Perampanel (PER) is the first clinically available selective antagonist of α-amino-3-hydroxy-5-methylisoxazole-4-propionic acid (AMPA) receptor approved globally for the treatment of epilepsy. Studies have recently underlined the significant association between dose-exposure-effect-adverse events of PER in patients with epilepsy, so the therapeutic drug monitoring (TDM) of PER is critical in clinical practices, especially for pediatric patients with drug-resistant epilepsy. Due to several limits in previous published analytical methods, herein, we describe the development and validation of a novel liquid chromatography tandem mass spectrometry (LC-MS/MS) method for monitoring PER in human plasma samples. Protein precipitation method by acetonitrile containing PER-d5 as internal standard was applied for the sample clean-up. Formic acid (FA, 0.2 mM) in both aqueous water and acetonitrile were used as the mobile phases and the analyte was separated by an isocratic elution. Qualification and quantification were performed under positive electrospray ionization (ESI) mode using the m/z 350.3 → 219.1 and 355.3 → 220.0 ions pairs transitions for PER and PER-d5, respectively. Potential co-medicated anti-seizure medications (ASMs) have no interference to the analysis. Calibration curves were linear in the concentration range of 1.00–2,000 ng mL−1 for PER. The intra- and inter-batch precision, accuracy, recovery, dilution integrity, and stability of the method were all within the acceptable criteria and no matrix effect or carryover was found. This method was then successfully implemented on the TDM of PER in Chinese children with drug-resistant epilepsy. We firstly confirmed the apparent inter- and intra-individual PER concentration variabilities and potential drug-drug interactions between PER and several concomitant ASMs occurred in Chinese pediatric patients, which were also in line with previous studies in patients of other race.
Gluten-free (GF) breads are often described with low quality, rapidly staling, dry mouthfeel and crumbling texture attributes. In lack of recent texture profile data on commercially available, preservative-free, freshly-baked GF bread, this study aimed to compare different types of GF products with their wheat-based counterparts during a 4-day-long storage test. Texture analysis data showed that GF loaves performed better than or comparable to the wheat-based ones in hardness, springiness and cohesiveness. Among sensorial properties mouth-feel, softness and aroma were evaluated as significantly better or similar for GF versus wheat-based products. GF cob had a saltier taste, which reduced the flavour experience. Both the texture results of the storage test and sensory data showed that the quality of GF bread products improved in recent years; they stayed comparable with their wheat-based counterparts even during a 4-day-long storage period.
The selectivity of the separation of five antihistamines has been investigated by TLC on silica gel 60 F254 and on aluminium oxide 60 F254 with a variety of mobile phases in horizontal chambers. The best separation selectivity and retention differences for the drugs on the two types of plate were obtained with the mobile phases chloroform–ethyl acetate, 1 + 1 (v/v), ethyl acetate, and butan-2-one–toluene, 7 + 3 (v/v).
The plates were visualized by illumination at l = 254 nm and by reaction with different reagents. The greatest detection sensitivity – 0.06 mg for cetirizine, 0.1 mg for chloropyramine, and 0.2 mg for antazoline, doxylamine, and ketotifene – was obtained by spraying with potassium iodoplatinate reagent.
Knowledge of the composition of an incorporated alloy is a precondition for avoiding polymetallism in subsequent prosthetic treatment, or detection of the cause of an allergic reaction attributed to a metallic component of the prosthesis restoration. The method proposed in this paper can be a very useful means of determining the presence of Ni–Cr or Co–Cr dental alloys, and, especially, beryllium in Ni–Cr alloys which, despite its toxicity, gives the alloy desirable properties. Nickel is also a well-known allergen. This paper reports an analytical procedure for detection and identification of cobalt-and nickel-based dental alloy components. The method involves anodic sampling, and separation and identification of the components by thin-layer chromatography on precoated microcrystalline cellulose layers. Computer-assisted optimization was used to choose the mobile-phase composition. Excellent detection and identification of nickel, chromium, cobalt, molybdenum, and beryllium, on the basis of different RF values and spot colors, was achieved after anodic sampling in-situ.
Microanodic dissolution of dental alloys enables intra-oral, in-situ, and almost non-destructive sampling of a permanent prosthesis restoration.
The object of this study was determination of the content and composition of the essential oil of the fruits of three varieties of stalk celery – Helios, Zefir, and Orient. We also investigated hexane extracts obtained from the fruits of two varieties of stalk celery – Helios and Zefir. The essential oils and the extracts were examined by TLC and GC–MS.
Analysis showed the presence of terpene (mono- and sesquiterpene) and non-terpene (phthalide) fractions in the oils and extracts investigated. The combined amount of limonene, α- and β-pinene and myrcene in the monoterpene fraction of the essential oils ranged from 79.1 to 82.9%. The amount of the sesquiterpene fraction (α-and β-selinene) was from 15.7% to 18.8%. The phthalide fraction (3-n-butylphthalide, dehydrosedanolide, and sedanolide) was found in trace amounts. The amounts of these fractions in the hexane extracts ranged from 40.2 to 43.6% for the monoterpene fraction, from 19.4 to 20.7% for the sesquiterpene fraction, and from 35.7 to 37.7% for the phthalide fraction.
The conditions used for TLC and HPTLC analysis of catechins have been optimized. Chemically modified stationary phases (HPTLC CN, HPTLC NH2, and HPTLC RP-18W) were used for qualitative examination of polyphenol fractions obtained by an SPE–RP 18 method from Uncaria tomentosa bark. Although the best separation of catechin from epicatechin was achieved on octadecyl plates, silica gel plates are good enough for preliminary investigations of crude plant extracts.
A high performance thin layer chromatographic method has been developed for the determination of idebenone in pharmaceutical preparations. The method uses silica gel 60 F254 as the stationary phase, toluene–diethyl ether–methanol–triethylamine, 4 + 4 + 1.5 + 0.5 (v/v) as mobile phase, and detection at λ = 279 nm, the wavelength of maximum absorption of idebenone. Diclofenac sodium was used as internal standard. The response was found to be linearly dependent on amount of idebenone between 100 and 1000 ng mL–1. The method was validated to determine its accuracy and precision and the repeatability of the method was also determined. System suitability tests were conducted to verify that the resolution and reproducibility of the chromatographic system are adequate for the analysis. The determination of idebenone in tablets is described.
A quantitative instrumental high-performance thin-layer chromatographic (HPTLC) method has been developed for assessment of the photodegradation of bensulfuron-methyl on silica gel. The method uses automated band application on to silica gel plates with fluorescent indicator, direct development after irradiation, and scanning densitometry of fluorescence-quenched zones of samples and standards. The accuracy of the analyses was confirmed by performing recovery studies with preanalyzed samples and a blank sample fortified with the analytes. Precision was determined by analyzing samples in replicate; loaded amounts of 500–2000 ng per spot were suggested for assessing the photodegradation of the pesticides. The simplicity of sample preparation and the chromatographic techniques, high sample throughput, high reproducibility, and the strong possibility of separating the photoproducts seem to make the test on HPTLC plates highly suitable for estimation of the photodegradability of pesticides in the adsorbed state.
Homologous series of higher fatty acids, higher alcohols, and methyl esters of higher fatty acids have been separated by RPTLC. The values of RM and of the log PRek partition coefficient from Rekker for the compounds of the homologous series could be correlated with numerical values of topological indexes based on the adjacency matrix (M, °χ, 1χ, °χν, 1χν), and on the distance matrix (W, A, °B,1B). The most accurate prediction of the RM and log PRek values of the compounds investigated was achieved by use of monoparametric equations containing one topological index based on the adjacency matrix.
Two-dimensional thin layer chromatography of twelve flavonoids and three phenolic acids from Betula sp. leaves has been performed in normal-phase systems. Plots showing the dependence of RM on modifier concentration in some non-aqueous systems were used to optimize the chromatographic separation. RM values were correlated for all the chromatographic systems investigated and optimum pairs of systems were then selected for use in two-dimensional TLC separations. Complete separation of the compounds investigated was achieved by use of two optimum non-aqueous mobile phases on silica plates.