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1

Organic compounds formed in thermally treated high-protein food. Part I: Polycyclic aromatic hydrocarbons

Janoszka B., Warzecha L., Błaszczyk U., Bodzek D.

Acta Chromatographica

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2004

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No. 14

115-128

EN

This work concerns the use of analytical procedures to determine polycyclic aromatic hydrocarbons (PAH) in heat-treated meat dishes prepa-red under household cooking conditions. These compounds have not yet been analysed in food in Poland. Application of tandem solid-phase extrac-tion (SPE) with columns filled with Extrelut diatomaceous earth and C18 phase, and column chromatography on silica gel enabled selective isolation of PAH fractions from the meat sample matrix. Identification and quanti-tative analysis of the individual compounds were achieved by HPLC and GC–MS. Five PAH were identified and quantified in nine meat (beef, pork, and poultry) dishes prepared according to recipes used for cooking in Upper Silesia (roasted, fried) and in grilled dishes. The total PAH content was within the range 2.43–16.10 ng g-1 meat.

2

Organic compounds formed in thermally treated high-protein food. Part II: Azaarenes

Janoszka B., Warzecha L., Błaszczyk U., Bodzek D.

Acta Chromatographica

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2004

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No. 14

129-141

EN

An analytical scheme developed for determination of PAH and aminoazaarenes has been applied to the analysis of aza-PAH formed in thermally treated high-protein food. The clean-up procedure, which was based on tandem solid-phase extraction (SPE) on columns filled with Extrelut diatomaceous earth and with cation exchanger (propylsulphonic acid, PRS), enabled selective isolation of carcinogenic azaarenes (benzo-acridines and dibenzoacridines) from meat samples. Nine meat dishes (beef, pork, and poultry) grilled or prepared according to recipes used in the Upper Silesia region (roasted, fried) were investigated. Identification and quantitative analysis of four individual compounds – benzo(a)acridine, ben-zo(c)acridine, dibenzo(a,c)acridine and dibenzo(a,h)acridine – were achie-ved by HPLC and GC–MS. The total azaarene content of the meat ranged from 0.79 to 3.30 ng g-1 and the value calculated for daily human exposu-re to these azaarenes did not exceed 0.35 žg day-1 person-1.

3

Investigation of nicotine transformation products by densitometric TLC and GC-MS

Tyrpień K., Dobosz C., Chróściewicz A, Ciołecka M., Wielkoszyński T., Janoszka B., Bodzek D.

Acta Chromatographica

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2003

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No. 13

154-160

EN

Samples of nicotine were exposed to air and UV light and the products formed were separated by TLC on RP-18 with acetonitrile-water, 88:12 (v/v), as mobile phase. GC-MS analysis was also performed to confirm the identities of the nicotine transformation products. Cotinine, reported to be one of the main products resulting from the action of environmental agents on nicotine, was identified, as was nicotyrine. The results obtained were compared with nicotine biotransformation products identified in urine from children and pregnant women. trans-3'-Hydroxy-cotinine was identified in these samples but was absent from the products formed by exposure of nicotine to air.

4

Effect of steroid hormones on results from the determination of oxycholesterol by TLC

Janoszka B., Wielkoszyński T., Tyrpień K., Dobosz C., Bodzek D.

Acta Chromatographica

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2003

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No. 13

95-101

EN

Chromatographic systems comprising different stationary and mobile phases were investigated to determine their suitability for determination of oxysterols in plasma by TLC. It was found that if some steroid hormones are present in the sample, two systems and a variety of detection condi-tions must be used for oxysterol analysis to ensure the selectivity of the determinations.

5

Usuwanie mikrozanieczyszczeń oeganicznych wód za pomocą procesów membranowych. Metodyka kontroli zawartości ftalanów w wodach

Luks-Betlej K., Bodzek D.

Zeszyty Naukowe. Inżynieria Środowiska / Politechnika Śląska

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2002

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z. 47

121-129

PL

Diestry kwasu ftalowego należą do wszędobylskich zanieczyszczeń środowiska, których rozprzestrzenienie związane jest z masową produkcją i użytkowaniem tworzyw sztucznych, głównie PCV, gdzie stosuje się je jako plastyfikatory. Ze względu na ich szkodliwe oddziaływanie na organizmy żywe obecność tych związków powinna być kontrolowana w różnych elementach środowiska, a w szczególności w wodach pitnych. W pracy przedstawiono analityczne metody oznaczania ftalanów i dokonano wyboru metody do kontroli przebiegu ich usuwania z wody za pomocą procesów membranowych.

EN

Diesthers of Phthalate Acid belong to widespread environmental pollutants whose spreading results from plastics mass production and use, especially PCV, in which diesthers are used as plasticizers. Due to their harmful influence on organisms the presence of these compounds must be controlled in different;environmental elements particularly in drinking waters. In this work the analytical methods of phthalate determination have been presented and the extraction method has been chosen to control their removing from water by membrane processes.

6

The analysis of heterocyclic aromatic amines using high performance liquid chromatography

Warzecha L., Stróżyk M., Janoszka B., Błaszczyk U., Bodzek D.

Chemia Analityczna

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2002

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Vol. 47, No. 4

539-557

EN

The optimum conditions for reversed-phase high performance liquid chromatography analysis of five mutagenic and carcinogenic heterocyclic aromatic amines (aminoazaarenes) were described. The following aminoazaarenes were chosen for the determination: 2-amine-3,4-dimethylimidazo[4,5-fjquinoline, 2-amine-3-methylimidazo[4,5-f]quinoline, 2-amine-3,4,8-tnmethylimidazo[4,5-f]quinoxaline, 2-amine-3,8-dimethylimidazo[4,5-f]quinoxaIineand 2-amine-1-methyl-6-phenylimidazo[4,5-b]pyridine. Three analytical columns: Synchropak RP-8, Vydac C(18)-300 and TSK gel ODS 80-T(M') as well as several elution systems were tested using isocratic and gradient elution. The columns, mobile phases and elution conditions were assessed by comparing retention factor, separation factor and resolution values. It is demonstrated that the most selective separation of five aminoazaarenes tested was achieved with a TSK gel ODS 80-TM column equipped with a Supelguard Hypersil ODS precolumn and using the triethylamine—phosphate buffer (pH = 3.3) / acetonitrile as the mobile phase. The following gradient elution profile was applied: 5% acetonitrile and 95% buffer for 2 min initially, then linear increase to 25% acetonitrile within 20 min, then to 55% acetonitrile within 10 min and, finally, 55% acetonitrile for 20 min. Use of chemically bonded columns C(8) and C(18) did not yield separation of aminoazaarenes as good as in the case of TSK'gel column. For these two types of columns the best separation was achieved using a procedure involving isocratic elution with mobile phase consisting of 10% acetoni-trile in triethylamine-phosphate buffer (pH = 3.2). The selected optimum conditions of HPLC analysis by use of Vydac C(18)-300 and TSK-gel ODS 80-T(M) columns were applied for qualitative determination of aminoazaarenes fractions isolated from two meat samples: charcoal grilled chicken breast and pork fillet. In both samples the presence of five tested compounds was confirmed.

PL

Przedstawiono wyniki doboru optymalnych warunków analizy metodą RP-HPLC pięciu muta- i kancerogennych wielopierścieniowych amin aromatycznych (aminoazaarenów): 2-amino-3,4-dimetyloimidazo[4,5-fJchinoliny, 2-amino-3-metyloimidazo[4.5-f]chinoliny, 2-amino-3,4,8-trinietyloimidazo[4.5-f]chinoksaliny, 2-amino-3,8-dimetyloimidazo -[4,5-f]chinoksaliny i 2-aniino-l-metylo-6-fenyIoimiclazof4,5-b]pirydyny. Przetestowano trzy kolumny analityczne: Synchropak RP-8, Yydac C|S-300 i TSK-gel ODS 80-T(M); zbadano też elucję w warunkach izokratycznych i gradientowych. Zastosowane ukJady pomiarowe scharakteryzowano wyznaczając współczynniki retencji i rozdziału oraz rozdzielczość. Najlepszy rozdział mieszaniny pięciu wybranych aminoazaarenów uzyskano przy użyciu kolumny TSK-gel ODS 80-T(M) z przedkolumną Supelguard Hypersil ODS, stosując jako fazę ruchomą bufor fosforanowo-trietyloaminowy (pH = 3.3) i acetonitryl w gradiencie: 5%acetonitrylu i 95% buforu przez 2 min, następnie liniowy wzrost do 25% acetonitrylu w ciągu 20 min, kolejno do 55% acetonitrylu w czasie 10 min i ostatecznie 55% acetonitrylu przez 20 min. Użycie kolumn z fazą chemicznie związaną (C(8) i C(18) nie dało tak dobrych wyników rozdzieleniajak użycie kolumny TSK-gel. Dla tych dwóch kolumn najlepszy rozdział uzyskano stosując jako fazę ruchomą roztwór 10% acetonitrylu w buforze fosforanowo-trietyloaminowym (pH = 3.3) i prowadząc elucję w warunkach izokratycznych. Wyznaczone optymalne warunki analizy przy użyciu kolumn: Yydac C(18)-300 oraz TSK-gel ODS 80-T(M) zastosowano do identyfikowania frakcji aminoazaarenów wyodrębnionych z dwóch próbek mięsa tj. grilowanych piersi z kurczaka oraz grilowanej polędwicy wieprzowej. W obydwu próbkach stwierdzono obecność badanych aminoazaarenów.

7

Determination of polycyclic aromatic hydrocarbons, azaarenes, and aminoazaarenes in meat samples by solid-phase extraction (SPE) and HPLC

Warzecha L., Stróżyk M., Janoszka B., Błaszczyk U., Bodzek D.

Acta Chromatographica

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2002

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No. 12

104-121

EN

A study has been conducted to determine the optimum conditions for selective enrichment, by use of coupled solid-phase extraction (SPE) cartridges, of mutagenic and/or carcinogenic organic compounds from meat samples, before qualitative and/or quantitative analysis. Such compounds, generated during heat-processing of meat, can be polycyclic aromatic hydrocarbons (PAH), polycyclic aromatic heterocyclic nitrogen compounds (azaarenes, PANH), or heterocyclic aromatic amines (HAA). To determine the optimum conditions for the clean-up procedure three kinds of Extrelut-type diatomaceous earth columns were tested. The aminoazaarene fraction was analyzed by reversed-phase high-performance liquid chromatography (RP HPLC) on a chemically bonded C8 column and isocratic elution with 10% (v/v) acetonitrile in triethylamine-phosphate buffer (pH 3.2). Analysis of the PAH and PANH fractions was performed by RP HPLC on a C18 column with acetonitrile-water, 84:16 (v/v), as mobile phase. The identities of HPLC peaks were confirmed by GC-MS for both PAH and PANH. The clean-up procedure was used to analyze samples of roasted chicken breast meat. The aminoazaarenes 2-amino-3-methylimidazo[4,5-f]quinoline (IQ), 2-amino-3,4-dimethylimidazo[4,5-f]quinoline (MeIQ), 2-amino-3,4,8-tri-methylimidazo[4,5-f]quinoxaline (4,8-DiMeIQx), and 2-amino-1-methyl-6-phenylimidazo[4,5-b]pyridine (PhIP) were detected in such samples, at total levels from 8.6-13.9 ng g-1. Polycyclic aromatic hydrocarbons identified included benzo(a)anthracene (6.5-7.5 ng g-1) and benzo(a)pyrene (4.9-7.6 ng g-1). Among the azaarenes benzo(a)acridine was found at concentrations of 10.3-12.9 ng g-1.

8

Determination of selected oxycholesterols in human blood plasma by means of thin-layer chromatography with densitometry

Janoszka B., Tyrpień K., Wielkoszyński T., Dobosz C., Bodzek D., Bodzek P., Olejek A.

Chemia Analityczna

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2001

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Vol. 46, No. 1

11-21

EN

Selected oxycholesterols: 5-cholesten-3|3-ol-7-one, sum of 5-cholestene-3p,7p-diol and 5-choleslene-3p,7a-diol, sum of 5alpha,6alpha-epoxycholestan-3p-ol and 5p,6p-epoxycho-lestan-3p-ol were determined in human blood plasma samples by the use of TLC with densitometry. The plasma was hydrolysed with ethanol solution of KOH and then extraction of lipids with n-hexane was performed. After cleanup of organic phase on silica gel SPE cartridges, oxycholesterols fraction was eluted with 2-propanol in n-hexane. Next, the fraction, after separation by TLC, was quantificated by densitometry. For the determination of 5-cholesten-3beta-ol-7-one and sum of 5-cholestene-3p,7p-diol and -3p,7a-diol the plates coated with silica gel and acetone with chloroform (1:9,v/v) as mobile phase were used. RP-18 stationary phase and 3% 2-propanol in dichloromethane solution was used for the sum of 5beta,6beta- and 5alpha,6alpha-epoxycholestan-3p-ol determination. Quantitation was carried out after Liebermann-Burchard reaction for all oxycholesterols, except 5-choles-ten-3beta-ol-7-one, for which visualization and determination was performed under UV light (X = 239 nm). Recoveries from plasma spiked with known amount of 5-choles -ten-3beta-ol-7-one as well as sensitivity and repeatability of this method were sufficient.

PL

Opracowano procedurę densytometrycznego oznaczania wybranych oksycholesteroli: 5-cholesten-3alfa-ol-7-onu, sumy 5-cholesten-3beta7beta-diolu i 5-cholesten-3p,7a-diolu oraz sumy 5alpha,6alpha-epoxycholestan-3beta-olu i 5beta, 6beta-epoxyxholestan-3beta-olu wyizolowanych z osocza krwi i rozdzielonych techniką TLC. Lipidy ekstrahowano n-heksanem z osocza poddanego wcześniej hydrolizie alkalicznej za pomocą etanolowego roztworu KOH. Frakcje oksycholesteroli wyodrębniono z ekstraktu lipidów techniką SPE stosując kolumienki wypełnione żelem krzemionkowym oraz elucję roztworem 2-propanolu w heksanie. W celu oznaczenia 5-cholesten-3beta-ol-7-onu oraz sumy 5-cholesten-3beta,7p-dioIu i -3beta,7onu-diolu rozdziały TLC prowadzono na płytkach pokrytych żelem krzemionkowym stosując mieszaninę acetonu i chloroformu (9:1, v/v) jako fazę ruchomą. Dla oznaczenia sumy 5beta,6beta- i 5alpha,6alpha-epoxycholestan-3beta-olu rozdział prowadzono w układzie RP-18/2-propanol-dichlorometan (3:97, v/v). Pomiar densytometryczny fiuores-cencji lub reflektancji powstałych produktów reakcji z odczynnikiem Liebermanna-Burcharda był podstawą oznaczeń ilościowych wszystkich badanych oksycholesteroli, za wyjątkiem 5-cholesten-3beta-ol-7-onu, który jako związek wykazujący absorpcję w zakresie UV (Lambda = 239 nm), mógł być oznaczany bezpośrednio po rozwinięciu chromatogramu. Odzysk 5-cholesten-3beta-ol-7-onu dodanego do osocza wynosił 90% a powtarzalność oznaczeń oksycholesteroli w osoczu wynosiła 10-20%.

9

Determination of selected PAH carbonyl derivatives by TLC with densitometric detection

Bodzek D., Dobosz C., Tyrpień K.

Acta Chromatographica

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2001

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No. 11

108-117

EN

Thin layer chromatography on aluminium-backed silica gel and C18 plates, with dichloromethane and a mixture of methanol, water, and acetonitrile, respectively, as mobile phases, has been used to develop methods for separation, identification, and quantification of the polyaromatic carbonyl compounds most commonly found in environmental samples. Chromatograms were developed in a horizontal chamber and compounds were quantified by means of a Shimadzu CS-9301 densitometer. RF values and detection limits for both chromatographic systems were measured for ten polyaromatic carbonyl compounds. Selective separation was achieved by normal phase chromatography on silica gel 60F254 with dichloromethane as mobile phase. The determination limits for the compounds studied were within the range 10-40 ng per spot.

10

Utlenione pochodne cholesterolu : występowanie, rola biologiczna, metody analizy

Bodzek D., Janoszka B., Wielkoszyński T.

Wiadomości Chemiczne

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2000

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[Z] 54, 11-12

1089-1108

EN

The trends of cholesterol oxidation in living organisms and the main products of this process have been presented [1-7]. Biological activity of oxycholesterols have been characterised as well as their occurence in biological material [8-32]. A three-step analytical procedure of oxycholesterols determination has been suggested. A range and conditions for the following methods (Solid Phase Extraction, Thin Layer Chromatography, Gas Chromatography, High Performance Liquid Chromatography, Mass Spectrometry) application in oxycholesterols separation, identification and quantitative determination have been discussed [33-63]. Reagents most often used for oxycholesterol derivatization as well as reagents used for oxycholesterol visualization after the separation by TLC method have been presented. Some difficulties in analysing these compounds have been mentioned.

11

Determination of tri-, tetrachloromethanes and trichloroethane by using microextraction with GC-ECD detection

Luks-Betlej K., Bodzek D.

Chemia Analityczna

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2000

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Vol. 45, No. 1

45-51

EN

Microextraction technique in liquid phase with the use of the fibres coated with polydi-methylsiloxane phase for separation trichloromethane, tetrachloromethane and 1,1,1 -tri-chloroethane from drinking water samples coming from the Upper Silesia was applied. Quantitative analysis was performed by using Gas Chromatography with electron cap-ture detection (ECD) detector. The contents of investigated compounds did not exceed the maximum permissible concentration recommended by WHO.

PL

Technikę mikroekstracji zastosowano do wyizolowania z wód pitnych Górnego.Śląska trichlorometanu, tetrachlorometanu oraz 1,1,1-trichloroetanu. Ekstrakcję analitów z fazy ciekłej przeprowadzono przy użyciu włókien pokrytych fazą polidimetylosilo-ksanu. Analizę ilościową przeprowadzono za pomocą chromatografii gazowej z detekto-rem ECD. Zawartość badanych związków nie przekraczała dopuszczalnych stężeń zalecanych przez Światową Organizację Zdrowia.

12

HPLC determination of azaarenes in environmental organic extracts

Warzecha L., Janoszka B., Stróżyk M., Bodzek D.

Acta Chromatographica

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2000

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No. 10

132-147

EN

A procedure has been developed for analysis of azaarenes in environmental organic extracts. Normal-phase semi-preparative HPLC and classical liquid–solid column chromatography were used to separate azaarene fractions. Reversed-phase (RP) HPLC analysis of the separated fractions enabled identification of nine azaarenes including compounds containing 2–5 aromatic rings per molecule. The total amount of benzo[c]cin-noline and benzoquinolines in airborne particulate extracts from the Upper Silesia region was between 0.7 and 2.3%; the amount in sewage sludge extract was ca 1.25%.

13

Aromatyczne związki siarki w złożonych mieszaninach pochodzenia naturalnego i technicznego

Janoszka B., Bodzek D.

Karbo

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1999

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Nr 1

20-27

PL

Przedstawiono podstawowe struktury heterocyklicznych związków siarki (CHS, CHNS, CHNO) zidentyfikowane w cieczach węglowych, innych mieszaninach pochodzenia technicznego oraz r6Znych elementach środowiska przyrodniczego. W oparciu o dane literaturowe scharakteryzowano właściwości biologiczne aromatycznych związków Przedstawiono metody analizy związków siarki w mieszaninach, charakteryzując poszczególne etapy tej analizy, tj. wyodrębnienie związków siarki z materiału organicznego, chromatograficzne i chemiczne metody ich separacji od związków węglowodorowych oraz techniki stosowane do identyfikacji i pomiarów ilościowych.

EN

It was presented the basic structures of heterocyclic sulphur compounds (CHS, CHNS, CHNO) identified in coal liquids, in other mixtures of synthctic origin as well as in various elements of environment. Basing on writings data the biological properties of aromatic sulphur compounds have been charactcrised. It was presented the methods of analysis for sulphur compounds in mixtures and characterised the various steps of this analysis i.e. isolation of sulphur compounds from organic material, chromatographic and chemical methods of their separation from hydrocarbon compounds as well as techniques applied to identification and quantitative measurements.

14

Occurence and determination of aminoarenes in sewage sludges from the Upper Silesia

Janoszka B., Tyrpień K., Bodzek D.

Inżynieria i Ochrona Środowiska

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1999

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T. 2, nr 2

197-203

EN

Aminoarenes have been isolated from the chosen Upper Silesia sewage sludges. Liquid column chromatography using aluminium oxide and silicic acid as stationary phases as well as semipreparative thin-layer chromatography using aluminium oxide layer were used. The separation NH2-PAHs fraction and the identification of individual compounds were performed by TLC and HPLC using in both techniques the same chromatographic system: RP-C18 stationary phase and acetonitrile-water (9+1, v/v) as mobile phase. The investigated sewage sludges have contained three and four rings amino derivatives of polycyclic aromatic hydrocarbons. Quantitative measurements of 2-aminofluorene and 1-aminopyrcne by means of HPLC technique were performed.

PL

Z osadów ściekowych pochodzących z oczyszczalni Górnego Śląska wyodrębniano frakcję aminoarenów technikami chromatografii kolumnowej na tlenku glinu oraz kwasie krzemowym, jak również semipreparatywnej chromatografii cienkowarstwowej na tlenku glinu. Rozdział i identyfikację indywidualnych aminoarenów prowadzono z użyciem TLC oraz HPLC w tych samych warunkach chromatograficznych: RPC18 jako faza stacjonarna oraz acetonitryl-woda (9+1 v/v) jako faza ruchoma. Opierając się na powyższych metodach, stwierdzono obecność w badanych osadach ściekowych trzy- i czteropierścieniowych aminowych pochodnych wielopierścieniowych węglowodorów aromatycznych. Techniką HPLC oznaczono zawartość 2-aminofluorenu i 1-aminopirenu.

15

Application of HPTLC with densitometry to the quantitative determination of PAHs in water

Tyrpień K., Dobosz C., Bodzek D.

Chemia Analityczna

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1999

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Vol. 44, No. 6

1007-1012

EN

The aim of this work was isolation from water and the determination of PAHs, which are the most dangerous for human health. It was done by the use of solid phase extraction and planar chromatography with densitometric detection. Planar separations were performed using HPTLC impregnated with caffeine. Standards and samples were applied to the chromatographic plates by Nanomat, and then developed with dichloromethane in horizontal chamber. Limits of detection of six PAHs were evaluated as well as their quantitation by means of a densitometer was perfornled.

PL

W pracy wydzielano i oznaczano w wybranych wodach sześć wielopierścieniowych węglowodorów aromatycznych (WWA), które są najbardziej niebezpieczne dla zdrowia ludzkiego. W tym celu wykorzystano ekstrakcję do fazy stałej oraz chromatografię planarną z detekcją densytometryczną. Rozdziały techniką chromatografii planarnej przeprowadzono stosując płytki HPTLC z warstwą żelu krzemionkowego impregnowaną kofeiną. Wzorce i próbki nanoszono na płytki chromatograficzne za pomocą aplikatora i rozwijano dichlorometanem w komorze poziomej. Wyznaczono granice wykrywalności sześciu WWA oraz przeprowadzono ich analizę ilościową w wodzie.

16

Determination of aromatic sulphur compounds polluting the environment by means of chromatographic and chemical methods: studies on standard compounds

Bodzek D., Janoszka B., Luks-Betlej K.

Acta Chromatographica

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1999

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No. 9

96-112

EN

A mixture of aromatic sulphur compounds and hydrocarbons containing different numbers of aromatic rings has been separated in two ways. In the first procedure the sulphur compounds were oxidized and the oxidation products were separated by solid-phase extraction on silica gel. In the other procedure sulphur compounds were isolated by means of column chromatography on silica gel modified with PdCl2. In both procedures separation and compound identification were monitored by UV–Vis spectrophotometry, GC–MS and HPLC. The results have been compared and it has been found that both methods are suitable for analysis of aromatic sulphur compounds in environmental samples and technical mixtures.

17

Zawartość związków wapnia i magnezu w wybranych wodach i osadach ściekowych Górnego Śląska

Bodzek D., Janoszka B., Tyrpień K., Wielkoszyński T.

Ochrona Środowiska

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1998

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nr 4

18-19

EN

Magnesium and calcium ion concentrations were determined in drinking water and wastewater sludge samples coming from the industrialized Upper Silesian Region and ( for comparative purposes ) from different non- industrialized bockground areas.Mg2+ Ca2+ concentrations in water samples were measured by spectrophotometry ( Mg2+ concentration in the reaction with the Mann and Yoe agent,and Ca2+ concentration in reaction with metalphthalein). In wastewater sludge, Mg2+ and Ca2+ content was determined by AAS.The concentration of Mg2+ in the water samples was generally below the concentrations of both the ions were noticeably high,thus making the investgated sludge snitable for agricultural uses,provided that the concentration of heavy metals is within the range of permissible values.

18

Kolorymetryczne oznaczanie chloroformu w procesie jego usuwania z wody za pomocą membran

Bąkowski W., Bodzek D., Zmarzły J., Szotek A.

Inżynieria i Ochrona Środowiska

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1998

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T. 1, nr 2

153-161

PL

Kolorymetryczną metodę oznaczania haloformów opartą na ich barwnej reakcji z pirydyną (reakcja Fujiwary) adaptowano do kontroli efektywności oczyszczania wód pitnych z chloroformu za pomocą membran. Metodę sprawdzono, wykonując po trzy równoległe oznaczenia w nadawie, do której dodano znaną ilość chloroformu, oraz w permeacie. Granica oznaczalności metody wyznaczona na podstawie tych pomiarów wynosi 270 μg/dm3 wody. Stosując zaproponowaną metodę, sprawdzono trwałość pentanowych ekstraktów chloroformu z próbek wody, stwierdzając brak zmian w zawartości chloroformu w ciągu 24 godzin. Pozwala to na pobór prób wody do oznaczeń chloroformu w dowolnych miejscach bez obawy, że w czasie transportu nastąpi zmiana jego stężenia. Metodyka może znaleźć zastosowanie do kontroli stężenia trójhalometanów w wodach, w których ze względu na intensywny proces chlorowania można spodziewać się dużej zawartości tych związków (baseny kąpielowe, lecznicze i rekreacyjne).

EN

The colorimetric method of haloforms determination based on the colour pyridine reaction (Fujiwara reaction) was adapted to the control of chloroform removal from drinking waters by the use of membranes. The method was tested by carrying out three parallel determinations in inlet water containing known amounts of chloroform as well as in permeat. These determination permitted to establish the limit of detection of the method. It amounted to 270 μg/dm3 of water. Stability of pentane extracts of chloroform from water was checked by the use of the proposed method; the lack of any changes in chloroform contents within 24 hours was pointed out. It permits to collect samples of water for chloroform determinations in any places without of danger of changes of its concentration during the transport time. The method may be applied to the threehalomethanes concentration control in waters which are intensively chlorinated (swimming, therapeutic and recreation pools) and in which large contents of these compounds could be expected.

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Tlc and GC - MS determination of cholesterol in consumable fats

Bodzek D., Bąkowski W., Wielkoszyński T., Janoszka B., Jaremczuk B., Tarnawski R., Tyrpień K.

Acta Chromatographica

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1998

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No. 8

122-143

EN

Cholesterol is one of the more important compounds causing arteriosclerosis and other illnesses of the circulatory system. In this work we have developed a procedure for separating a mixture of sterols from commercial consumable fats and, as the next step, identifying the main components of the sterol mixture. The method of separation included conventional and over-pressure thin-layer chromatography and solid-phase extraction (SPE); capillary gas chromatography with mass spectrometric detection was the main method of identification. Sterols and sterol esters were separated from the fats by solid-phase extraction on Bakerbond aminopropyl or silica gel columns. Preli-minary identification of the isolated sterols was achieved by TLC in a DS-sandwich type chamber. Full identification of the isolated sterols was performed by GC-MS and quantitative estimation of the cholesterol content by capillary GC with flame ionization detection. The amount of sterols was found to be in the range 4.01-11.46 mg g-1 fat; the amount of cholesterol was 0-5.14 mg g-1 fat.