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Tytuł:
Relationship between micellar liquid chromatography retention of sulfonamides and the pH and concentration of surfactants and organic modifiers in the mobile phase
Autorzy:
Szymański, A.
Powiązania:
https://bibliotekanauki.pl/articles/347039.pdf
Data publikacji:
2011
Wydawca:
Politechnika Bydgoska im. Jana i Jędrzeja Śniadeckich. Wydział Technologii i Inżynierii Chemicznej
Tematy:
micellar liquid chromatography
retention mechanism
sulfonamides
Opis:
The paper presents an attempt to adapt a retention model suggested and verified by classic RP LC in micellar liquid chromatography, MLC. Instead of hydrophobic interactions with ODS groups and electrostatic interactions with silanol residues in C-18 packing, hydrophobic interactions with alkyl groups and ionic interactions with anionic moieties of the SDS-modified stationary phase were considered. Due to the different characteristics of the stationary phase in the MLC depending on the pH of the mobile phase, the equation used to determine the contribution of electrostatic interactions to retention was modified. Theoretical curves for the relationship between retention and SDS micelle concentration in the mobile phase, organic modifier concentration and eluent pH were determined. For comparison, curves based on data obtained in basic sulfonamide studies were plotted in the same coordinate systems and units. A complete qualitative similarity was noted between the theoretical curves predicting retention changes with changing micellar mobile phase parameters and the curves determined based on experimental results for the sulfonamides. The qualitative similarity involves a similar shape of the respective curves and identical tendencies. In general, a larger reduction of sulfonamide retention with respect to the predicted value is noted. The deviation results from changes in the sulfonamide property with changing pH of the mobile phase.
Źródło:
Ars Separatoria Acta; 2011, 8; 51-67
1731-6340
Pojawia się w:
Ars Separatoria Acta
Dostawca treści:
Biblioteka Nauki
Artykuł
Tytuł:
Separation of nonreacted acrylamide from polyacrylamide gel for endoprothesing
Autorzy:
Gertsyuk, M.
Samchenko, Y.
Powiązania:
https://bibliotekanauki.pl/articles/346993.pdf
Data publikacji:
2007
Wydawca:
Politechnika Bydgoska im. Jana i Jędrzeja Śniadeckich. Wydział Technologii i Inżynierii Chemicznej
Tematy:
hydrogels
acrylamide
acrylic monomers
liquid chromatography
endoprothesis
Opis:
The separation of toxic acrylic monomers (mainly acrylamide) from some polymeric hydrogels of medical application was studied. It was found that “clean hydrogel” can be obtained after 4-6 days of washing with nonpyrogenic water. The quantity of monomeric acrylamide remained in the samples was controlled by a liquid chromatography method.
Źródło:
Ars Separatoria Acta; 2007, 5; 98-101
1731-6340
Pojawia się w:
Ars Separatoria Acta
Dostawca treści:
Biblioteka Nauki
Artykuł
Tytuł:
Food quality control by hyphenated separation techniques
Autorzy:
Walczak, J.
Pomastowski, P.
Buszewski, B.
Powiązania:
https://bibliotekanauki.pl/articles/2052456.pdf
Data publikacji:
2015
Wydawca:
Akademia Bialska Nauk Stosowanych im. Jana Pawła II w Białej Podlaskiej
Tematy:
food analysis
hyphenated techniques
liquid chromatography
mass spectrometry
Opis:
Food as complex mixture of proteins, lipids, vitamins, etc. cannot be separated and identified by using in only one method. This article presents a revision on the hyphenated chromatographic techniques and methods used in food analysis and described main application in food science research, and determination of xenobiotics and their metabolites in environmental. Also article discusses applications of “omics” in food analysis (proteomics, transcriptomics, genomics, metabolomis) and new discipline of – foodomics.
Źródło:
Health Problems of Civilization; 2015, 09, 1; 33-38
2353-6942
2354-0265
Pojawia się w:
Health Problems of Civilization
Dostawca treści:
Biblioteka Nauki
Artykuł
Tytuł:
Retention mechanism of sulfonamides in micellar reversed phase liquid chromatography
Autorzy:
Szymański, A.
Powiązania:
https://bibliotekanauki.pl/articles/347037.pdf
Data publikacji:
2011
Wydawca:
Politechnika Bydgoska im. Jana i Jędrzeja Śniadeckich. Wydział Technologii i Inżynierii Chemicznej
Tematy:
micellar liquid chromatography
quantitative structure-activity relationships
sulfonamides
Opis:
A mechanism of retention of sulfonamides in the micellar liquid chromatography, based on similar models verified for other compounds, was proposed. The magnitudes of hydrophobic and electrostatic interactions of sulfonamides were estimated for different concentrations of surfactant in the mobile phase and at varied pH. With increasing SDS concentrations and at a constant pH, a decrease in the hydrophobic interaction intensity was noted. When pH is varied, the values of the constant, describing the hydrophobicity of the sulfonamides, remained at an approximately same level (taking into account the standard deviation values). Greater differences were observed in the constants related to the electrostatic interactions informing about the increase or decrease in retention, following from ionic interactions. For each sulfonamide, the molar fraction of the ionic fractions present in the mobile phase was calculated from the formula derived, which permitted determination of the type of electrostatic interactions, varying with the eluent’s changing pH. On the basis of the chromatographic data collected, it was established that retention of sulfonamides in the SDS micellar system depends on the hydrophobic and electrostatic interactions. For varied pH values, the hydrophobic interactions of sulfonamides did not change significantly, all changes in the retention of the sulfonamides were attributed to changes in the electrostatic interactions.
Źródło:
Ars Separatoria Acta; 2011, 8; 69-80
1731-6340
Pojawia się w:
Ars Separatoria Acta
Dostawca treści:
Biblioteka Nauki
Artykuł
Tytuł:
DETERMINATION OF ACYCLOVIR IN RABBIT PLASMA BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC (HPLC) TECHNIQUE
Autorzy:
Malik, Nadia S.
Ahmad, Mahmood
Minhas, Muhammad U.
Khalid, Qandeel
Powiązania:
https://bibliotekanauki.pl/articles/895236.pdf
Data publikacji:
2019-06-28
Wydawca:
Polskie Towarzystwo Farmaceutyczne
Tematy:
plasma
acyclovir
Reversed phase high-performance liquid chromatography
Opis:
A rapid, sensitive and simple reversed-phase high-performance liquid chromatographic (HPLC) method has been developed and validated for the determination of acyclovir (ACV) in rabbit plasma. BDS C18 column was used to conduct analysis using ammonium dihydrogen phosphate buffer (50mM) and methanol as mobile phase (98:2), with pH adjusted to 2.5 using orthophosphoric acid. Flow rate was kept at 1 mL/min. Selective precipitation of plasma proteins were done by adding 5% perchloric acid. Precipitated plasma proteins were separated by centrifugation. ACV moves in a supernatant, which was snapped and passed through a syringe filtration assembly. Direct injection of supernatant was given into a BDS C18 column and ACV was detected at 256 nm. The limit of detection for ACV in plasma was estimated as 15ng/mL whereas the limit of quantitation was calculated as 25 ng/mL. Moreover, the developed method has been found to be selective and linear into concentration range of 25 – 2000 ng/mL. The present method could be successfully applied to samples from bioavailability and bioequivalence studies.
Źródło:
Acta Poloniae Pharmaceutica - Drug Research; 2019, 76, 3; 421-429
0001-6837
2353-5288
Pojawia się w:
Acta Poloniae Pharmaceutica - Drug Research
Dostawca treści:
Biblioteka Nauki
Artykuł
Tytuł:
The Sensitive Method of Determination of Hazardous Phthlates in Polymeric Building Materials by High Performance Liquid Chromatography
Autorzy:
Kaniowska, Elżbieta
Kaczmarczyk, Grzegorz
Powiązania:
https://bibliotekanauki.pl/articles/2174914.pdf
Data publikacji:
2022
Wydawca:
Politechnika Koszalińska. Wydawnictwo Uczelniane
Tematy:
liquid chromatography
HPLC
phthalates
REACH
PVC
polyvinyl chloride
Opis:
Polymeric building materials and equipment for indoor use in spaces intended for people may, in an essential way, contribute to the deterioration of wholesome quality of life. Phthalates, present in many products, constitute an omnipresent group of compounds used widely as plasticisers. The research results show that these substances may negatively impact human health, and thus European Union has implemented several regulatory measures restricting their use. Manufacturers and suppliers must comply with these regulations. As a result, it is necessary to investigate and determine the contents of phthalates in these materials. This paper presents the analytic profile of the method of marking phthalates extracted from polyvinyl chloride using HPLC chromatography with UV-VIS detection and selected results obtained in examinations of materials used in interior design. The results of described examinations of phthalates content indicate that not all materials recommended by manufacturers may be used indoors in spaces intended for people. The method was verified for its suitability for routine analyses of materials made of PVC and submitted for attestation. The elaborated method can be used to determine the banned phthalates’ presence in PVC. The method allows for detecting these phthalates at the level required by the REACH regulation, and its validation parameters are highly satisfactory considering a very complex matrix.
Źródło:
Rocznik Ochrona Środowiska; 2022, 24; 190--201
1506-218X
Pojawia się w:
Rocznik Ochrona Środowiska
Dostawca treści:
Biblioteka Nauki
Artykuł
Tytuł:
Chromatographic methods for determination of neopterin in urine
Chromatograficzne metody oznaczania neopteryny w moczu
Autorzy:
Waligóra, A.
Waligóra, S.
Tyrpień-Golder, K.
Powiązania:
https://bibliotekanauki.pl/articles/270489.pdf
Data publikacji:
2017
Wydawca:
Centralny Ośrodek Badawczo-Rozwojowy Aparatury Badawczej i Dydaktycznej, COBRABiD
Tematy:
neopteryna
pterydyny
chromatografia cieczowa
ELISA
neopterin
pteridines
liquid chromatography
Opis:
Neopterin is considered to be a non-specific marker for the activation of the human immune system. It is synthesized by monocytes/macrophages in the immune response caused by T cells. The physiological role of neopterin and its derivatives is based on the modulation of macrophage cytotoxicity by enhancing the activity of reactive oxygen species under certain conditions. The concentration of neopterin is regarded as the evaluation parameter of oxidative stress immunologically induced. High concentrations of neopterin were observed in biological fluids of patients with bacterial infection, viral, autoimmune diseases and cancer and vascular diseases. At the proper neopterin elimination from the body, its concentrations in urine correlate to those in the serum or plasma. Measuring the concentration of neopterin is important in monitoring of the course of immunological activity in disease. In special cases, the determination of neopterin concentration was used in the differential diagnosis. This paper describes various methods for determining neopterin in urine primarily by high performance liquid chromatography (HPLC), and enzyme-linked immunosorbent assay (ELISA). HPLC techniques are predominant due to the possibility of modifying the chromatographic system and other parameters. The combination of these methods may be useful in developing new analytical procedures for determining neopterin in urine.
Neopteryna, uważana za niespecyficzny marker aktywacji ludzkiego układu odpornościowego, syntezowana jest przez monocyty/makrofagi w odpowiedzi immunologicznej wywołanej przez limfocyty T. Fizjologiczna rola neopteryny oraz jej pochodnych polega na modulowaniu cytotoksyczności makrofagów poprzez zwiększanie aktywności reaktywnych form tlenu w określonych warunkach. Stężenie neopteryny jest uznawane za parametr oceny stresu oksydacyjnego wywołanego stanem zapalnym, a jej wysokie stężenia odnotowano m.in. w płynach biologicznych osób z infekcją bakteryjną, wirusową, chorobami autoimmunologicznymi i nowotworowymi oraz z chorobami układu krwionośnego. Przy prawidłowej eliminacji neopteryny z organizmu jej stężenie w moczu jest skorelowane z oznaczanymi w surowicy lub w osoczu. Oznaczanie stężenia neopteryny ma istotne znaczenie w monitorowaniu ak tywności immunologicznej wielu chorób. W szczególnych przypadkach oszacowanie jej stężenia w materiale biologicznym znalazło zastosowanie w diagnostyce różnicowej. W pracy zostały opisane różne metody oznaczania neopteryny w moczu, głównie z zastosowaniem wysokosprawnej chromatografii cieczowej (HPLC) i kompetycyjnego testu immunoenzymatycznego (ELISA). Dominują głównie techniki chromatograficzne (HPLC), ze względu na możliwość modyfikacji układu chromatograficznego oraz innych parametrów. Zestawienie tych metod może być pomocne w opracowaniu nowych procedur analitycznych oznaczania neopteryny w moczu.
Źródło:
Aparatura Badawcza i Dydaktyczna; 2017, 22, 1; 12-19
2392-1765
Pojawia się w:
Aparatura Badawcza i Dydaktyczna
Dostawca treści:
Biblioteka Nauki
Artykuł
Tytuł:
Characterization of flavonoid components in Scutellaria L. species (Lamiaceae) using finger-printing analysis
Autorzy:
Dehkordi, F.J.
Kharazian, N.
Lorigooini, Z.
Powiązania:
https://bibliotekanauki.pl/articles/2117811.pdf
Data publikacji:
2020
Wydawca:
Polska Akademia Nauk. Czasopisma i Monografie PAN
Tematy:
chemical groups
flavone
liquid chromatography
Scutellaria multicaulis
Scutellar-
ioideae
Opis:
The genus Scutellaria L., Lamiaceae family, Scutellarioideae sub-family is known as the most important medicinal plant in the world. This research aimed to investigate the flavonoid content of seven Scutellaria species from the center, southwest, and west of Iran. Via thin layer and column chromatography, the flavonoid was extracted from leaves and then purified. To screen the flavonoid compositions, a chromatographic method was applied by liquid chromatography mass spectrometry on a triple quadrupole mass spectrometer (LC/TQMS/MS). Fingerprint analysis was implemented so as to characterize a total of 73 chemical compounds, from which 71 compounds were flavonoids belonging to different classes. Flavone with 37 derivatives possessed major values. The most abundant flavonoid compounds were observed in S. multicaulis (23 compounds) and S. patonii (22 compounds). Flavonoid composition, including apigenin, kaempferol, quercetin, and hydroxyl- flavones represented remarkable derivatives. A total of 45 flavonoids, one tannin and one anthraquinone compound, were observed to be primarily separated and identified for Scutellaria species. Moreover, six categorized chemical groups were identified in this genus and proposed as chemical barcodes. The specific chemical groups strongly provided the boundaries of Scutellaria species, the pharmacological value enhancement, breeding programs, and comprehensive documents of the species. According to the results, LC/TQMS/MS was proven a dominant method regarding genus Scutellaria.
Źródło:
Acta Biologica Cracoviensia. Series Botanica; 2020, 62, 1; 79-96
0001-5296
Pojawia się w:
Acta Biologica Cracoviensia. Series Botanica
Dostawca treści:
Biblioteka Nauki
Artykuł
Tytuł:
The effect of the concentration of the ionic liquid didecyldimethylammonium lactate on the retention and separation of pyrimidine bases
Autorzy:
Szymański, M.
Zapart, J.
Florek, G.
Szymański, A.
Powiązania:
https://bibliotekanauki.pl/articles/347003.pdf
Data publikacji:
2013
Wydawca:
Politechnika Bydgoska im. Jana i Jędrzeja Śniadeckich. Wydział Technologii i Inżynierii Chemicznej
Tematy:
ionic liquids
reversed-phase high-performance liquid chromatography
additives
Opis:
Ionic liquids (IL) are new materials with a wide spectrum of use. Being a variable combination of an organic cation and an organic or inorganic anion, their have controllable properties. The effect of the ionic liquid added to the mobile phase on the separation of uracil derivatives is studied and demonstrated in this paper. The ionic liquid used was didecyldimethylammonium lactate, which has an advantageous effect on the separation of the analytes studied. Pyrimidine bases which were used as the test compounds are characterized by alkaline properties due to which so-called peak tailing is observed during separation. A methanol/water mixture was used as the mobile phase in the chromatographic analyses. Optimum separations were obtained for 8% levels of the organic modifier. The best separations of the test isomers were obtained for 0.01% IL added to the mobile phase. The findings obtained are evidence that the use of ionic liquids in HPLC is an efficient method for the separation of polar compounds: the duration of the analysis is shorter and the resulting peaks are sharp and symmetrical.
Źródło:
Ars Separatoria Acta; 2012-2013, 9/10; 15-24
1731-6340
Pojawia się w:
Ars Separatoria Acta
Dostawca treści:
Biblioteka Nauki
Artykuł
Tytuł:
Determination of oleuropein in herbal preparation and Olea europaea L. extracts by HPLC
Autorzy:
Szymański, M.
Witkowska-Banaszczak, E.
Matławska, I.
Szymański, A.
Powiązania:
https://bibliotekanauki.pl/articles/346909.pdf
Data publikacji:
2013
Wydawca:
Politechnika Bydgoska im. Jana i Jędrzeja Śniadeckich. Wydział Technologii i Inżynierii Chemicznej
Tematy:
oleuropein
Olea europaea L.
herbal products
high performance liquid chromatography
Opis:
Oleuropein is a secoiridoide monoterpene. It is found primarily in all parts of the Olea europaea L. tree, mostly in its unripe fruit and leaves. It has a number of beneficial effects on the human body, being readily absorbed from the gastrointestinal tract due to its hydrophilic properties. The paper presents a simple, rapid and precise method for the assay of oleuropein in herbal formulations and the European Olive leaf extract. Chromatographic separation was performed using a C-18 column with an acetonitrile/water 20/80% vol. mixture as the mobile phase. The method has a wide range of linearity between 0.05 and 1.5 mg/mL, very good repeatability of retention time, and accuracies between 95.8 and 103.3%. Its limit of detection is 0.04 mg/mL. The developed method was tested on two herbal formulations which are commercially available in Poland.
Źródło:
Ars Separatoria Acta; 2012-2013, 9/10; 55-63
1731-6340
Pojawia się w:
Ars Separatoria Acta
Dostawca treści:
Biblioteka Nauki
Artykuł
Tytuł:
The use of a bead mill for the production of agrochemical suspensions
Autorzy:
Szwedziak, Katarzyna
Grzywacz, Żaneta
Tomaszewski, Sławomir
Powiązania:
https://bibliotekanauki.pl/articles/298130.pdf
Data publikacji:
2019
Wydawca:
Uniwersytet Warmińsko-Mazurski w Olsztynie
Tematy:
suspension
pearl mill
plant protection products
liquid chromatography
formulation
fungicides
Opis:
Plant protection products represent one of the most innovative branches of the agrochemical industry which requires considerable financial investment to adequately meet agricultural needs. The optimal agrochemicals should enable farmers to maximize yields, and their components should remain active over long periods of time regardless of weather conditions. This article describes an innovative technology for the production of agrochemical suspensions in a bead mill. The suspension acts as a carrier of active ingredients. The parameters of the bead mill were presented, and the resulting suspensions were used in the production of fungicides. The parameters of the substrates used in the production of agrochemicals have to comply with legal regulations. The present experiment involved liquid chromatography, and it was conducted in accordance with good practice, in line with CIPAC guidelines.
Źródło:
Technical Sciences / University of Warmia and Mazury in Olsztyn; 2019, 22(3); 271-280
1505-4675
2083-4527
Pojawia się w:
Technical Sciences / University of Warmia and Mazury in Olsztyn
Dostawca treści:
Biblioteka Nauki
Artykuł
Tytuł:
Determination of trace quantities of dutasteride in water and wastewater by solid phase extraction and high-performance liquid chromatography
Autorzy:
Wasilewska, A.
Madajczyk, M.
Szymański, A.
Urbaniak, W.
Powiązania:
https://bibliotekanauki.pl/articles/347041.pdf
Data publikacji:
2011
Wydawca:
Politechnika Bydgoska im. Jana i Jędrzeja Śniadeckich. Wydział Technologii i Inżynierii Chemicznej
Tematy:
dutasteride
emerging pollutants
solid-phase extraction (SPE)
liquid chromatography
HPLC
Opis:
Steroid compounds are a kind of pollutants which are increasingly more frequently found in environmental samples. Due to the ever more increasing level of such pollutants and their biological activity, they are of interest to analysts. Our study involved the development of a simple and fast method for the assay of dutasteride in treated industrial waste water using high-performance liquid chromatography. As the steroid concentration in water is much lower than the limit of detection of the UV detector used, the compound assayed in the test water was pre-concentrated using solid-phase extraction. Our procedure has high accuracy and a precision of 2.6%, and the recovery of the analyte from water is 78.6%. The procedure enables the assay of dutasteride at a level of 2 microg/L in water.
Źródło:
Ars Separatoria Acta; 2011, 8; 39-49
1731-6340
Pojawia się w:
Ars Separatoria Acta
Dostawca treści:
Biblioteka Nauki
Artykuł
Tytuł:
Micro-capillary liquid chromatography Fourier transform ion cyclotron resonance mass spectrometry—apowerful tool for peptide and protein identification.
Autorzy:
Ramström, Margareta
Palmblad, Magnus
Amirkhani, Ardeshir
Tsybin, Youri
Markides, Karin
Håkansson, Per
Bergquist, Jonas
Powiązania:
https://bibliotekanauki.pl/articles/1044053.pdf
Data publikacji:
2001
Wydawca:
Polskie Towarzystwo Biochemiczne
Tematy:
liquid-chromatography
peptides
Fourier transform ion cyclotron resonance mass spectrometry
proteins
Opis:
In order to be able to study complex biological samples, a micro-capillary liquid chromatography system was coupled to a 9.4 T Fourier transform ion cyclotron resonance mass spectrometer. The setup was tested on a tryptic digest of bovine serum albumin, which resulted in high sequence coverage (> 92% the protein.
Źródło:
Acta Biochimica Polonica; 2001, 48, 4; 1101-1104
0001-527X
Pojawia się w:
Acta Biochimica Polonica
Dostawca treści:
Biblioteka Nauki
Artykuł
Tytuł:
Synthesis and properties of model humic substances derived from gallic acid
Autorzy:
Slawinska, D.
Polewski, K.
Rolewski, P.
Slawinski, J.
Powiązania:
https://bibliotekanauki.pl/articles/25730.pdf
Data publikacji:
2007
Wydawca:
Polska Akademia Nauk. Instytut Agrofizyki PAN
Tematy:
humic acid
humic substance
gallic acid
antioxidant
high performance liquid chromatography
Źródło:
International Agrophysics; 2007, 21, 2
0236-8722
Pojawia się w:
International Agrophysics
Dostawca treści:
Biblioteka Nauki
Artykuł
Tytuł:
Determination of chloramphenicol in milk powder using liquid-liquid cartridge extraction (Chem Elut) and liquid chromatography-tandem mass spectrometry
Autorzy:
Zawadzka, I.
Rodziewicz, L.
Powiązania:
https://bibliotekanauki.pl/articles/876762.pdf
Data publikacji:
2014
Wydawca:
Narodowy Instytut Zdrowia Publicznego. Państwowy Zakład Higieny
Tematy:
chloramphenicol
determination
milk powder
liquid-liquid extraction
liquid chromatography-tandem mass spectrometry
veterinary drug residue
Opis:
Background. The European Union prohibits the use of chloramphenicol (CAP) as a veterinary drug in food-producing animals. Nevertheless, CAP have been detected in milk products (liquid milk and milk powder). Therefore, it is necessary to develop sensitive methods for determining CAP residues in milk powder. Objective. The aim of this study was to develop and validate a confirmatory method for determination of CAP in milk powder. Material and methods. Chloramphenicol was determined in milk powder using LC-ESI-MS/MS in negative mode. After fat removing milk powder sample was extracted/cleaned-up with a Chem Elut extraction cartridge. Separation was achieved on a Phenomenex Luna C-18 column with acetonitrile-water as a mobile phase. The mass spectrometer was operated in multiple reaction monitoring mode (MRM). Four transitions were monitored m/z 321→152, 321→194, 321→257 (CAP) and 326→157 (IS CAP-d5). Results. Linearity, accuracy, precision, decision limit (CCa), detection capability (CCb) and ruggedness were determined for m/z 321→152. The mean relative recoveries (inter standard-corrected) of CAP from whole milk powder spiked at levels 0.1, 0.2, 0.3 and 0.6 mg/kg were in the range 95 - 103%. Relative standard deviation (RSD%) of recoveries at all spiked levels were less than 14%. RSDs within-laboratory reproducibility calculated at fortification of 0.3 mg/kg was less than 16%. CCa and CCb were below 0.1 mg/kg. Conclusions. The developed LC-MS/MS method allows the determination of CAP in milk powder. The method was validated according to the Commission Decision No. 2002/657/EC requirements. This method can be applied to determination CAP in whole and skim milk powder.
Wprowadzenie. Unia Europejska zabroniła stosowania chloramfenikolu (CAP) jako leku weterynaryjnego u zwierząt, których produkty są przeznaczone do spożycia. Pomimo tego, CAP jest wykrywany w produktach mleczarskich (mleko i mleko w proszku). Cel. Celem badań było opracowanie i zwalidowanie metody pozwalającej na oznaczanie CAP w mleku w proszku. Materiał i metoda. CAP był oznaczany w mleku w proszku metodą LC-ESI-MS/MS w trybie jonizacji ujemnej. Po usunięciu tłuszczu próbka była ekstrahowana/oczyszczana za pomocą ekstrakcyjnych kolumienek Chem Elut. Do rozdziału CAP stosowano kolumnę chromatograficzną Phenomenex Luna C-18. Fazę ruchomą stanowił acetonitryl/woda. Spektrometr masowy pracował w trybie monitorowania wybranych reakcji (MRM). Cztery przejścia były monitorowane m/z 321→152, 321→194, 321→257 (CAP) i 326→157 (IS CAP-d5). Wyniki. Liniowość, odzysk, precyzja, limit decyzyjny (CCa), zdolność wykrywania (CCb) i odporność metody zostały wyznaczone dla 321→152. Średni względny odzysk CAP z mleka pełnego był wyznaczony dla próbek wzbogaconych na poziomach odpowiadających 0.1, 0.2, 0.3 i 0.6 mg/kg i mieściły on się w zakresie 95 - 103%. Względne odchylenie stadardowe (RSD%) dla wszystkich poziomów było mniejsze niż 14%. Powtarzalność wewnątrzlaboratoryjna (RSDs) obliczona dla poziomu wzbogacenia 0.3 mg/kg była mniejsza niż 16%. CCa and CCb były poniżej 0.1 mg/kg. Wnioski. Opracowana metoda LC-ESI-Ms/MS pozwala oznaczyć CAP w mleku w proszku. Metoda została zwalidowana zgodnie z wymaganiami decyzji Komisji nr 2002/657/WE. Metoda może być stosowana do mleka pełnego i odtłuszczonego.
Źródło:
Roczniki Państwowego Zakładu Higieny; 2014, 65, 3
0035-7715
Pojawia się w:
Roczniki Państwowego Zakładu Higieny
Dostawca treści:
Biblioteka Nauki
Artykuł
Wyświetlanie 1-15 z 70

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