2 pg and repeatability ∼15% for each individual species.

• Klíčová slova
• Cobalamin, Diode laser thermal vaporization, Hyphenated techniques, Inductively coupled plasma mass spectrometry, Speciation, Thin-layer chromatography,
• MeSH
• chromatografie na tenké vrstvě metody   MeSH
• hmotnostní spektrometrie přístrojové vybavení   metody   MeSH
• lasery polovodičové * MeSH
• limita detekce MeSH
• potravní doplňky MeSH
• vitamin B 12 izolace a purifikace   MeSH
• vitaminy izolace a purifikace   MeSH
• volatilizace MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH
• Názvy látek
• vitamin B 12 MeSH
• vitaminy MeSH

The quantification of phospholipid classes and the determination of their molecular structures are crucial in physiological and medical studies. This paper's target analytes are cell membrane phospholipids, which play an important role in the seasonal acclimation processes of poikilothermic organisms. We introduce a set of simple and cost-effective analytical methods that enable efficient characterization and quantification of particular phospholipid classes and the identification and relative distribution of the individual phospholipid species. The analytical approach involves solid-phase extraction and high-performance thin-layer chromatography, which facilitate the separation of particular lipid classes. The obtained fractions are further transesterified to fatty acid methyl esters and subjected to gas chromatography coupled to flame ionization detection, which enables the determination of the position of double bonds. Phospholipid species separation is achieved by high-performance liquid chromatography with mass spectrometry, which gives information about the headgroup moiety and attached fatty acids. The total content of each phospholipids class is assessed by phosphorus determination by UV spectrophotometry. The simultaneous analysis of phosphorus, fatty acid residues, and phospholipid species provides detailed information about phospholipid composition. Evaluation of these coupled methods was achieved by application to an insect model, Pyrrhocoris apterus. High correlation was observed between fatty acid compositions as determined by gas chromatography and high-performance liquid chromatography analysis.

• Klíčová slova
• Insects, Mass spectrometry, Phospholipids, Thin-layer chromatography,
• MeSH
• chromatografie na tenké vrstvě ekonomika   metody   MeSH
• chromatografie plynová ekonomika   metody   MeSH
• extrakce na pevné fázi ekonomika   metody   MeSH
• fosfolipidy chemie   izolace a purifikace   metabolismus   MeSH
• Heteroptera chemie   metabolismus   MeSH
• zvířata MeSH
• Check Tag
• zvířata MeSH
• Publikační typ
• časopisecké články MeSH
• hodnotící studie MeSH
• práce podpořená grantem MeSH
• Názvy látek
• fosfolipidy MeSH

OBJECTIVES: Adenylosuccinate lyase deficiency (dADSL) is a rare inherited metabolic disorder. Biochemical diagnosis of the disease is based on the determination of enormously elevated urinary levels of succinylaminoimidazole carboxamide riboside (SAICA-riboside) and succinyladenosine (SAdo). We report a case of false negative screening for dADSL caused by deribosylation of the urinary biomarkers SAICA-riboside and SAdo. DESIGN AND METHODS: A thin-layer chromatography (TLC) method with Pauly reagent detection of SAICA-riboside was used as a screening method. High-performance liquid chromatography with diode-array detection (HPLC-DAD) and LC-MS/MS methods were used for the identification and quantitative determination of SAICA-riboside, SAdo, succinylaminoimidazole carboxamide (SAICA) and succinyladenine (SA). RESULTS: Following a negative TLC screening in a known case of dADSL, we analyzed urine using HPLC-DAD. The concentration of SAICA-riboside was 2.7mmol/mol creatinine (below the TLC detection limit), and we detected the two abnormal metabolites identified by LC-MS/MS as SAICA and SA. We showed that SAICA and SA were produced by deribosylation of SAICA-riboside and SAdo in the patient's urine. Studies performed by monitoring the production of SAICA and SA after the addition of SAICA-riboside and SAdo to the patient's urine and to urine samples from patients with urinary tract infections suggested that deribosylation is facilitated by bacterial enzymes. CONCLUSIONS: Screening methods for the diagnosis of dADSL may be falsely negative due to bacteria-mediated deribosylation of SAICA-riboside and SAdo. HPLC-DAD or LC-MS/MS analyses allowing for simultaneous detection of SAICA-riboside, SAdo and their deribosylation products SAICA and SA should be preferentially used for the diagnosis of dADSL in urine.

• Klíčová slova
• ADSL, Adenylosuccinate lyase deficiency, HPLC-DAD, LC–MS/MS, Purine metabolism, SA, SAICA, SAICA-riboside, SAdo, Succinyladenosine, Succinylaminoimidazole carboxamide riboside, Succinylpurines, TLC, adenylosuccinate lyase, adenylosuccinate lyase deficiency, dADSL, high-performance liquid chromatography with diode array detection, liquid chromatography–tandem mass spectrometry, succinyladenine, succinyladenosine, succinylaminoimidazole carboxamide, succinylaminoimidazole carboxamide riboside, thin-layer chromatography,
• MeSH
• adenosin analogy a deriváty   moč   MeSH
• adenylsukcinátlyasa nedostatek   moč   MeSH
• aminoimidazolkarboxamid analogy a deriváty   metabolismus   moč   MeSH
• autistická porucha MeSH
• bakteriální proteiny metabolismus   MeSH
• chromatografie na tenké vrstvě metody   MeSH
• Enterococcus faecalis MeSH
• enzymy metabolismus   MeSH
• falešně negativní reakce MeSH
• Klebsiella pneumoniae MeSH
• lidé MeSH
• moč mikrobiologie   MeSH
• poruchy metabolismu purinů a pyrimidinů diagnóza   moč   MeSH
• předškolní dítě MeSH
• ribonukleosidy metabolismus   moč   MeSH
• tandemová hmotnostní spektrometrie metody   MeSH
• vysokoúčinná kapalinová chromatografie MeSH
• Check Tag
• lidé MeSH
• předškolní dítě MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH
• Názvy látek
• adenosin MeSH
• adenylsukcinátlyasa MeSH
• aminoimidazolkarboxamid MeSH
• bakteriální proteiny MeSH
• enzymy MeSH
• ribonukleosidy MeSH
• succinyladenosine MeSH Prohlížeč
• succinylaminoimidazole carboxamide riboside MeSH Prohlížeč