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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.

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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.

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The analysis of aminoazaarenes as their derivatives with GC-MS method in the heat processed meat samples

Janoszka B., Błaszczyk U., Warzecha L., Luks-Betlej K., Stróżyk M.

Chemia Analityczna

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2003

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Vol. 48, No. 4

707-721

EN

Aminoazaarenes are heterocyclic aromatic amines (HAAs), which are formed in food during the heat processing. The aim of this study was to work out a method for HAAs' derivatisation and identification with GC-MS system. The five most common mutagenic and carcinogenic aminoazaarenes have been analysed: 2-amino-3-methylimidazo-[4,5-fJquinoline (IQ), 2-amino-3,4-dimethylimidazo[4,5-f]quinoline (MelQ), 2-amino-3,8-dimethylimidazo[4,5-f]quinoxaline (MelQx), 2-amino-3,4,8-trimethylimidazo-[4,5-f]quinoxaline (4,8-DiMeIQx), 2-amino-1 -methyl-6-phenylimidazo[4,5-b]pyridine (PhIP). Three procedures for derivatisation of HAAs have been applied: iodination, condensation to N-dimethylaminomethylene derivatives and acylation to pentafluoropropyl amides. Aminoazaarene fractions isolated from the grilled meat samples and spiked with the studied five HAAs have been analysed and all the added aminoazaarenes were identified as amide and N-dimethylaminomethylene derivatives. In the unspiked grilled meat samples IQ, MelQx and DiMelQx were identified as pentafluoropropyl amides. Detection limits of aminoazaarene's derivatives determined with GC-MS were ranging from 5 ng to 50 ng per single injection. The quantitative analysis was performed using HPLC method.

PL

Aminoazaareny to heterocykliczne aromatyczne aminy, które tworzą się pod wpływem temperatury w żywności zawierającej białko. Celem badań było opracowanie metody identyfikacji aminoazaarenów metodą GC-MS poprzez ich pochodne. Analizie poddano mieszaninę wzorcową pięciu aminoazaarenów, najczęściej oznaczanych w żywności i wykazujących aktywność muta- i kancerogenną: 2-amino-3-metyloimidazo[4,5-f]chinolinę (IQ), 2-amino-3,4-dimetyloimidazo[4,5-f]chinolinę (MelQ), 2-amino-3,8-dimetyloimidazo-[4,5-fJchinoksalinę (MelQx), 2-amino-3,4,8-trimetyloimidazo[4,5-fJchinoksalinę (4,8-DiMelQx) oraz 2-amino-l-metylo-6-fenyloimidazo[4,5-b]pirydynę (PhIP). Zastosowano trzy procedury derywatyzacji aminoazaarenów: do pochodnych jodowych, kondensację do pochodnych N,N-dimetyloaminometylenowych oraz acylowanie do amidów kwasu penta-fluoropropionowego. Analizie poddano frakcje aminoazaarenów wyizolowane z próbek mięsa z dodatkiem wzorców. W próbkach tych poprzez pochodne amidowe i N-dimetylo-aminometylenowe zidentyfikowano wszystkie dodane aminoazaareny. W próbkach mięsa bez dodatku wzorców, poprzez derywatyzację do pochodnych amidowych potwierdzono obecność następujących związków: IQ, MelQx i DiMelQx. Granice detekcji aminoazaarenów oznaczanych poprzez pochodne wynosiły od 5 ng do 50 ng wzorca wprowadzonego do kolumny GC. Stężenia ich oznaczono metodą HPLC.

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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.

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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.

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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%.

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Qualitative and quantitative determination of azaarenes by high-performance liquid chromatography

Warzecha L., Janoszka B., Dobosz C.

Chemia Analityczna

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1999

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Vol. 44, No. 4

677-687

EN

On the basis of the analysis performed on mixtures of standards we attempted to optimize a method of qualitative and quantitative determination of azaarenes using reversed phase high-perfonnance liquid chromatography. The values of k coefficients of standards were compared for the separation under isocratic conditions and by gradient elution. The opti-mum separation conditions for 2-5-ring azaarenes were obtained by using the following gradient. 40% CH3CN in water (2 min), increasing linearly (up to 100%) CH3CN (24 min), 100% CH3CN (14 min). By applying the above procedure for the extracts from airborne particulate matter and sewage sludge samples collected in the Upper Silesia region of Poland we were able to identify in these extracts the following compounds: benzoquinolines, acridine, phenanthridine and benzo(c)cinnoline. The total concentration of these compounds in the airbome particulate matter extract was 2x 10-2 % while in the sewage sludge extract it was 1.25x 10(-2) %.

PL

Przy wykorzystaniu mieszanin wzorców przeprowadzono badania nad optymalizacją oznaczeń jakościowo-ilościowych azaarenów metodą wysokosprawnej chromatografii cieczowej w odwróconym układzie faz. Porównano wartości współczynników retencji k wzorców rozdzielanych w warunkach izokratycznych oraz przy użyciu elucji gradientowej. Optymalne warunki rozdzia1u 2-5 pierścieniowych azaarenów otrzymano stosując gradient elucji: 40% CH3CN W wodzie (2 min), liniowy wzrost stężenia CH3CN do 100% (24 min), 100% CH3CN (14 min). Stosując opracowaną metodykę zidenty-fikowano w ekstrakcie pył owych zanieczyszczeń powietrza oraz w ekstrakcie osadu ściekowego z rejonu Górnego Śląska m.in. benzochinoliny, akrydynę, fenantrydynę, benzo( c )cynnolinę. Łączne stężenie tych związków w ekstrakcie pyłów wynosił o 2x 10-2 % m, a w ekstrakcie z osadu ściekowego 1.25 x 10-2 % m.

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Solid-phase extraction and HPLC method for isolation and analysis of organic compounds formed in thermally treated proteinaceous foods

Warzecha L., Janoszka B., Stróżyk M.

Acta Chromatographica

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1999

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No. 9

176-193

EN

On the basis of analyses performed on standard mixtures we have optimized a method for selective separation and qualitative determination of organic compounds formed during cooking of proteinaceous foods. These compounds belong to three chemical groups – polycyclic aromatic hydrocarbons (PAH), azaarenes, i.e. nitrogen-containing polycyclic aromatic hydrocarbons (PANH), and heterocyclic aromatic amines (HAA). The selective enrichment procedure includes coupling of solid-phase extraction (SPE) steps on diatomaceous earth, propylsulphonic acid and octadecyl-silane columns. The fractions eluted were analysed by high-performance liquid chromatography with UV detection. Peak identification was confirmed by GC–MS for PAH, PANH, and for amide derivatives of aminoazaare-nes. Recoveries were higher than 82% for PAH but lower for azaarenes, 60–76%.

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HPLC determination of acridine-type polycyclic aromatic nitrogen heterocompounds (PAHNs, azaarenes)

Stróżyk M., Warzecha L.

Acta Chromatographica

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1999

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No. 9

142-154

EN

A study has been conducted to optimize the qualitative analysis of azaarenes by HPLC. Values of the capacity factors, k, of standards separated by reversed-phase gradient elution on a non-polar octadecylsilica adsorbent or by normal-phase isocratic elution on a polar aminopropyl-silica adsorbent were compared. Both methods enabled the separation of azaarenes containing 2–5 aromatic rings per molecule. Although analysis time was considerably less on the aminopropylsilica stationary phase, it was found that this column, as opposed to the C18 column, was deactivated more rapidly, and its performance changes after a few analyses of azaarene fractions isolated from organic extracts of airborne material.

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Application of high performance liquid chromatography with fluorescence detection for determination of nitroarenes, after their reduction to aromatic amines

Warzecha L., Stróżyk M.

Chemia Analityczna

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1998

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Vol. 43, No. 5

807-816

EN

Reversed-phase high performance liquid chromatography with fluorescence detection has been used for qualitative/quantitative determination of nitroarenes after their reduction to corresponding aromatic amines. Two methods of nitroarenes reduction to aromatic amines were compared. The reduction efficiency of nitroarene standards using NaHS was found to be higher than NaBH(4)/CuCl(2) reduction system. 2-Nitrofluorene and 1-nitropyrene were identified in the organic extract of dusts collected in Upper Silesia Region with detection limits of 9 pg and lpg respectively. It has been shown that the contents of nitroarenes were within the range of 4.3-5.0 ug g(-1) of dust.

PL

Zastosowano wysokosprawną chromatografię cieczową w odwróconym układzie faz i detektor fluorescencyjny do oznaczania jakościowego i ilościowego nitroarenów po ich redukcji dwoma metodami, do odpowiednich amin aromatycznych. Wydajności redukcji wzorcowych nitroarenów przy użyciu NaHS jako reduktora były wyższe, niż w przypadku zastosowania do redukcji NaBH(4)/CuCl(2). W ekstrakcie pyłów pobranych w rejonie Górnego Śląska zidentyfikowano 2-nitrofluoren oraz 1-nitropiren przy granicy oznaczalności odpowiednio 9 pg i 1 pg. Sumaryczna zawartość tych nitrozwiązków, w zależności od zastosowanej metody analitycznej, wyniosła 4.3-5.0 ug g (-1) pyłu.