8 research outputs found

    Gospodarka odpadami w ramach regionu płockiego – deklaracje mieszkańców

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    The text of the article pertained to waste management in local government in the region of Płock. In my article described were changes to waste management after 1 July 2013, as well as methods of comparing local governments.Tekst artykułu dotyczy gospodarki odpadami w samorządzie w regionie płockim. W artykule opisano zmiany w gospodarce odpadami po 1 lipca 2013 r., a także metody porównywania samorządów

    Application of hydrophilic interaction liquid chromatography for the quantification of succinylcholine in Active Pharmaceutical Ingredient and medicinal product. Identification of new impurities of succinylcholine chloride

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    A new method, using hydrophilic interaction chromatography (HILIC), for quantification of succinylcholine and impurities in Active Pharmaceutical Ingredient (API), as well as in the medicinal product, was developed. Additionally, the new impurities in API were discovered using ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UHPLC-QTOF) technique. The substances were quantified with the application of a UV detector (λ = 214 nm). Chromatographic separation was performed isocratically with the application of 30% phosphate buffer (pH 4,0; 0.05 M) in ACN as a mobile phase. A major feature of the developed method is a very high resolution (Rs > 3), between succinylcholine and its main impurity - succinylmonocholine, whereas the width of peak bands does not exceed 0.7 min. A low value of limits of detection (LOD) were obtained for succinic acid, succinylmonocholine and for succinylcholine, which amounted to 2.4, 6.0 and 11.5 μg ml−1, respectively. Another feature of the developed method is linearity in a very wide range of concentrations: 7.3 μg ml−1 – 670 μg ml−1 amounting to R2 = 0.999. The recovery provided by this method at three different fortification levels for all analytes remained within the following range: 95.7 – 98.9 %. Intra-day and inter-day precision remained within the following range: 1.0 – 5.9 % coefficient of variation (CV), whereas accuracy within the range: −1.3 – 6.3. The developed method of hydrophilic interactions made it possible to quantify two new impurities, probably originating from the synthesis of an API: [2-(trimethylaminium)ethyl]-[2ʹ-(trimethylaminium)vinyl] succinate and [2-(dimethylamino)etyl]-[2ʹ-(trimethylaminium)etyl] succinate, which were identified and described for the first time. In addition, a physicochemical form of peak doublet described in the USP as impurities was studied and it was demonstrated that these peaks are the result of the specific physicochemical interactions in ion pair chromatography

    Analysis of Menaquinone-7 Content and Impurities in Oil and Non-Oil Dietary Supplements

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    Rapid, global technological development has caused the food industry to use concentrated food component sources like dietary supplements ever more commonly as part of the human diet. This study analysed the menaquinone-7 (MK-7) content of dietary supplements in oil capsule and hard tablet forms. A novel method for separating and measuring geometric isomers of MK-7 in dietary supplements was developed and validated. Eleven different isomers of cis/trans- menaquinone-7 were identified. Identification of cis/trans isomers was performed by combination of HPLC, UPLC and HRMS-QTOF detection, whereas their quantities were determined by DAD detection. The content of menaquinone impurities was ascertained, including cis/trans- menaquinone-6 isomers (5.5–16.9 µg per tablet/capsule) and cis/trans-menaquinone-7 isomers (70.9–218.7 µg tablet/capsule), which were most likely formed during the chemical synthesis of the menaquinone-7. The all-trans MK-7 content was lower than the isomeric form and often lower than what the labels declared. A new method of quantification, developed and validated for menaquinones in oil capsules, provided on average 90% recovery and a limit of quantification (LOQ) of approximately 1 µg mL−1

    Synthesis of Oxidized 3β,3′β-Disteryl Ethers and Search after High-Temperature Treatment of Sterol-Rich Samples

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    It was proven that sterols subjected to high-temperature treatment can be concatenated, which results in polymeric structures, e.g., 3β,3′β-disteryl ethers. However, it was also proven that due to increased temperature in oxygen-containing conditions, sterols can undergo various oxidation reactions. This study aimed to prove the existence and perform quantitative analysis of oxidized 3β,3′β-disteryl ethers, which could form during high-temperature treatment of sterol-rich samples. Samples were heated at 180, 200 and 220 °C for 0.5 to 4 h. Quantitative analyses of the oxidized 3β,3′β-disteryl ethers were performed with liquid extraction, solid-phase extraction and liquid chromatography coupled with mass spectrometry. Additionally, to perform this analysis, the appropriate standards of all oxidized 3β,3′β-disteryl ethers were prepared. Eighteen various oxidized 3β,3′β-disteryl ethers (derivatives of 3β,3′β-dicholesteryl ether, 3β,3′β-disitosteryl ether and 3β,3′β-distigmasteryl ether) were prepared. Additionally, the influence of metal compounds on the mechanism of ether formation at high temperatures was investigated
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