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Abstract

Gas chromatography-ion mobility spectrometry (GC-IMS) is an emerging analytical technique that has the advantages of fast response, high sensitivity, simple operation, and low cost. The combination of the fast speed and resolution of GC with the high sensitivity of IMS makes GC-IMS play an important role in the detection of food volatile substances. This paper focuses on the basic principles and future development trend, and the comparative analysis of the functions, similarities and differences of GC-IMS, GC-MS and electronic nose in the detection of common volatile compounds. A comprehensive introduction to the main application of GC-IMS in food volatile components: fingerprint identification of sample differences and detection of characteristic compounds. On the basis of perfecting the spectral library, GC-IMS will have broad development prospects in food authentication, origin identification, process optimization and product classification, especially in the analysis and identification of trace volatile food flavor substances.

Open access

Abstract

A simple, rapid, and environmentally friendly sample preparation method for pyrethroids determination in cereals using cyclodextrin-assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplets coupled with high-performance liquid chromatography was established. The cereal samples were extracted with acetonitrile, cleaned up, and concentrated by green extractant menthol via γ-cyclodextrin assisted extraction process. The extractant menthol dispersed as fine droplets in the cyclodextrin solution and then solidified at room temperature for efficient extraction and convenient collection. The optimized method provided good linearity in the range of 0.01–10 mg kg−1 with limits of detection of 3.5–9.5 μg kg−1. The fortified recoveries of three pyrethroids (i.e., lambda-cyhalothrin, deltamethrin, and bifenthrin) in four cereals (i.e., rice, wheat, maize, and millet) at three levels were in the range of 77.6–101.6% with relative standard deviations of 0.6–6.6%. Overall, the proposed method can be successfully applied for the determination of pyrethroids in cereals.

Open access

Abstract

A systematic DoE and Analytical Quality by Design (AQbD) approach was utilized for the development and validation of a novel stability indicating high-performance thin–layer chromatographic (HPTLC) method for Rivaroxaban (RBN) estimation in bulk and marketed formulation. A D-optimal design was used to screen the effect of solvents, volume of solvents, time from spotting to development and time for development to scanning. ANOVA results and Pareto chart revealed that toluene, methanol, water and saturation time had an impact on retention time. The critical method and material attributes were further screened by Box-Behnken design (BBD) to achieve optimal chromatographic condition. A stress degradation study was carried out and structure of major alkaline degradant was elaborated. According to the design space, a control strategy was used with toluene: methanol: water (6:2:2) and the saturation time was 15 min. A retention factor (RF) of 0.59 ± 0.05 was achieved for RBN using chromatographic plate precoated with silica gel at detection wavelength 282 nm with optimized conditions. The linear calibration curve was achieved in the concentration range of 200–1,200 ng/band with r 2 > 0.998 suggesting good coordination between analyte concentration and peak areas. The quadratic model was demonstrated as the best fit model and no interaction was noted between CMAs. The optimized HPTLC method was validated critically as stated in International Conference on Harmonization (ICH) Q2 (R1) guideline and implemented successfully for stress degradation study of RBN. The developed HPTLC method obtained through AQbD application was potentially able to resolve all degradants of RBN achieved through forced degradation study. The obtained results demonstrate that a scientific AQbD approach implementation in HPTLC method development and stress degradation study drastically minimizes the number of trials in experiments, ultimately time and cost of analysis could be minimized.

Open access

Abstract

Bicalutamide (BCL) has been approved for treatment of advanced prostate cancer (Pca), and vitamin D is inevitably used in combination with BCL in Pca patients for skeletal or anti-tumor strategies. Therefore, it is necessary to study the effect of vitamin D application on the pharmacokinetics of BCL.

We developed and validated a specific, sensitive and rapid UHPLC–MS/MS method to investigate the pharmacokinetic behaviours of BCL in rat plasma with and without the combined use of vitamin D. Plasma samples were extracted by protein precipitation with ether/dichloromethane (2:1 v/v), and the analytes were separated by a Kinetex Biphenyl 100A column (2.1 × 100 mm, 2.6 μm) with a mobile phase composed of 0.5 mM ammonium acetate (PH 6.5) in water (A) and acetonitrile (B) in a ratio of A:B = 35:65 (v/v). Analysis of the ions was run in the multiple reactions monitoring (MRM) mode. The linear range of BCL was 5–2000 ng mL−1. The intra- and inter-day precision were less than 14%, and the accuracy was in the range of 94.4–107.1%. The mean extraction recoveries, matrix effects and stabilities were acceptable for this method. The validated method was successfully applied to evaluate the pharmacokinetic behaviours of BCL in rat plasma. The results demonstrated that the pharmacokinetic property of BCL is significantly affected by combined use of vitamin D, which might help provide useful evidence for the clinical therapy and further pharmacokinetic study.

Open access

Abstract

Several studies on the pharmacokinetic parameters of antidementia drugs have reported that plasma concentration is linked to the drugs’ efficacy and adverse effects. At present, there is no quantitation method that is highly sensitive and can be applied to simultaneous monitoring of the pharmacokinetics of rivastigmine and its metabolites (NAP 226-90) in rat plasma. No methods fulfilling the assay validation requirements of the US Food and Drug Administration and the European Medicines Agency was also established. Therefore, this study developed a quantitative method for measuring rivastigmine and NAP 226-90 concentrations using high-performance liquid chromatography and tandem mass spectrometry, examining plasma samples after rivastigmine administration. Rat plasma samples were prepared via the protein precipitation method. The methods for measuring rivastigmine and NAP 226-90 concentrations showed good fit over wide ranges of 1–100 ng mL−1 and 0.5–50 ng mL−1, with lower limits of quantification at 1 ng mL−1 and 0.5 ng mL−1, respectively. The plasma concentrations of rivastigmine and NAP 226-90 in six healthy rats were successfully determined, demonstrating the feasibility of applying the developed method. Thus, this research has successfully developed a sensitive, selective method, to simultaneously quantify rivastigmine and NAP 226-90 concentrations in rat plasma and be applicable to a pharmacokinetic study.

Open access

Abstract

A sensitive and accurate LC-MS/MS method was developed and validated for the simultaneous quantification of rivaroxaban (RIV) and sitagliptin (SIT) in rat plasma using apixaban as internal standard (IS). An Agilent Eclipse plus C18 column (2.1 × 100 mm, 3.5 µm, Agilent) was used for chromatographic separation with isocratic elution. Multiple reaction monitoring (MRM) using positive-ion ESI mode to monitor ion transitions of m/z 436.8→144.9 for RIV, m/z 407.7→173.8 for SIT, m/z 459.8→442.8 for IS. The procedure of method validation included selectivity, linearity, precision, accuracy, matrix effect, extraction recovery and stability were conducted according to the guidelines of EMA and FDA. The results indicated that no obvious drug-drug interactions occurred might be owing to their differences in metabolic pathways.

Open access

Abstract

A rapid, simple and efficient ultra-performance liquid chromatography-electrospray ionization-tandem mass spectrometry (UPLC-ESI-MS/MS) method was established to simultaneous determination of shikonin, isobutyryl shikonin, β, βʹ-dimethylacryl alkanin in beagle plasma and evaluated by using esculetin as internal standard. The electrospray ionization (ESI) source was operated in negative ionization mode. Multi-reaction monitoring (MRM) was used to quantitatively analyzed shikonin m/z 287.0 → 217.9, isobutyryl shikonin m/z 357.0 → 268.9, β, βʹ-dimethylacryl alkanin m/z 370.0 → 270.1 and esculetin m/z 177.0 → 89.0, respectively. The method was validated for selectivity, linearity, lower limit of quantification, precision, accuracy, recovery, matrix effect and stability. All validation parameters met the acceptance criteria according to regulatory guidelines. This method was successfully applied for the pharmacokinetic study of shikonin, isobutyryl shikonin, β, βʹ-dimethylacryl alkanin in beagle dogs plasma after oral administration of A. euchroma extract.

Open access
Agrokémia és Talajtan
Authors: Birkás Márta, Balla István, Gyuricza Csaba, Kende Zoltán, Kovács Gergő Péter, and Percze Attila

A magyar talajművelésben a kezdetektől az 1900-as évek közepéig a hagyományos szántásos rendszerek domináltak. Az ekék tökéletesedése révén a mélyebb szántások hozzájárultak a talajminőség romlásához.

Az 1900-as évek első évtizedeiben a külföldön kidolgozott művelési módszerek még kevesek érdeklődését keltették fel, azonban a szántásnál kedvezőbb körülmények létrehozása érdemi figyelmet keltett.

Az 1970-es évektől a talajvédő művelés Magyarországon is kedvező fogadtatásra talált. Kísérletekkel igazolódott, hogy a direktvetés előnyei – folyamatosság esetén – a hatodik-hetedik évtől észlelhetők. A mulcshagyó művelés kultivátor alkalmazása esetén rövidebb idő alatt nyújtotta a várt talajvédelmi előnyöket, ennek tudható be a gyorsabb terjedése. A kultivátoros művelés értékét a felszínvédő mulcshagyás, a talajminőség megóvás és a biológiailag aktív talaj erősítette meg.

Az időjáráshoz kapcsolható szélsőségek megjelenése az 1980-as évektől újabb művelési megoldások felé fordították a figyelmet. A talajlazítás a vízbefogadás és tárolás, a mulcshagyás, valamint a növények mélyebb gyökerezése révén került a korábbinál szélesebb körű alkalmazásra. A sávos művelési rendszer a nemzetközileg bizonyított eredmények hátterével számos magyar gazdálkodónál is sikeressé vált.

A magyar talajművelés előrehaladásában a talajközpontú szemlélet kiszélesedése, a növényközpontú szemlélet felváltása révén eredményezett kedvező változásokat a talajállapot javulásában.

Tekintettel a talajok sokféleségére és a talajállapot eltéréseire, jelenleg a termőhelyhez, talajhoz adaptált művelési rendszer alkalmazása látszik eredményesnek. Az időjárási szélsőségek fokozódása általában és adott termőhelyen is rangsorba állítja a lehetséges módszereket. A korábban jónak tartott megoldások, beleértve a szántást, ugyanis már egyre kevésbé biztonságosak.

A talajkímélő művelés iránti érdeklődés közel százhúsz évre tekint vissza Magyarországon. Sajátos, de az előrehaladás és a visszatartás tényezői a talajművelésben párhuzamosan jelentek meg az eltelt évek alatt. A művelési előrehaladást visszafogó tényezők között a sok évtized óta fennálló hiedelmek voltak a leginkább hátráltatók, mivel figyelmen kívül maradt a talajvédelem, továbbá a klímaváltozással kapcsolatos veszélyek enyhítésének igénye. Az előrehaladást a talajvédelem felvállalása, a gazdálkodási színvonal emelésének esélye és a klímakár csökkentés kényszere mozdította elő. Az előrehaladást alátámasztó tényezők között legfontosabbak a talajállapot tartós javulása és a klíma eredetű károk enyhítése, továbbá a termés biztonság megtartása és javulása.

Open access

Abstract

As the world is facing numerous global ecological issues at once, the question arises of what will help mitigate and solve contemporary matters related to resource management or climate change without devastating the economies. Fortunately, the widespread application of the circular economy would help countries worldwide simultaneously ensure economic growth without significant environmental deterioration, essentially decoupling the two factors. While Hungary’s contribution to environmental problems is not significant in absolute terms, the economic sector’s circular transition could help the country decrease its impact in relative terms and pave the path for a green economy. Nevertheless, companies, especially SMEs, tend to struggle the most with the initial phases of the shift thus it is crucial to assess the factors that prevent and support their transition.

Open access

Abstract

This study establishes a method for rapid detection of clonidine and cyproheptadine in foods of animal origin. In order to obtain the best detection method, capillary zone electrophoresis (CZE), large volume sample stacking (LVSS), and sweeping-micellar electrokinetic capillary chromatography (sweeping-MEKC) were used respectively. The limits of detection (LODs) of clonidine and cyproheptadine by LVSS-CZE were 0.028 μg mL−1 and 0.034 μg mL−1, and those by sweeping-MEKC were 0.023 μg mL−1 and 0.031 μg mL−1, respectively. Compared with the CZE method, the two online pre-concentration technologies have greatly improved the detection sensitivity and achieved good enrichment results. However, compared with the sweeping-MEKC system, the LVSS system consumed a longer time and was greatly affected by the actual sample matrix. The sweeping-MEKC method was proved to be suitable for real sample analysis. Under the best sweeping-MEKC conditions, clonidine and cyproheptadine could be well separated within 8 min and good linear relationships in the range of 0.1–1.0 μg mL−1 (r 2 > 0.99) were obtained. This method was successfully applied to the determination of clonidine and cyproheptadine in animal-derived foods with the recoveries of 82.3%–90.1% and the relative standard deviations (RSDs) less than 3.11%. The sweeping-MEKC method is simple to operate and has great potential in the rapid detection of clonidine and cyproheptadine in animal-derived foods.

Open access