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Abstract
Due to the frequent use of paracetamol formulations, it is useful to develop an analytical technique for the determination of intact paracetamol in presence of other drugs and excipients or the degradation products. In this study, a simple, isocratic, fast, specific, accurate and precise stability-indicating high performance liquid chromatography (HPLC) method has been developed and validated for simultaneous quantitative determination of paracetamol (PCM) and potassium sorbate (PS) in oral liquid formulations. The chromatographic separation was achieved on Zorbax SB C18 column (150 × 4.6 mm, 5 µm) with Zorbax SB C18 precolumn (12.5 × 4.6 mm, 5 µm) using distilled water pH 2 with ortho-phosphoric acid and acetonitrile (70:30, v/v) as a mobile phase, and UV detection at 235 nm. The temperature of the column was kept constant at 25 °C. The method was validated according to International Conference on harmonization (ICH) guidelines. The method demonstrated excellent linearity, with a correlation coefficient of 0.9996 and 0.9998 for PCM and PS, respectively, over the concentration ranges of 10–600 μg mL−1 (PCM) and 6–500 μg mL−1 (PS). The retention time was found to be 1.98 and 4.86 min for PCM and PS, respectively. Oral liquid formulation samples were subjected to various stress conditions (acidic and alkaline hydrolysis, as well as oxidative, heat and photolytic degradation) for the purpose of forced degradation study. The major degradation of paracetamol was achieved in acidic and basic stress conditions, while thermal and photolytic degradation generally had the least influence. On the other hand, potassium sorbate was highly susceptible to photolytic degradation. It was also shown that the formulation has strong influence on stability of tested compounds. Forced degradation studies demonstrated the stability-indicating power of the method and can be used to assess the stability of paracetamol and potassium sorbate in oral liquid formulations.
Abstract
Baricitinib (BRT) is a drug substance with potent anti-inflammatory activity indicated in rheumatoid arthritis, atopic dermatitis, severe alopecia areata and recently for the treatment of Covid-19. Process impurities of the drug during its formulation are quite known, however studies regarding its degradation products (DPs) under stress conditions are limited. In this study, the drug was subjected to forced degradation under various degradation conditions, including acidic hydrolysis, alkaline hydrolysis, oxidative and thermal, to determine its inherent stability. To this purpose, a novel HPLC method was developed for the determination of degradation impurities of BRT. Alkaline hydrolysis test showed a selectivity towards breaking C–C bonds. This resulted to five DPs formed by chain scission reactions occurred at the pyrrolo-pyrimidine group between C6–C10 and C8–C9. Also, the ethylsulfonyl-azetidin-ylidene group was subjected to C–C bond cleavage at C12–C15 and C16–C18. Degradation products were further characterized with the use of liquid chromatography quadrupole time of flight tandem mass spectrometry (LC-Q-TOF-MS/MS).
Abstract
A gradient high-performance liquid chromatography (HPLC) method has been developed to determine the concentrations of latanoprost (LP) and latanoprost free acid (LPA) in aqueous solutions. It is novel due to a combination of its simplicity, speed, and detection capability in aqueous solutions for both active drug (LPA) and prodrug (LP). This method is applicable for the research and development of novel drug delivery devices and quality control assays for experimental and commercial laboratory settings, as it allows for a high sample throughput. Samples were chromatographed across a C18 + 2.7 µm 4.6 × 7.5 mm reversed-phase column with gradient elution using a mobile phase of aqueous acetic acid (pH 3.1) and acetonitrile with 0.1% acetic acid. UV spectrophotometry was used to monitor the eluents at 210 nm. Drug concentrations from 1.0 to 150 μg mL−1 were tested, with good linearity observed across the range. LPA had a signature peak at approximately 4.82 min (SD < 0.08) and LP at 9.27 min (SD < 0.07). For both drug and pro-drug, LOD and LOQ were 1.0 and 2.5 μg mL−1, respectively. This assay which accurately measures both prodrug and drug in a single injection, has significant applicability in determining the release kinetics of novel LP drug delivery systems.
Abstract
The advection-convection models (ACM) have practical applications in the investigation of separation processes, where mass (heat) is transferred by convection and diffusion (dispersion) along mass/heat exchanger, eq. adsorption, chromatography column, tubular reactor, etc. The ACM consists of nonlinear partial differential equations which can be solved only with numerical methods. In the article, a comparison of the volume method (VM) and orthogonal collocation on finite elements (OCFE) is presented in terms of their reliability, accuracy of calculations, and speed of calculation. The OCFE proved to be more robust than VM.
The linear ACM model for the chromatography column has an analytical solution in the form of the equation for the number of theoretical plates (N). This equation is often applied in the interpretation and evaluation of model parameters. However, the versions of N equation published in the literature are not correct. The error can lead to significant imprecision for specific cases. Here, in the paper, the revised equations are presented and discussed for the most frequently used chromatography column models.
Abstract
Plant protection products (PPP), crucial for agricultural production, are experiencing increased global demand, particularly with the growing need for food production. To meet this demand, robust analytical methods are essential for confirming the presence and determining active substance concentrations in PPP. This study introduces an analytical method utilizing high-performance liquid chromatography with a diode array detector (HPLC-DAD) for determination of acetamiprid in water-soluble powder formulations. The method, validated according to SANCO/3030/99 rev.5, demonstrated exhibited adequate accuracy and precision, with repeatability expressed as the ratio of the standard deviation (% RSD) to the relative standard deviation (% RSDr) being lower than 1. Recoveries for the active substance at concentrations above 10% ranged from 97% to 103%. The developed method is also characterized by suitable linearity, confirmed by a correlation coefficient >0.99. Specific chromatographic profiles were generated, and acetamiprid content in 180 formulations was analyzed, including reference products. The developed method aligns with “green chemistry” principles, minimizing solvent use and emphasizing energy efficiency. Overall, it offers a comprehensive approach for qualitative and quantitative analysis, ensuring the reliability of PPP quality control.
Pilóta nélküli légi járművek alkalmazása a vizes élőhelyek modern felmérésében
Application of unmanned aerial vehicles as modern tools for wetland monitoring
A vizes élőhelyek a vízi és a szárazföldi ökoszisztémák között elhelyezkedő, igen változatos, és általában nehezen lehatárolható területek. Kiemelt jelentőségük annak köszönhető, hogy bár csak a globális szárazföldi területek mintegy 6–7%-át borítják, kulcsfontosságú szerepet játszanak az éghajlat szabályozásában, a vizes ökoszisztémák biodiverzitásának és hidrológiai viszonyainak fenntartásában, valamint számos további ökológiai és társadalmi funkciót is szolgáltatnak, beleértve az árvízvédelmi, víztisztítási, szén-dioxid-tárolási, élőhelytámogatási és kulturális, rekreációs előnyöket. A vizes élőhelyek azonban mind természetes, mind antropogén hatások következtében térben és időben is dinamikusan változnak, ezért védelmük és megfigyelésük napjainkra igen fontos kutatási területté nőtte ki magát. A műholdas távérzékelés nagyobb területek egyidejű megfigyelését teszi lehetővé, azonban érzékeny a felhőzetre és a légköri hatásokra, bizonytalanságot okozva ezzel az eredményekben. A hagyományos monitoring technológiák mellett a pilóta nélküli légi járművek térnyerése egyre kifejezettebb, köszönhetően rugalmasságának, hatékonyságának és alacsony költségének, miközben nagy térbeli és időbeli felbontású, szisztematikus adatszolgáltatásra képes. Tanulmányunk a pilóta nélküli légi járművek alkalmazási lehetőségeibe nyújt betekintést a vizes élőhelyek felmérésében, valamint áttekinti és összehasonlítja az egyéb távérzékelés technológiák alkalmazhatóságát ezen területek megfigyelésében. Célja, hogy elősegítse a dróntechnológia további terjedését és széles körű alkalmazását a vizes élőhelyek monitorozásában.
Abstract
In this work, an assessment of effective solvents and extraction methods was carried out to recover the bioactive compounds from hawthorn fruit (Crataegus monogyna Jacq.). Extractions assisted by heat, microwave, and ultrasound were carried out using various organic solvents (methanol, ethanol, and isopropanol). pH differential, Folin–Ciocalteu's, and aluminum chloride methods were used to determine total monomeric anthocyanin (TMA), total phenolic compound (TPC), and total flavonoid content (TFC), consecutively. Ferric Reducing Antioxidant Power (FRAP), 2,2-Diphenyl-1-picrylhydrazyl Hydrate (DPPH), and 2,2′- azino- bis (3-ethylbenzothiazoline-6- sulfonic acid) (ABTS) assays were used to measure the antioxidant activity (AA) of the extracts. The outputs revealed that extraction methods and solvents significantly affect anthocyanin concentration, TPC, TFC, AA, and color values of hawthorn fruit extracts. Due to the highest recovered TMA (0.152 ± 0.002 mg ECy3Gl/g of dry weight), TPC (49.14 ± 0.38 mg gallic acid equivalents/g of dry weight), and TFC (18.38 ± 0.19 mg quercetin equivalents/g of dry weight) contents, the ultrasonic-assisted extraction is superior to heat and microwave-assisted extractions. Accordingly, it was also observed that the methanol solvent is more profound than ethanol and isopropanol. Further, the bioactive compounds' content and the extracts' antioxidant activity are shown to be highly correlated. Thus, hawthorn extracts are considered to have antioxidant properties because of their concentrated bioactive compounds.
Abstract
Venetoclax is the first oral Bcl-2 inhibitor with high affinity targeting tumor cell apoptosis mechanism. In this study we developed a simple, sensitive and reliable LC–MS/MS method to determine venetoclax in children's hemolytic or lipemic samples. The method utilized an electrospray ion source and operated in multiple reaction monitoring mode. Venetoclax-d8 was used as an internal standard. Plasma samples were precipitated by acetonitrile containing 10% dimethyl sulfoxide and were separated by a Hypersil GOLD column (2.1 mm × 150 mm, 5 μm). The mobile phase consisted of acetonitrile-2 mM ammonium acetate (30:70, v/v) containing 0.4% formic acid. The quantification for venetoclax and venetoclax-d8 were m/z 868.1 → 636.1, m/z 876.1 → 644.1, respectively. The linear range was 10–2,000 ng mL−1 for venetoclax. The matrix in normal plasma, hemolytic or lipemic plasma had no significant effect on the detection results. The specificity, recovery and stability also met the acceptance criteria of guiding principles for the validation of biological sample quantitative analysis presented in the Chinese Pharmacopoeia (2015). As a result, this method is particularly suitable for determining venetoclax in hemolytic or lipemic samples from children with acute myeloid leukemia. The method, with the application of monitoring drug concentrations in pediatric patients, was successful.
Abstract
Due to the relative independence from the operational parameters, the linear retention indices (LRIs) are useful tool in gas chromatography-mass spectrometry (GC-MS) qualitative analysis. The aim of the current study was to develop a multiple linear regression (MLR) model for the prediction of LRIs as a function of selected molecular descriptors. Liquid injection GC-MS was used for the analysis of Essential oils (Rose, Lavender and Peppermint) separating the ingredients by a semi-standard non-polar stationary phase. As a result, a sum of 103 compounds were identified and their experimental LRIs were derived relying on reference measurements of a standard mixture of n-alkanes (from C8 to C20). As a next step, a set of molecular descriptors was generated for the distinguished chemical structures. Further, a stepwise MLR was applied for the selection of the significant descriptors (variables) which can be used to predict the LRIs. From an exploit set of over 2000 molecular descriptors, it was found that only 16 can be regarded as significant and independent variables. At this point split validation was applied: the identified compounds were randomly divided into training (85%) and validation (15%) sets. The training set (87 compounds) was used to derive two MLR models by applying i) the ‘enter’ algorithm (R 2 = 0.9960, RMSЕ = 17) and ii) the ‘stepwise’ one (R 2 = 0.9958, RMSЕ = 17). The predictive power was assessed by the validation set (16 compounds) as follows i) q2 F1 = 0.9896, RMSE = 25 and ii) q2 F1 = 0.9886, RMSE = 26, respectively. The adequateness of both regression approaches was further evaluated. Newly developed headspace-solid phase microextraction (HS-SPME) procedures in combination with GC-MS were used for an alternative analysis of the studied Essential oils. Twelve additional compounds, not previously detected by the liquid sample introduction mode of analysis, were identified for which the values of the significant descriptors were within the working range of the developed MLRs. For the last compounds, the LRIs were calculated and the experimental data was used as an external set for assessment of the regression models. The predictive power for both regression approaches was assessed as follows: Enter RMSE = 41, q2 F2 = 0.9503 and Stepwise RMSE = 40, q2 F2 = 0.9521.
Abstract
Monitoring benzoylphenylureas (BPUs) residues in ready-to-eat vegetables is of great interest for an adequate assessment of human pesticide exposure. A rapid, inexpensive, simple, and effective method for determining 8 BPUs insecticides in tomatoes and cucumbers was developed and validated. Vortex-assisted liquid-liquid extraction (VA-LLE) followed by dispersive solid-phase extraction (d-SPE) using graphitized carbon black (GCB) for cleanup was used before LC-MS/MS analysis. Different parameters were optimized, including the type and volume of extractants, vortex time, and the type and amount of adsorbents used for cleanup. The evaluation showed that the method has excellent linearity (R 2 ≥ 0.994). The recovered 8 BPUs insecticides from spiked tomato and cucumber samples at 0.01, 0.05, and 0.25 mg kg−1 ranged from 83.2 to 105.2%, with RSD of 4.9–14.6%. The limits of quantitation (LOQs) were 0.0025 mg kg−1 (0.005 mg kg−1 for lufenuron). Within-day repeatability ranged from 3.9 to 13.9%, while between-day repeatability ranged from 8.9% to 17.7%. The optimized method was used to analyze 100 samples of tomatoes and cucumbers marketed in Saudi Arabia.
