Journal of Analytical Methods in Chemistry最新文献

Cirsium japonicum, a traditional medicinal plant, has been widely used for its therapeutic properties in treating various ailments. However, a comprehensive analysis of its chemical composition remains limited, hindering a full understanding of its chemical basis and pharmacological activities. This study aims to identify and characterize the chemical constituents of C. japonicum using ultra-high-performance liquid chromatography coupled with quadrupole-Orbitrap mass spectrometry (UHPLC-Q-Exactive Orbitrap MS) and parallel reaction monitoring (PRM). A total of 94 compounds were identified, including 57 organic acids, 25 flavonoids, 3 phenylpropanoids, and 9 other components, with chlorogenic acid dominating the organic acid fraction. Organic acids and caffeic acid, among organic acid compounds, exhibit hemostatic effects based on prior evidence. The UHPLC-Q-Exactive Orbitrap MS-based approach provided a detailed chemical profile of C. japonicum, which could facilitate a deeper understanding of its medicinal properties and guide future pharmacological studies. The identified compounds can be used as potential biomarkers for the standardization and quality control of medicinal products of C. japonicum.

Considering the economic and edible values of sesame seeds, it is important to monitor sesame seed for the safety of consumers and for international trade as it helps the country government and suppliers as products to gain market acceptance more effectively. The objective of this study was to determine selected organochlorine pesticide (OCP) residues in sesame seeds. Quick, easy, cheap, efficient, rugged, and safe method followed by gas chromatography coupled with tandem mass spectrometry (GC-MS/MS) was used for the rapid separation and determination of 20 OCPs in sesame seeds. Acetonitrile in combination with 1% glacial acetic acid was used as an extraction solvent. Primary secondary amine, graphitized carbon black, and octadecylsilane in QuEChERS kit were used for d-SPE clean up before GC-MS/MS analysis. The GC-MS/MS analysis was evaluated in terms of linearity, recovery, and precision. The calibration curves were obtained for all analytes and displayed good linearity over the selected concentration range with regression coefficients (r ²) ≥ 0.999. The recoveries for spiked analytes in sesame seed samples were ranged from 93.58 to 115.81 with RSDs lower than 1%. The LOD and LOQ for all investigated pesticides were in the range of 0.05-0.88 μg/kg and from 0.16 to 2.93 μg/kg, respectively.

[This corrects the article DOI: 10.1155/jamc/6883692.].

Pandanus tectorius fruits are a promising but underutilized source of bioactive constituents. We optimized extraction conditions for phenolic- and saponin-enriched fractions using Box-Behnken/response surface methodology across ethanol concentration, temperature, solvent-to-material ratio, and time and then evaluated antioxidant and anti-inflammatory activities. Total phenolic content (TPC; Folin-Ciocalteu, 760 nm) and total saponin content (TSC; vanillin-sulfuric acid, 560 nm) served as responses for model fitting (R ² > 0.96), validation, and multiresponse optimization that yielded seven distinct optimums targeting different extract profiles. Phenolic-rich extracts showed potent DPPH and hydroxyl radical scavenging, whereas saponin-rich extracts more strongly inhibited LPS-induced nitric oxide in RAW 264.7 cells; excessive saponin enrichment, however, coincided with cytotoxicity. These results demonstrate that tuned extraction can deliver purpose-built extracts for antioxidant or anti-inflammatory applications, supporting the valorization of P. tectorius as a natural source for functional and nutraceutical ingredients.

Fagopyri Dibotryis Rhizoma (FDR), the dried rhizome of Fagopyrum dibotrys (D. Don) Hara (F. dibotrys), is a famous herbal drug with a long application history in China. Recently, FDR and its preparations have attracted wide attention due to their therapeutic values for coronavirus disease 2019 (COVID-19) and COVID-19-related acute lung injury. There is a significant difference in quality among FDRs from different habitats, which can seriously affect the clinical efficacy. The original medicinal materials can only be used in the clinic after being processed into decoction pieces, but there is currently a lack of comprehensive quality evaluation of FDR decoction pieces prepared using FDRs from different origins. In this study, the HPLC fingerprints of 23 batches of FDR decoction pieces prepared using FDRs from 8 provinces such as Yunnan and Guizhou in China were established; 47 common peaks in these fingerprints were marked, among which, 80 components were identified by Q-TOF-MS/MS, including 32 tannins, 17 phenols, 12 flavonoids, 11 phenylpropanoid glycosides, 3 amino acids, 2 organic acids, 1 terpenoid, 1 alkaloid, and 1 other component; the chemical pattern recognition analysis, including hierarchical cluster analysis, principal component analysis, and orthogonal partial least squares discriminant analysis, was conducted by using the quantified peak areas of the common peaks as variables; and the contents of 4 tannins such as procyanidin B1, procyanidin B3, procyanidin C1, and procyanidin A2, 3 phenolics such as gallic acid, protocatechuic acid, and protocatechualdehyde, and 3 flavonoids such as catechin, epicatechin, and epicatechin gallate were determined in 23 batches of FDR decoction pieces. The results indicate that there is a significant difference in the quality between the decoction pieces prepared using FDRs from Yunnan and Guizhou and those prepared using FDRs from 6 other provinces, and the former have a better quality compared with the latter.

Soil metabolites are not only the integrated expression of soil biological activities but also the pivotal drivers of biogeochemical cycling, thereby significantly influencing the formation of crop quality. This study established an improved ultra-performance liquid chromatography (UPLC) fingerprint with chemometrics for characterizing the nonvolatile metabolite profiles of soils from geographical locations defined by different tobacco flavor styles in Guizhou. The homogenization extraction and then UPLC analysis were selected as the optimal system due to their superior repeatability and reproducibility, with intraday and interday RSD% of the common peaks (retention time and peak area) below 2.75%. The fingerprint profiling was established using 18 soil samples from three locations, namely the honey-sweet region I, II, and the fresh-sweet region. Thirty common peaks were identified, with similarities ranging from 0.809 to 0.956. Then, the common peaks were subjected to chemometrics analysis. These results indicated that significant differences were observed by principal component analysis (PCA), and 17 characteristic metabolites were viewed as primarily discriminatory by partial least squares discriminant analysis (PLS-DA). The total content of characteristic metabolites followed a trend of honey-sweet region II > honey-sweet region I > fresh-sweet region, with individual metabolites generally higher in the honey-sweet region. Finally, external validation using the hierarchical cluster analysis (HCA) and Fisher discriminant analysis (FDA) model accurately classified four soil samples, further confirming the representativeness of the characteristic metabolites. This study supplies a theoretical foundation to understand the relationship between tobacco flavor formation and soil metabolism, showing great potential applications in agricultural research.

This study developed a method for simultaneously detecting 10 mycotoxins in Dendrobium officinale using the QuEChERS technique combined with ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The method was optimized for sample purification, pretreatment, chromatographic conditions, and mass spectrometric settings. It effectively addressed the matrix effects from impurities like pigments and cellulose. The validation of the method showed good linearity (R ² > 0.990), with limits of detection (LODs) ranging from 0.23 to 8.61 μg kg^-1 and limits of quantification (LOQs) from 0.77 to 28.7 μg kg^-1. Average recoveries for the 10 mycotoxins ranged from 77.9% to 98.5%, with relative standard deviations (RSD) between 2.26% and 8.28%. The method demonstrated high accuracy, precision, and suitability for large-scale screening of mycotoxins in Dendrobium officinale. When applied to 84 samples, the contamination rate was 2.38%, with the main contaminants being AFB1, ZEN, and AFG1. This method provides a reliable, cost-effective approach for detecting mycotoxin contamination in traditional Chinese medicine.

Mango peel is one of the main byproducts in mango processing. In order to improve the utilization and added-value of mango peel, effects of the ultrasound-assisted enzymatic method on the extraction rate of mangiferin from mango peel were investigated by single-factor tests (enzyme addition amount, enzymolysis time, ethanol concentration, ultrasonic temperature, ultrasonic power, and ultrasonic time), and the extraction process was optimized by Box-Behnken response surface. The antioxidant activity and antidiabetic assay of mangiferin in vitro were studied. The results showed that enzymolysis time 44 min, enzyme addition amount 0.1%, ethanol concentration 70%, ultrasonic power 300 W, ultrasonic temperature 66°C, and ultrasonic time 45 min were the optimal extraction process parameters. Under these conditions, the extraction rate of mangiferin was 3.63% ± 0.04%, which was not significantly different from the model prediction value (3.71%), and it was 3.90 times and 1.78 times that of single cellulase and ultrasonic extraction, respectively. Within the test concentration range, the scavenging rate of mangiferin for DPPH·, ABTS⁺·, and O₂ ^-· increased with the increase of its mass concentration, and the EC₅₀ values were 0.03829 mg/mL, 0.06032 mg/mL, and 0.04949 mg/mL, respectively, which were slightly higher than those of Vc. Meanwhile, mangiferin exhibited inhibitory activity effects on α-amylase and α-glucosidase, with IC₅₀ values of 0.1952 and 0.08696 mg/mL, respectively. Results indicate that the mangiferin in mango peel had strong bioactivity. The study provides a theoretical reference for the efficient extraction of mangiferin from mango peel and provides a scientific basis for further realizing the high-value utilization of mango processing waste.

Lauraceae plants are diverse in species and rich in volatile components, which possess functions such as insect repellency, antioxidant activity, and antibacterial properties. However, currently, the methods for analyzing the volatile components of Lauraceae plants are relatively single. The essential oils are mainly extracted by steam distillation, but the pretreatment is relatively complex and cumbersome. Therefore, it is essential to find a simple and cost-effective method. By comparing different extraction methods, HS-SPME-GC-MS was selected as the optimal extraction condition. Regarding Head-space Solid-Phase Microextraction and Gas Chromatography-Mass Spectrometry (HS-SPME-GC-MS), single-factor condition optimization and response surface analysis were carried out for different fiber coatings, equilibrium time, extraction temperature, and extraction time. Eventually, 75-μm CAR/PDMS fiber head was chosen, with an equilibrium time of 15 min, and extraction was conducted at 70°C for 57 min as the optimal HS-SPME extraction conditions. Furthermore, a differential analysis of the volatile components of five Lauraceae plants from different genera was performed, and differential metabolites were screened out respectively. This can effectively separate Cinnamomum and Litsea from the other three genera, providing certain assistance for the chemotaxonomy of the volatile components of Lauraceae plants and the subsequent development of medicinal plant resources.

The fixed-dose combination (FDC) of ibuprofen (IBU) and paracetamol (PAR) has emerged as a preferred option in pain management, owing to its distinct practical advantages. Both drugs have well-documented efficacy and safety profiles, providing synergistic pain relief through complementary mechanisms of action. IBU not only offers central analgesic effects but also inhibits cyclooxygenase (COX) enzymes, particularly COX-1 and COX-2, thereby reducing prostaglandin synthesis at the site of pain to deliver both analgesic and anti-inflammatory benefits. Despite the growing use of this combination, a comprehensive review focusing on the analytical methods for its determination has not yet been published. This review aims to bridge that gap by presenting an extensive compilation of documented analytical methods for the quantification of IBU and PAR in both bulk and pharmaceutical formulations. It serves as a valuable resource for researchers and professionals seeking detailed insights into the diverse techniques employed for accurate and precise analysis of these FDCs. Through a systematic search of major scientific databases, including Science Direct, Springer Link, PubMed, Scopus, and Google Scholar, the review identifies the most commonly utilized methods, such as high-performance liquid chromatography (HPLC), gas chromatography (GC), high-performance thin-layer chromatography (HPTLC), ultraviolet (UV)/Visible spectrophotometry, Fourier-transform infrared spectroscopy (FTIR), and micellar electrokinetic chromatography (MEKC). Notably, HPLC and UV/Visible spectrophotometry were the most frequently reported, each accounting for 37.9% of studies. By consolidating these analytical approaches, this review highlights the state-of-the-art methodologies available for the determination of IBU/PAR FDCs and underscores its novel contribution as a definitive reference for future research and development in this field.