V této práci je popsána citlivá HPLC metoda na reverzní fázi pro analýzu alkaloidů v F. densifiora, F. officinalis a F. schramii. V gradientovém uspořádání s použitím acetonitrilu a trimetylamoniového fosfátového pufru bylo dosaženo úspěšné separace 16 izochinolinových alkaloidů. Pro analýzu organických kyselin a fenolických látek byla použita metoda GC-MS.
The present paper describes a sensitive reversed phase HPLC method used for the analysis of alkaloids in F. densifiora, F. officinalis and F. schramii. Successful separation of sixteen isoquinoline alkaloids was achieved using a gradient elution of an acetonitriletrimethylammonium phosphate buffer. For the analysis of organic acids and phenolics, a GC-MS method was used.
Uveden postup při současné identifikaci a kvantifikaci a amfetaminu a metamfetaminu v lidských vlasech. Metoda zahrnuje promytí vlasů (postupně destilovaná voda teploty asi 50 'C, 0,1M kyselina chlorovodíková, destilovaná voda do neutrální reakce, metanol), usušení na vzduchu, homogenizaci rozstříháním (1 - 2 mm délky), alkalickou hydrolýzu (20 mg vlasů, 1 ml IM hydroxidu sodného, 55 °C, 120 min.), neutralizaci IM kyselinou chlorovodíkovou na pH = 7, extraktivní benzoylaci s 2,3,4,5,6-pentafluorobenzoylchloridem (0,3 ml IM hydroxidu sodného, 4 ml cyklohexanu, 30 lil cyklohexylaminu v cyklohexanu koncentrace 20 ng/μl - vnitřní standard, 50 μl vodného roztoku trietylaminhydrochloridu koncentrace 100 mg/ml - katalyzátor reakce a 10 μl derivatizačního cinidla 2,3,4,5,6-pentafluorobenzoylchloridu ředění 1:10, třepáni 5 min. v ruce a 10 min. ponechani v klidu), odstředění (5 min., 3000 ot./min.), odebrání 2 ml cyklohexanové vrstvy, její odpaření při 40 °C v dusíkové atmosféře a naředění 100 μl cyklohexanu. Derivatizovaný extrakt byl podroben analýze metodou GC-MS. Uvedený postup byl použit k segmentační analýze vlasů dvou osob dlouhodobě zneužívajících metamfetamin. Nalezené koncentrace se pohybovaly v rozmezi U,99 - 5,25 mg/kg metamfetaminu a 0,13 - 0,73 mg/kg amfetaminu.
The authors present a procedure of concurrent identification and quantification of amphetamine and metamphetamine in human hair. The method involves rinsing of the hair (distilled water 55 °C, 0.1 M hydrochloric acid, distilled water to neutral reaction , methanol) drying in air, homogenization by cutting (1-2 mm long), alkaline hydrolysis (20 mg hair, 1 ml IM sodium hydroxide, 55 "C, 120 min.), neutralization with 1 M hydrochloric acid to pH=7, extracting benzoylation with 2,3,4,5,6-pentafluorobenzoyl chloride (0.3 ml 1 M sodium hydroxide, 4 ml cyclohexane, 30 ul cyclohexylamine in cyclohexane of a concentration of 20 ng/ul - internal standard, 50 ul aqueous ^oiution of triethylamine hydrochloride concentration of 100 mg/ml - reaction catalyst and 10 ul of derivation agent 2,3,4,5,6-pentafluorobenzoyl chloride dilution 1:10 , shaking for 5 mins. by hand and leaving to stand for 10 mins.), centrifugation (5 mins., 3000 rotations/min.), collection of 2 ml cyclohexane layer, its evaporation at 40 *C in nitrogen atmosphere and dilution with 100 ul cyclohexane.The derivated exctract was subjected to analysis by the GC-MS method. The procedure was used for segmentation analysis of hair of two subjects abusing metamphetamine for prolonged periods. The revealed concentrations varied within the range of 0.99-5.25 mg/kg metamphetamine and 0.13-0.73 mgAcg amphetamine.
- MeSH
- Amphetamine analysis MeSH
- Chromatography, Gas methods instrumentation MeSH
- Humans MeSH
- Sequence Analysis methods MeSH
- Forensic Medicine MeSH
- Spectrometry, Mass, Secondary Ion MeSH
- Hair MeSH
- Check Tag
- Humans MeSH
- Publication type
- Review MeSH
Citlivý průkaz stopových koncentrací benzodiazepinových derivátů a jejich metabolitů v moči je umožněn po speciální přípravě vzorku zahrnující enzymovou hydrolýzu, speciální extrakci na směsné pevné fázi, přípravu trimethylsilylderivátů s následným využitím plynové chromatografíe V kombinaci s hmotovou spektrometrií v módu elektronové ionizace. Po optimalizaci postupu je dosahováno extrakční výtěžnosti v rozmezí 50 až 85 %. Pro řadu benzodiazepinů v silylované formě je prezentována řada retenčních dat spolu se základními údaji o příslušných hmotových spektřech, které mohou doplnit mezery v současné standardní toxikologické literatuře.
A sensitive evidence of trace concentrations of benzodiazepines and their metabolites in urine can be enabled after special sample preparation including enzymatic hydrolysis, special solid phase extraction, silylation and folowing analysis by gas chromatograhpy with mass spectrometry in electron impact mode. After optimalization of the procedure the extraction recovery values in the range 50 - 85 % are achieved. The scale of retention times with basic mass spectral data are presented for the spectrum of silylated benzodiazepines which can overlap some gaps in the standard toxicological literature up to now available.
The study deals with the GC-MS determination of acrylamide in various matrices. The proposed method involves bromination of acrylamide to 2,3-dibromopropanamide, its conversion to 2-bromopropenamide and the GC-MS determination. The method was used for the determination of acrylamide in water, gaseous products of combustion and in food such as potato chips and cookies. The measured concentrations of acrylamide ranged from 46 to 1980 g kg–1 the highest levels being found in ground coffee and tobacco smoke.
The aim of this study was to estimate the lowest concentration of pesticide residues in non-fatty food matrix at which the residues can be successfully identified by automatic spectral deconvolution software AMDIS. For GC-MS measurements fast GC with narrow capillary column was utilized. For a mixture of 18 pesticides, the identification was successful at concentration levels 4–0.4 mg kg-1 in real matrix samples (apples). With decreasing concentration, the number of identified pesticides and the quality of deconvoluted spectra decreased. The calculated limits of full-scan detection ranged from 0.20 ng for chlorpyrifos to 1.10 ng for captan. Software AMDIS with the used experimental set-up is not sufficiently sensitive for reliable identification of pesticide residues in non-fatty food matrices with low maximal residual limits (e.g. baby food 0.01 mg kg-1).
- MeSH
- Chromatography, Gas * economics methods standards instrumentation trends utilization MeSH
- Clinical Laboratory Techniques methods instrumentation trends utilization MeSH
- Gas Chromatography-Mass Spectrometry * economics methods standards instrumentation trends utilization MeSH
- Chromatography, High Pressure Liquid * economics methods standards instrumentation trends utilization MeSH
- Publication type
- Lecture MeSH
The aim of this study was GC-MS screening of drin¬king water supplies for the presence of traces of pharmaceuticals. The target analytes were naproxen, ibuprofen, diclofenac, carbamazepine and 17α-ethynylestradiol. Solid-phase extraction (SPE) was used for for their preconcetration. Derivatization of target analytes in the eluted extracts was performed using N-(tert-butyldimethylsilyl)-N-methyltrifluoroacetamide. Limits of quantification were less than 0.5 ng/L for naproxen, ibuprofen, diclofenac, carbamazepine and less than 2.0 ng/L for ??α-ethynyl¬estradiol. The presence of target pharmaceuticals in drin¬king water in the Czech Republic is very rare; their concentrations range on the ng/L level.
