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1

Effect of ripening process and fat content on changes in vitamin K level of cheese®

Polak-Śliwińska Magdalena, Remiszewska Jolanta, Śliwiński Mariusz

Postępy Techniki Przetwórstwa Spożywczego

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2022

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nr 2

52--64

EN

In this study, the vitamin K1 (phylloquinone) and vitamin K2 (menaquinone) contents of a selected range of cheeses were measured by high-performance liquid chromatography (HPLC) and compared with the fat content, maturation time and origin of the cheeses. In our study, the highest vitamin K2 content was recorded in Gouda (678.12 ng/g), Edam (712.70 ng/g) and Emmentaler (733.10 ng/g) cheeses with comparable levels of vitamin K1 in the analysed products (31.60 ng/g, 34.63 ng/g and 24.35 ng/g, respectively) and fat content (27%, 28% and 30%, respectively), as well as in Gouda cheese with a fat content of 48% after 48 weeks of maturation (756.50 ng/g). The fat content of the cheese was a factor that influenced the vitamin K content, with products with lower fat content having lower total vitamin K content compared to the other products analysed. Given the reports that poor vitamin K status is one of the risk factors for cardiovascular disease in the absence of conclusive evidence of adverse cardiovascular effects of dairy fats, cheese should be considered as an important dietary component for those concerned about heart health.

PL

W tym badaniu oznaczono zawartość witaminy K1 (filochinonu) i witaminy K2 (menachinonu) w wybranej gamie serów metodą wysokosprawnej chromatografii cieczowej (HPLC) i porównano z zawartością tłuszczu, czasem dojrzewania i pochodzeniem serów. W badaniach własnych największą zawartość witaminy K2 odnotowano w serach Gouda (678,12 ng/g), Edam (712,70 ng/g) i Emmentaler (733,10 ng/g) przy porównywalnych poziomach witaminy K1 w analizowanych produktach (odpowiednio 31,60 ng/g, 34,63 ng/g i 24,35 ng/g) i zawartości tłuszczu (odpowiednio 27%, 28% i 30%), jak również w serze Gouda o zawartości tłuszczu 48% po 48 tygodniach dojrzewania (756.50 ng/g). Zawartość tłuszczu w serze była czynnikiem, który wpływał na zawartość witaminy K, przy czym produkty o niższej zawartości tłuszczu miały niższą całkowitą zawartość witaminy K w porównaniu z pozostałymi analizowanymi produktami. Biorąc pod uwagę doniesienia, że słaby status witaminy K jest jednym z czynników ryzyka chorób sercowo-naczyniowych przy braku jednoznacznych dowodów na niekorzystny wpływ tłuszczów mlecznych na układ krążenia, sery powinny być traktowane jako ważny składnik diety osób, które dbają o zdrowie serca.

2

Wykorzystanie nowoczesnych metod w badaniach niezawodnościowych amunicji eksploatowanej w SZ RP

Kamieńska-Duda A., Prasuła P.

Problemy Techniki Uzbrojenia

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2015

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R. 44, z. 135

91--101

PL

W artykule przedstawiono wybrane przypadki zastosowania nowoczesnych metod analizy fizykochemicznej (metodę chromatograficzną HPLC oraz termiczną DSC) w badaniach amunicji, w sytuacjach wymagających uzyskania danych identyfikacyjnych substancji nieznanego pochodzenia w krótkim czasie. Artykuł jest kontynuacją badań realizowanych w Zakładzie Badań Materiałów Wybuchowych przedstawionych w pracy „Szczególne przypadki wad materiałów wybuchowych”.

EN

The paper presents selected cases of using modern physicochemical analysis methods (HPLC chromatography and thermal DSC methods) for testing ammunition when the identification data of material with unknown origin is required in a short period of time. The following paper is a continuation of the work conducted in Research and Testing Department of High Explosives presented in publication “Particular cases of explosive material defects”.

3

Validation of the assay and purity determination of the FOX-7 (1,1-diamino-2,2-dinitroethylene) using HPLC method

Kamieńska-Duda A., Kasprzak P.

Problemy Techniki Uzbrojenia

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2014

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R. 43, z. 130

79--87

EN

1,1-diamino-2,2 dinitroethylen (DADNE, FOX-7) is a novel explosive with low sensivity. The valuable properties is a result of specific chemical construction, in which inter- and intramolecular hydrogen bonds stabilize the structure. From the reason of low sensivity, FOX-7 has a very broad spectrum of use for elaborating many kinds of munnition. Hence a very important aspect is to conduct the research of this substance to determine chemical purity, assay content of water etc. The HPLC method is the one of the analytical technique which has a very high precision of determination of the purity and assay of the substance. The aim of this work was to compile a new method of the assay and purity determination of FOX-7. The C18-Xbridge column and the mobile phase: Acetonitryle: Water: Triethylamine were used. Through application of the C18- XBridge column and mobile phase the substrate MPD and main substance FOX-7 had very good resolution and the analysis time was relatively short. The validation of the new method has been performed: selectivity, specificity, linearity, precision, assay and limits of detection and quantitation. We have also checked the stress tests of the FOX-7 in acidic, basic and oxidative conditions.

PL

1,1-diamino-2,2 dinitroetylen (DADNE, FOX-7) jest nowoczesną małowrażliwą substancją wybuchową. Jej cenne właściwości są rezultatem specyficznej budowy chemicznej, w której wewnątrz i zewnątrz cząsteczkowe wiązania wodorowe stabilizują strukturę, powodując jej małą wrażliwość na bodźce. Dzięki takim właściwościom, FOX-7 może być zastosowany do elaboracji wielu rodzajów małowrażliwej amunicji. Dlatego tak ważnym aspektem jest prowadzenie badań chemicznych uwzględniających czystość i zawartość chemiczną tej substancji. Metoda HPLC jest nowoczesną techniką, szeroko stosowaną do określenia tych parametrów z dużą dokładnością i precyzją. Celem naszej pracy było zwalidowanie nowej metody oznaczania czystości i zawartości FOX-7. Do oznaczania tych parametrów użyto kolumny C-18 X-Bridge natomiast jako fazy ruchomej mieszaniny acetonitrylu trietyloaminy: wody zmieszanej w odpowiednim stosunku. Zastosowanie właśnie takiej kolumny oraz fazy z modyfikatorem pozwoliło na podzielenie zanieczyszczenia MPD od substancji głównej w odpowiednio krótkim czasie z dobrą rozdzielczością oraz symetrią pików. Walidacja metody obejmowała: selektywność, specyficzność, precyzję, dokładność oraz limity detekcji oraz oznaczalności. Podczas walidacji zostały również przeprowadzone testy stresowe w warunkach kwaśnych, zasadowych oraz utleniających.

4

Optimization of determination of reduced and oxidized glutathione in rat striatum by HPLC method with fluorescence detection and pre-column derivatization

Gawlik M., Krzyżanowska W., Gawlik M. B., Filip M.

Acta Chromatographica

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2014

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Vol. 26, no. 2

335--345

EN

A high-performance liquid chromatography (HPLC) method was used to assess the concentration of reduced and oxidized glutathione (GSH and GSSG) in rat striatum. Following decapitation, striatum was isolated from the male Wistar rat brain and immediately homogenized with double distilled water. GSH level was determined after pre-column derivatization with o-phthalaldehyde (OPA). The optimal incubation time with OPA was tested. The concentration of GSSG was determined after blockage the thiol groups of GSH by N-ethylmaleimide (NEM). The useful time for incubation with NEM was optimized. Next, disulfide bounds of GSSG were reduced by dithiothreitol (DTT), and released GSH is derivatized with OPA. The total glutathione, tGSH (sum of free and bound GSH, GSSG, and other low-molecular-mass aminothiols), was determined after reduction with DTT and then derivatization with OPA. The level of GSSG was calculated of the difference in concentrations of tGSH and GSH, but we showed that the calculated concentration of GSSG was within the range of standard deviation of the mean concentration of tGSH or GSH. Finally, the concentration of GSH was determined after 5-min incubation with OPA and the concentration of GSSG after 30-s incubation with NEM and 5-min incubation with DTT and OPA. The relative standard deviation (RSD) values obtained for the assay of GSH and GSSG were lower than 10%. The values obtained for accuracy for GSH (50–500 nM) and GSSG (0.5–5 nM) were within limits regarded as acceptable for analysis of biological samples (percent of recovery: 95–105%). Mean absolute recovery of GSH and GSSG was ranged from 97.1% to 99%. Limit of detection for GSH was 2.7 nM, and limit of quantification was 8.2 nM. Limit of detection (LOD) for GSSG is twice the value for GSH. Described method allows to determine GSH and GSSG levels in isolated rat brain structures with high level of reliability.

5

Oznaczanie czystości enancjomervcznej oraz kontrola międzyoperacyjna metodą HPLC w technologii wytwarzania optycznie czynnej substancji aktywnej na przykładzie winianu tolterodyny

Puchalska M., Zagrodzka J., Czerniec-Michalik E., Zezula M., Chmiel J., Łuniewski W., Zagrodzki B.

Przemysł Chemiczny

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2012

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T. 91, nr 3

358-364

PL

Przedstawiono izokratyczną chiralną metodę HPLC z detekcją UV stosowaną do oznaczania czystości enancjomerycznej L-(+)-winianu (R)-tolterodyny. Metodę zastosowano do kontroli międzyoperacyjnej procesu oczyszczania oraz do badania substancji aktywnej otrzymywanej w technologii opracowanej w Instytucie Farmaceutycznym. Opracowane procedury analityczne zostały zwalidowane zgodnie z wytycznymi ICH.

EN

Applicability of the isocratic chiral high-performance liq. chromatog. with UV detection for detn. of the enantiomeric purity of active pharmaceutical ingredients was successfully tested on an example of (R)-2-[3-(diisopropylamino)- 1-phenylpropyl]-4-methylphenyl L-(+)-tartarate. Contents of both (R) and (S) isomers were detd.

6

2-Cyjanoakrylan etylu – metoda oznaczania

Kowalska J.

Podstawy i Metody Oceny Środowiska Pracy

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2011

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Nr 1 (67)

73--78

PL

Metoda polega na adsorpcji par 2-cyjanoakrylanu etylu na żywicy XAD-7 pokrytej kwasem fosforo-wym(V), desorpcji mieszaniną kwasu fosforowego w acetonitrylu i analizie chromatograficznej (HPLC/UV) otrzymanego roztworu. Oznaczalność metody wynosi 0,06 mg/m³.

EN

This determination method is based on the adsorption of ethyl 2-cyanoacrylate vapours on phosphoric acid-treated XAD-7 sampling tubes (80/40 mg sections), desorption with 2 ml of acetonitryle and high performance liquid chromatographic (HPLC/UV) analysis of the resulting solution. The determination limit of the method is 0.1 mg/m3.

7

An HPLC method for the determination of the anticancer complex 3-hydroxycarboplatin

Yang Sh., Chen X., Zhen P, Ye Q., Xie X, Liu W.

Acta Chromatographica

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2011

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Vol. 23, no. 4

539--550

EN

A simple and rapid HPLC method using a photodiode array (PDA) detector for the analysis of 3-hydroxycarboplatin and its related complex has been established for the first time. Separation of 3-hydroxycarboplatin and 3-hydroxy-1,1-cyclobutanedicarboxylic acid (3-HO-cbdca) was carried out on a Phenomenex ODS3 column using an aqueous solution containing 50 mM ammonium acetate and 5 mM sodium 1-octanesulfonate as the mobile phase. The flow rate was 0.8 mL min-1, the column temperature was 40°C, and the detection wavelength was 230 nm for 3-hydroxycarboplatin and 220 nm for 3-HO-cbdca. Different analytical performance parameters such as precision, accuracy, linearity, stability of the solution, specificity, limit of detection (LOD), limit of quantification (LOQ), and system suitability were determined using the Empower 2 software. The calibration curve of standard 3-hydroxycarboplatin showed good linearity (r = 0.9995) within the range 0.5–1.4 mg mL-1. The method was accurate and precise, with an average accuracy of 100.4% (RSD = 1.53%, n = 9), and the results of the system suitability test showed symmetrical peaks, good resolution (Rs), and repeatability. It can be applied to the quality control of 3-hydroxycarboplatin.

8

The influence of biotic factors on phytoplankton pigment composition and resources in Baltic ecosystems: new analytical results

Stoń-Egiert J., Łotocka M., Ostrowska M., Kosakowska A.

Oceanologia

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2010

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No. 52 (1)

101-125

EN

Mathematical expressions were derived describing the distribution and concentration of individual phytoplankton pigments with respect to biotic factors in the southern Baltic. Relationships were established between the chlorophyll a concentration and the total phytoplankton biomass (represented by the organic carbon content), as well as between the concentration of marker pigments and the biomasses of the corresponding phytoplankton classes. Knowledge of chlorophyll a concentrations allows the phytoplankton biomass to be estimated with a precision characterised by relative statistical errors according to logarithmic statistics of σ_= ca 56%. The best approximation was obtained for the dependence of the Bacillariophyceae biomass on the fucoxanthin concentration (σ_= 60%), Chlorophyceae on the lutein concentration (σ_=48%), and the total biomass of Dinophyceae, Bacillariophyceae and Euglenophyceae on the concentration of diadinoxanthin, the main carotenoid pigment present in cells of species from these classes (σ_=60%).

9

Walidacja metody HPLC stosowanej dla kontroli procesu mycia aparatury przy wytwarzaniu substancji farmaceutycznej

Baran P. A., Bielejewska A., Glice M. M., Beczkowicz H., Maruszak W., Kosmacińska B., Gołębiewski P.

Przemysł Chemiczny

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2007

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T. 86, nr 8

747-750

10

Morfolina – metoda oznaczania

Kowalska J.

Podstawy i Metody Oceny Środowiska Pracy

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2007

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Nr 4 (54)

85--90

PL

Metoda polega na adsorpcji par morfoliny na żywicy XAD-2 pokrytej izotiocyjanianem 1-naftylu, desorpcji acetonitrylem otrzymanej pochodnej morfoliny i analizie chromatograficznej otrzymanego roztworu. Oznaczalność metody wynosi 3,6 mg/m3.

EN

The determination method is based on the adsorption of morpholine vapours on sampling tubes containing 80/40 mg sections of XAD-2 resin coated with 1-naphtylisothiocyanate (NIT), desorption with 2 ml of acetonitryle and high performance liquid chromatographic (HPLC/UV) analysis of the resulting solution. The determination limit of the method is 3.6 mg/m3.

11

2-Cyjanoakrylan metylu – metoda oznaczania

Kowalska J.

Podstawy i Metody Oceny Środowiska Pracy

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2006

|

Nr 4 (50)

11--16

PL

Metoda polega na adsorpcji par 2-cyjanoakrylanu metylu na żywicy XAD-7 pokrytej kwasem fosforowym, desorpcji mieszaniną kwasu fosforowego (0,2%, v/v) w acetonitrylu i analizie chromatograficznej (HPLC/UV) otrzymanego roztworu. Oznaczalność metody wynosi 0,2 mg/m3.

EN

The determination method is based on the adsorption of methyl 2-cyanoacrylate vapours on phosphoric acid- treated XAD-7 sampling tubes (80/40 mg sections), desorption with 2 ml of 0.2%(v/v) phosphoric acid in acetonitryle and high performance liquid chromatographic (HPLC/UV) analysis of the resulting solution. The determination limit of the method is 0.2 mg/m3.

12

Simultaneous separation of chlorophylls and carotenoids by RP-HPLC in some algae and cyanobacteria from the southern Baltic

Jodłowska S., Latała A.

Oceanological and Hydrobiological Studies

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2003

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Vol. 32, No. 2

81-89

EN

RP-HPLC (reversed-phase high-performance liquid chromatography) was used to analyse chlorophyll and carotenoid pigments in cyanobacteria and algae from the Baltic Sea, belonging to different taxonomic groups. The following species were used: Cyclotella meneghiniana - diatom, Oocystis submarina - green alga and Phormidium amphibium - cyanobacterium. Investigations on a favourable method of chlorophyll and carotenoid pigment separation have been carried out. This method allowed to separate the following pigments: lutein and zeaxanthin; diadinoxanthin and fucoxanthin; chlorophyll c1 and c2, into sharp peaks. It could be presumed that the method would be useful and universal in the identification of pigments in other algal and cyanobacteria species and natural phytoplankton assemblages.

13

Changes in phytoplankton pigments composition during 2000 in different southern Baltic regions

Ston J., Kosakowska A.

Oceanological Studies

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2002

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Vol. 31, No. 1-2

75-89

EN

The results of differences in phytoplankton pigments composition are presented in this paper. Samples from the Southern Baltic taken during three cruises on r/v "Oceania" (14.02 - 28.02.2000, 06.05 - 16.05.2000 and 20.09 - 01.10.2000) were examined. Qualification and quantification analyses of chlorophylls and carotenoids present in samples of naturally existing phytoplankton were based on the RP-HPLC technique. Seasonal and spatial variability in pigment characteristics was observed in the analysed seasons. Presence of: chlorophyll a, chlorophyll c1+c2, chlorophyll b, alloxanthin, zeaxanthin, fucoxanthin, peridinin, neoxanthin, diadinoxanthin - was noted in every season; violaxanthin and beta-carotene - only in May and September. Lutein was detected only in May samples. The quantity of May and September pigments exceeded 2-6 times the February pigments content. Vertical differentiation in the pigments amount was also noted. Spatial variability emphasized the influence of Vistula and Odra water masses. Different markers of phytoplankton species were found in each season: in February - cryptophytes (alloxanthin), May - diatoms (fucoxanthin) and September - cyanophytes and dinophytes (containing zeaxanthin and diadinoxanthin).

14

Pigment composition in relation to phytoplankton community structure and nutrient content in the Baltic Sea

Stoń J., Kosakowska A., Łotocka M., Łysiak-Pastuszak E.

Oceanologia

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2002

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No. 44 (4)

419-437

EN

The concentration of chlorophylls and carotenoids with respect to communities of characteristic phytoplankton species and hydrological parameters, such as temperature, salinity and nutrients were analysed. Samples from the southern Baltic were taken during three periods: spring 1999, autumn 1999 and 2000 during cruises of r/v 'Oceania' in this area. The seasonal differences between the phytoplankton species composition and pigmentation of samples (measured by HPLC) were noted. The total biomass of the spring phytoplankton population was 11-15 times greater than that of the autumn populations. However, the phytoplankton community was more diverse in the two autumns, whereas the spring population was almost mono-taxonomic: > 80% of the total biomass consisted of dinophytes. The total content of chlorophylls (a, b, c1 + c2) was about 20 times higher in spring. Moreover, in spring the concentrations of photosynthetic carotenoids (with dominant perdinin) were 2-4 times higher than those of the photoprotecting carotenoids (with dominant diadinoxanthin), whereas in the two autumns the situation was reversed: PPC concentrations (with dominant zeaxanthin and diadinoxanthin) exceeded those of PSC (with dominant fucoxanthin) by c. 3-10 times. Pigment markers have proved to be extremely useful biomarkers for elucidating the composition of phytoplankton populations in natural samples.

15

Wykorzystanie HPLC do oznaczania witamin rozpuszczalnych w tłuszczach

Wieliński S., Olszanowski A.

Wiadomości Chemiczne

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2001

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[Z] 55, 11-12

1075-1102

EN

In this review, selected chemical techniques such as TLC, UV-VIS, GC, HPLC and microbiological procedures (published since 1960) used for simultaneous determination of fat-soluble vitamins in different matrices have been discussed. Particular attention has been given to HPLC methods, not only in terms of chromatographic conditions, but also in comparison with other separation techniques. HPLC methods have been shown to have clear advantages over existing chemical or microbiological assays in terms of sensitivity, specificity and sample throughput for the analysis of these vitamins. In order to assist the analyst in the selection of a particular procedure, certain chromatographic conditions have been listed for this purpose. However, as currently, no specific HPLC procedures can be recommended, it was decided to develop new methods for these vitamins. Within the past 30 years, HPLC has become the predominant method for separation and quantification of fat-soluble vitamins. The two major, distinct methods of HPLC separation are referred to as normal-phase chromatography and reverse-phase chromatography. To generalise, reverse-phase HPLC is frequently preferred for analysis of biological samples as the columns are more easily purged of any contaminants and sample separation is usually less sensitive to slight changes in mobile-phase composition. A summary of HPLC systems used for fat-soluble vitamins analysis is provided in Table 1 [60-106] and 2 [107-152] in format: compounds determined, matrix, sample preparation and clean up, column, mobile phase, detection, time of analysis, reference. Finally, this paper describes a procedure for the simultaneous determination of vitamin A (retinol acetate, palmitate), vitamin D3 (cholecalciferol), vitamin E (alpha-tocopherol acetate) and alphacalcidol in capsules from a single sample extract using reverse phase HPLC and column backflushing techniques [162-165]. The procedure eliminates saponification, lengthy extractions and sample workup. It is specific to the compounds of interest, shows very good internal precision and is free of interference compared to current published methods.

16

Qualitative and quantitative analysis of Baltic phytoplankton pigments

Ston J., Kosakowska A.

Oceanologia

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2000

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No. 42 (4)

449-471

EN

The paper presents the results of research into the pigment composition of seawater samples taken from various depths in the Gulf of Gdansk in April and September 1999. Pigments were separated by RP-HPLC, and identification was confirmed by co-injection with reference standards and on-line diode array spectra. The following groups of pigments were identified: chlorophylls: a, b, c1 + c2; photosynthetic carotenoids (PSC) - peridinin, fucoxanthin, alfa-carotene; photoprotecting carotenoids (PPC) - diadinoxanthin, alloxanthin, zeaxanthin, lutein, neoxanthin, violaxanthin and beta-carotene. Quantitative and qualitative diversity in pigment characteristics were observed in both seasons, though lutein and alfa-carotene were not identified in the September samples. The respective April and September concentrations of the functional groups of pigments were: total chlorophylls content 0.47-104.25 and 0.57-13.66 žg dm–3; PSC 0.07-21.23 and 0.02-1.56 žg dm–3; PPC 0.05-14.08 and 0.04-1.79 žg dm–3. Within the PSC group, peridinin and fucoxanthin were dominant in the April samples, but only fucoxanthin in the September ones. Among the PPCs, diadinoxanthin and alloxanthin were dominant in April, zeaxanthin in September. Photosynthetic and photoprotecting carotenoids display a linear correlation with chlorophyll alfa content in all the samples.