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1

Jednoczesne oznaczanie aspiryny i kwasu salicylowego w wodzie za pomocą wysokosprawnej chromatografii cieczowej z detekcją UV po wstępnym zatężaniu metodą ekstrakcji do fazy stałej (SPE)

Kaniowska E., Kaczmarczyk G., Garboś S., Święcicka D.

Instal

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2018

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nr 12

41--43

PL

W związku z potencjalnym zanieczyszczeniem wody przeznaczonej do spożycia przez farmaceutyki, opracowano i zwalidowano czułą metodę służącą do oznaczeń powszechnie stosowanej substancji czynnej - kwasu acetylosalicylowego (ASP) oraz produktu jego rozkładu - kwasu salicylowego (SAL) w wodzie. W tym celu zastosowano technikę wysokosprawnej chromatografii cieczowej z detektorem z matrycą diodową (HPLC-PDA). Do analiz wykorzystano kolumnę chromatograficzną nowej generacji typu Develosil XG-C30M (150×4,6 mm, 3 μm), po wstępnym zatężaniu analitów na kolumienkach SPE Oasis HLB. Opracowana metoda charakteryzuje się granicami oznaczalności - 14 ng/l (ASP) i 28 ng/l (SAL) oraz średnimi odzyskami na poziomach odpowiednio 82% i 73%. Sprawdzono przydatność metody do oznaczania kwasu acetylosalicylowego i finalnego produktu jego rozkładu w próbkach wody wodociągowej, przy czym stwierdzono, że stężenia tych związków w badanych próbkach nie przekraczają ww. granic oznaczalności.

EN

In view of the potential pollution of water intended for human consumption by pharmaceuticals, a sensitive method for the determination of the commonly used active pharmaceutical ingredient - acetylsalicylic acid (ASP) and product of its degradation - salicylic acid (SAL) has been developed and validated. For this purpose, the technique based on high performance liquid chromatography with photodiode array detector (HPLC-PDA) was applied. Analyses were conducted with the use of a new generation of chromatographic column Develosil XG-C30M (150×4,6 mm, 3 μm), after preconcentration of analytes on SPE columns Oasis HLB. The developed method is characterized by quantification limits of 14 ng/l (ASP) and 28 ng/l (SAL) and average recoveries at the levels of 82% and 73%, respectively. Acetylsalicylic acid and product of its degradation were determined in drinking water samples of various origin, and it was found that concentrations of these compounds in investigated samples were not exceeded the above-mentioned quantification limits.

2

Zastosowanie tokoferolu i kwasu acetylosalicylowego w ochronie tkanki kostnej przed skutkami doświadczalnego zatrucia 2,3,7,8-tetrachloro-dibenzo-p-dioksyną (TCDD)

Dobrzyński M., Bazan J., Gamian A, Rosińczuk-Tonderys J, Parulska O, Całkosiński I.

Rocznik Ochrona Środowiska

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2014

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Tom 16, cz. 1

300--322

EN

Dioxins are released into the environment as by-products of technological processes, i.a. in the chemical industry, pulp and paper industry, metallurgical industry, textile industry and dyeing industry. Dioxins are a group of compounds recognized by the International Agency for Research on Cancer (IARC) as carcinogens of Group A since 01/06/1997. The carcinogenic action has been demonstrated on animals. Despite stringent obligations arising from the provisions of The Stockholm Convention on Persistent Organic Pollutants on reducing POPs emissions to the environment (including dioxins) emission of these substances is still significant. These compounds often enter the food chain in random or intentional way and accumulate in organisms in the top of the food chain. This leads to the poisoning of the organism and appearance of clinical symptoms. According to the real hazard of poisoning the people, especially employed in the chemical industry, who are exposed to dioxins, research to determine the impact of these xenobiotics on various tissues and organs as well as to develop of effective pharmacological prevention is constantly conducted. Despite of the wide spectrum of the assessment of dioxins biological effects among humans and animals, there are only a few publications evaluating the impact of dioxins on the bone tissue. The main components of the fully functional bone are calcium phosphates and magnesium phosphates. From the proper saturation of bone matrix with salts of these chemical elements (mineralization) depends the hardness and elasticity of the bone. The young bone mineralization is controlled by a group of proteins, from which the most important is osteonectin, osteocalcin and alkaline phosphatase. Many xenobiotics, including dioxins, have a negative influence on the biosynthesis of these proteins. The measurement of calcium and magnesium concentration in bone is one of the methods for assessing bone destruction. The aim of this study was to investigate the effect of 2,3,7,8-tetrachlorodobenzo-p-dioxin (TCDD) in rats on calcium and magnesium levels in bone tissue of their offspring. Moreover the aim of this study was to check whether the administration of the dioxin receptor antagonists – tocopherol and acetylsalicylic acid – can reduce negative effects of dioxin action. Study was performed on 2-day newborns of Buffalo strain rats. Lower levels of calcium and magnesium was found both in cranial vault bones and the knee from newborns of mothers exposed to 2,3,7,8-tetrachlorodibenzo-p-dioxin. It was shown that administration of mothers exposed to 2,3,7,8- tetrachlorodibenzo-p-dioxin tocopherol or acetylsalicylic acid prevent decreases in calcium and magnesium concentrations in the bone tissue of the offspring.

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Wpływ zmian pH i temperatury na adsorpcję kwasu acetylosalicylowego na przemysłowych węglach aktywnych

Szymonik A., Lach J.

Proceedings of ECOpole

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2014

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Vol. 8, No. 2

611--617

PL

Obecność kwasu acetylosalicylowego stwierdzono m.in. w Wiśle (0,4 μg/dm3), w Odrze (0,73 μg/ dm3), w Wełtawie (0,31 μg/dm3). Kwas acetylosalicylowy zidentyfikowano również w wodach pitnych (Francja - 19 ng/dm3, Niemcy - 10 ng/dm3). Przeprowadzono badania wpływu pH i temperatury nad sorpcją kwasu acetylosalicylowego z roztworów wodnych na przemysłowych węglach aktywnych: WG-12, ROW-08, F-300. Badania prowadzono w zakresie pH od 2 do 10 i w temperaturze 20 i 30ºC. Najefektywniej adsorpcja przebiegała na węglu aktywnym ROW-08. Najwięcej cząstek jest adsorbowanych przy niskich wartościach pH (pH = 2) i w niższej temperaturze (20ºC). Wraz ze wzrostem pH i temperatury wielkość adsorpcji maleje.

EN

The presence of acetylsalicylic acid was confirmed among others in River the Wisla (0.4 μg/ dm3), in the Odra River (0.73 μg/dm3), in River the Vltava (0.31 μg/dm3). The following acetylsalicylic acid was also found in drinking water (France - 19 ng/dm3, Germany - 10 ng/dm3). The article presents the results of the study on sorption of acetylsalicylic acid from water solutions on the selected industrial activated carbons: WG-12, ROW-08 and F-300. Studies carried out in the pH range from 2 to 10 and in 20, 30ºC temperature degree. The efficiency of sorption on selected activated carbons depends on pH and temperature of the solution subjected to sorption. The most effective adsorption proceeded on activated carbon ROW-08.The highest number of particles was adsorbed at low values of pH (pH = 2) and at low temperature (20ºC). With the increase in pH and temperature of the solution the efficiency of adsorption decreases.

4

Association between the N-acetylation genetic polymorphism and aspirin-induced urticartia

Porębski G., Obtulowicz K., Piwowar M., Roterman-Konieczna I.

Bio-Algorithms and Med-Systems

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2008

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Vol. 4, no. 8

19--23

EN

N-acetylation represents one of the key pharmacogenetic traits in metabolism of xenobiotics, including drugs. Dominance of ‘slow-acetylators’ has been demonstrated in atopic patients, contact allergy and has been investigated in patients with sulfonamide hypersensitivity. The aim of this survey was to assess genotype of N-acetyltransferase2 (NAT2) polymorphism in patients with aspirin-induced urticaria (AIU). To the study we included 24 consecutive patients with medical history of urticaria induced by aspirin and 123 healthy controls. In the patients’ group oral provocation tests (OPT) up to 565mg cumulative dose of acetylsalicylic acid were performed. The NAT2 alleles (*4-wilde type, *5, *6 and *7) were determined by polymerase chain reaction-restriction fragment length polymorphism method with DNA extracted from peripherial blood. It was observed 53.7% of slow acetylators in the control group, and respectively 66.7%, 83.3% and 100% in the patients with AIU, in patients with positive OPT and in patients with positive reaction in OPT assessed as severe. Statistical significance association between NAT2*5/NAT2*6 genotype and aspirin-induced urticaria was revealed. The linkage of AIU and slow acetylation (NAT2*5/NAT2*6) seems to be highly probable in the patients with medical history of skin hypersensitivity to aspirin confirmed by positive oral provocation test.

5

Theoretical simulation of infrared spectra of acetylsalicylic acid

Boczar M., Wójcik M. J., Szczeponek K., Jamróz D., Zięba A.

Bulletin of the Polish Academy of Sciences. Chemistry

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2002

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Vol. 50, No. 4

397-402

EN

Theoretical simulation of the v(s) stretching band is presented for acetylsalicylic acid (aspirin) at two temperatures 77 and 300 K. The simulation takes into account adiabatic couplings between the high-frequency O-H stretching and the low-frequency intermolecular O...O stretching modes, linear and quadratic distortions of the potential energy of the low-frequency vibrations in the excited state of the O-H stretching vibration, resonance interaction between the two hydrogen bonds in a dimer, and Fermi resonance between the O-H stretching and the overtone of the O-H bending vibrations.

6

Synteza i zastosowanie koniugatu kwasu oligo-3-hydroksymasłowego i kwasu acetylosalicylowego

Juzwa M., Kurek A., Zawidlak B., Jedliński Z.

Inżynieria Biomateriałów

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2001

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R. 4, nr 17-19

20-20

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Analysis of ternary solutions by applying the spectrophotometric measurements of unary, binary and ternary standard solutions

Stefański A., Stolarczyk M.

Chemia Analityczna

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2001

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Vol. 46, No. 2

261-268

EN

An original method described in [5] has been applied to the analysis of ternary solutions. The method is based on absorbance measurements made for an examined sample and the appropriate mixture. Both solutions were of almost identical concentration of the same substances. The quantitative composition of a sample has been determined from preliminary analysis by using the formulae derived from measurements of unary, binary and ternary standard solutions. The formulae which enable to calculate the concentrations for each constituent of the analysed sample are expressed as a simple sum of three products. Two sets of the control solutions were prepared, each containing 10 samples, in order to verify the accuracy of analysis carried out for the three-component drug called "Tabletki od bolu glowy z krzyzykiem" ("Cross-marked headache-relieving tablets"). One extra set of composition considerably different from those of other two sets was prepared to check the applicability of the above method to the analysis of other solutions.

PL

Zastosowanie opisanej w [5] metody pozwoliło na analizę mieszanin trójskładnikowych na podstawie pomiarów absorbancji roztworu próbki badanej i odpowiedniej mieszaniny modelowej, w której stężenia składników były zbliżone do analizowanej próbki. Ilościowy skład mieszaniny modelowej ustalono na podstawie wstępnej analizy próbki badanej, dokonując pomiarów absorbancji dla roztworów badanych i porównawczych jedno-, dwu- i trójskładnikowych. Zastosowane do obliczeń stężeń wzory są w postaci trzech iloczynów. W celu sprawdzenia dokładności wyników, przygotowano dwie serie roztworów kontrolnych po 10 próbek każda, o składzie zbliżonym do analizowanego leku, które wykorzystano do oznaczenia składników w preparacie "Tabletki od bólu głowy z krzyżykiem" oraz jedną serię roztworów, których skład odbiegał od poprzednich w celu sprawdzenia przydatności opisanej metody w analizie dowolnych próbek.

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Simultaneous spectrophotometric determination of acetylsalicylic acid, paracetamol and caffeine in pharmaceutical preparations

Nogowska M., Muszalska I., Zając M.

Chemia Analityczna

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1999

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Vol. 44, No. 6

1041-1048

EN

Differences the UV spectra of acetylsalicylic acid (ASA), paracetamol (P) and caffeine (C) in ethanol have made the grounds for a new spectrophotometric method for the determination of particular components in "Thomapyrin" preparation, without the separation of active substances. The analytical wavelengths were 226 nm for acetylsalicylic acid, 250 nm for paracetamol and 272 nm for caffeine. For all compounds analysed, the specific absorption in ethanol at these three wavelengths was detemined. The appropriate equations were derived and the method was validated taking into account its specificity, limits of quantiation of ASA, P and C, linearity in the range from about 50% to 120% relative to the values declared in "Thomapyril1", accuracy and precision.

PL

Zróżnicowane widma UV w etanolu kwasu acetylosalicylowego (ASA), paracetamolu (P) i kofeiny ( C) stały się podstawą opracowania bezpośredniej metody spektrofotometrycznej, pozwalającej oznaczyć zawartość poszczególnych składników w preparacie " Thomapyrin" bez rozdziału substancji czynnych. Jako analityczne długości fali przyjęto: dla kwasu acetylosalicyjowego 226 m, paracetamolu 250 nm i kofeiny 272 nm. Dla wszystkich oznaczanych związków wyznaczono absorpcję właściwą w etanolu przy ww. trzech długościach fali. Ustalono odpowiednie równania i przeprowadzono walidację. metody, w której uwzględniono specyficzność, granicę; oznaczalności ASA, P i C, liniowość w zakresie od ok. 50% do ok. 120% względem wartości deklarowanej- w preparacie ,,Thomapyrin", dokładność oraz: precyzję.