ABSTRACT Simultaneous determination of a tandem of drugs like perindopril and rosuvastatin with differences in water and organic solvent solubilities, hydrophobicity, polarities, and UV‐absorbing possibilities between them necessitates careful selection of chromatographic conditions. The four specified and different bonded reversed‐phase columns were tested with running mobile phases containing various composition contents concepts; the concept of using diluted trifluoroacetic acid in mobile phase composition with acetonitrile enabled simultaneous acidification and weak ion‐pairing with protonized molecules of analytes, yielding appropriate, short, reasonable run times and resolutions of analytes, satisfying UV‐transparency, and good peak symmetries. These facts especially stand for the peak of perindopril, as a member of the group of proline‐containing moiety in its structure, often and easily prone to peak‐tailing, skewing, or splitting on the high‐performance liquid chromatography chromatograms, which is usually solved by using alkyl‐sulfonate base and ion pairs on higher concentrations of buffering salts with low pH values and with column temperatures increasing by 50°C–60°C. Linearity range was 0.002/004–0.5 mg/mL. The score for method AGREE was 0.73–0.77. The method development approaches, with all columns employing our concepts in mobile phases and experimental conditions, can cover the complete needs and demands of quality control departments and laboratories as simple high‐throughput analysis methods.

Abstract Microwave‐assisted extraction (MAE) of cannabinoids from hemp tea was optimized, for the first, using response surface methodology. The effect of temperature (50, 65, and 80°C), irradiation time (4, 7, and 10 min), and solvent‐to‐solid ratio (20, 30, and 40 mL of methanol/g of hemp tea) on cannabinoid extractability were investigated. The concentrations of five cannabinoids, namely Δ 9 ‐tetrahydrocannabinol (Δ 9 ‐THC), cannabidiol (CBD), cannabigerol (CBG), cannabichromene (CBC), and cannabinol (CBN), were selected as response variables. For the quantitative analysis, a liquid chromatography‐mass spectrometry method was developed and validated. The proposed analytical approach demonstrated satisfactory performance characteristics in terms of linearity (R 2 ≥ 0.9998), precision (intra‐day: 1.99%–5.97% relative standard deviation [%RSD], inter‐day: 1.95%–6.08%RSD), sensitivity (limit of detection: 1.35–2.36 ng/g, limit of quantification: 4.05–7.08 ng/g) and carry‐over effect (signals ≤ 5.03%), with all cannabinoids eluting within 6 min. For comparison purposes, soxhlet extraction, ultrasound‐assisted extraction (UAE), and conventional‐stirring extraction were additionally performed. MAE proved to be a more effective technique for the extraction of CBD and CBN, while UAE managed to extract Δ 9 ‐THC, CBG, and CBC at higher concentration levels.

Abstract Neonicotinoids (NEOs), highly selective toward insect nicotinic acetylcholine receptors, are extensively used due to their effectiveness against pests and relative non‐toxicity to vertebrates. However, their prolonged persistence in soil and water has led to frequent detection in food and environmental samples, posing significant environmental and health concerns. Recent research indicates these pesticides infiltrate aquatic ecosystems, threatening aquatic life and human health. Here, we improved the ultra‐performance liquid chromatography‐mass spectrometry method for detecting NEOs in water samples, increasing its sensitivity to fulfill forthcoming detection needs. This approach enables the simultaneous quantification of eight NEOs and five NEO metabolites in diverse water sources, including tap, surface, groundwater, sewage, and seawater. Our method achieves remarkably low detection limits for direct injection (0.78–1.7 ng/L) and solid‐phase extraction methods (0.13–0.25 ng/L). Critically, our findings reveal that boiling domestic drinking water doesn't degrade NEOs; instead, it increases their concentration due to water evaporation. A 6‐min boiling period can amplify pesticide concentration by 4–5 times, presenting a significant hazard in culinary practices of specific regions where prolonged cooking could lead to alarmingly high levels of these insecticides. This research underscores the importance of monitoring and mitigating NEO contamination in water sources to safeguard environmental and public health.

Abstract Taibai ginseng (roots of Pedicularis decora Franch.) has been reported to possess anti‐Alzheimer's disease (anti‐AD) activity and can be potentially used for treating AD. However, the chemical constituents of taibai ginseng have not yet been elucidated because of the paucity of relevant studies, which hinders further research on the pharmacological mechanism and utilization of taibai ginseng. In this study, a rapid and efficient method for comprehensively analyzing the chemical constituents of taibai ginseng was established for the first time. We used ultra‐high performance liquid chromatography‐quadrupole time of flight mass spectrometry in combination with the UNIFI data‐processing platform to automatically characterize and identify the chemical profile of taibai ginseng. As a result, more than 76 compounds were detected, and their structures were characterized. These compounds include 24 iridoid glycosides, 24 phenylethanol glycosides, 15 terpenoids, and 13 other components. More than fifty of these compounds from taibai ginseng were reported for the first time. Our results provide a reference for the quality control of taibai ginseng and establish a higher quality standard for pharmacodynamic research. Appropriate modification of the method reported herein can enable its use for the screening and characterization of taibai ginseng and other compounds from the Pedicularis genus.

Abstract The present research aimed to comprehensively investigate the forced degradation of tepotinib through a combined in‐silico and experimental analysis. Tepotinib is a recently approved drug for metastatic non‐small cell lung cancer. A short and precise ultra‐high‐performance liquid chromatography (UHPLC) method utilizing a CSH C18 column (100 × 2.1 mm, 1.7 μm) was developed, using a mobile phase A as 0.1% formic acid and mobile phase B as HPLC‐grade acetonitrile. The flow rate was set at 0.2 mL/min, and detection was carried out at 260 nm. Forced degradation was carried out under acidic, basic, oxidative, and photolytic environments and also virtually with Zeneth software. Structural characterization of degradation products (DPs) was carried out using hyphenated techniques such as LC‐quadrupole time‐of‐flight‐tandem mass spectrometry in positive electrospray ionization mode. Further, toxicity was assessed with Derek and Sarah software. Analysis revealed the formation of five distinct forced DPs: DP‐1 ( m/z 511), DP‐2 ( m/z 527), DP‐3 ( m/z 525), DP‐4 ( m/z 512), and DP‐5 ( m/z 509) under experimental conditions and eight in Zeneth prediction. Furthermore, nephrotoxicity alerts were observed for DP‐3 and DP‐5, whereas DP‐3 also showed mutagenicity alerts. This integrated blend of in‐silico and real experimental analyses was found to be effective in quality control for routing monitoring of degradation products of tepotinib.

Abstract In the present study, a comprehensive strategy based on substances profiling in vivo and network pharmacology method was applied to screen out the potential immunomodulatory activity substances and mechanism of Wu Shen Wan. As a result, a total of 121 constituents were identified or tentatively characterized, including 26 flavonoids, 16 alkaloids, 10 tanshinones, four diterpenes, seven iridoid glycosides, eight coumarin, 18 phenolic acids, 29 ginsenosides, and three others. Moreover, 57 prototypes were clearly screened out in rat plasma and urine after ingestion of Wu Shen Wan. The Wu Shen Wan exhibited immunomodulatory effects via significantly increasing the phagocytic activity of macrophages and inducing the release of nitric oxide, tumor necrosis factor‐α, and interleukin 6 in RAW264.7 cells. In addition, the network pharmacology results showed that the top 20 Kyoto Encyclopedia of Genes and Genomes clusters were enriched, such as mitogen‐activated protein kinases pathway. This is the first systematic study on the chemical constituents of Wu Shen Wan. The analytical method features a quick and comprehensive dissection of the chemical composition and provides a basis for exploring its immunomodulatory effects.

Abstract A simple, accurate, and precise method is described for stability indicating a high‐performance thin‐layer chromatographic (HPTLC) method for development and validation in the pharmaceutical dosage form. The method was based on HPTLC separation of the drug by measurement of the spot at 478 nm. Separation was carried out on silica gel 60GF254 by using mobile phase methanol:toluene:acetic acid (3:7:0.1, v/v/v). The linearity range was between 500–3000 ng/spot with a coefficient of determination 0.999, respectively. The retardation value found was 0.55 ± 0.02 and the % recovery was found to be 100.610 ± 0.035%–101.0178 ± 0.035%. The limit of detection value for Rifapentine was 92.901 ng/spot and the limit of quantitation for Rifapentine was found to be 281.52 ng/spot. Forced degradation studies were carried out under various conditions. In acidic conditions, the % degradation was found to be 20.07%. In alkaline and oxidative conditions, the % degradation was found to be 61.27% and 11.12%. Photolytic and thermal conditions the % degradation was found to be 49.75% and 8.35%. Maximum degradation was found in alkaline condition with 61.27%, an assay for the marketed formulation was carried out and the amount of drug was found to be 149 ± 0.05 mg with a % of 99.25% ± 0.005%.