Among the plant's English names, Chinese magnolia vine is a key one. Asian medicine has relied on this treatment for millennia to combat a spectrum of ailments, encompassing chronic coughs, difficulty breathing, frequent urination, diarrhea, and the management of diabetes. Lignans, essential oils, triterpenoids, organic acids, polysaccharides, and sterols, along with numerous other bioactive constituents, contribute to this. On some occasions, the effectiveness of the plant's pharmacological properties is affected by these components. Within Schisandra chinensis, lignans possessing a dibenzocyclooctadiene-based structure are recognised as the prominent constituents and primary bioactive compounds. However, the compound complexity within Schisandra chinensis makes the extraction of lignans a process with significantly lower yields. Consequently, meticulous examination of pretreatment techniques in sample preparation is crucial for ensuring the quality of traditional Chinese medicine. Destruction, extraction, fractionation, and purification are fundamental components of the complete matrix solid-phase dispersion extraction method (MSPD). Effortlessly preparing liquid, viscous, semi-solid, and solid samples, the MSPD method stands out for its minimal sample and solvent requirements, while completely eliminating the need for specialized experimental equipment or instruments. The current study developed a method of matrix solid-phase dispersion extraction coupled with high-performance liquid chromatography (MSPD-HPLC) for the concurrent analysis of five lignans (schisandrol A, schisandrol B, deoxyschizandrin, schizandrin B, and schizandrin C) extracted from Schisandra chinensis. A gradient elution method, utilizing 0.1% (v/v) formic acid aqueous solution and acetonitrile as mobile phases, was employed to separate the target compounds on a C18 column; detection was performed at 250 nm. Evaluating the impact of 12 adsorbents, encompassing silica gel, acidic alumina, neutral alumina, alkaline alumina, Florisil, Diol, XAmide, Xion, along with inverse adsorbents C18, C18-ME, C18-G1, and C18-HC, was undertaken to investigate their effects on the extraction yield of lignans. The factors influencing the extraction yields of lignans included the mass of the adsorbent, the nature of the eluent, and the eluent's volume. Xion material was selected for the MSPD-HPLC method to analyze lignans present within Schisandra chinensis. The MSPD method's lignan extraction efficiency was maximized when using Schisandra chinensis powder (0.25 g), Xion (0.75 g) as the adsorbent, and methanol (15 mL) for elution. Schisandra chinensis lignans (five in total) were examined using newly developed analytical methods that resulted in excellent linearity (correlation coefficients (R²) consistently near 1.0000 for each analyte). In terms of detection and quantification limits, the former ranged from 0.00089 to 0.00294 g/mL and the latter ranged from 0.00267 to 0.00882 g/mL. The study examined lignans in three concentration categories: low, medium, and high. Recovery rates on average exhibited a range of 922% to 1112%, accompanied by relative standard deviations that fluctuated between 0.23% and 3.54%. Precision in both intra-day and inter-day contexts was demonstrably under 36%. LY2157299 cost MSPD excels over hot reflux extraction and ultrasonic extraction techniques by combining extraction and purification, leading to shorter processing times and reduced solvent usage. The optimized method was successfully deployed to analyze five lignans in Schisandra chinensis specimens from seventeen cultivation regions.
Newly prohibited substances are now frequently found as illicit ingredients in cosmetics. Clobetasol acetate, a novel glucocorticoid, falls outside the scope of current national standards and is structurally related to clobetasol propionate. Ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was employed to develop and implement a method for the analysis of clobetasol acetate, a novel glucocorticoid (GC), in cosmetic products. Five cosmetic matrices – creams, gels, clay masks, face masks, and lotions – exhibited suitability for this new method. The comparative study of pretreatment methods included direct acetonitrile extraction, PRiME pass-through column purification, solid-phase extraction (SPE), and QuEChERS purification methods. Further analysis was performed on the impact of diverse extraction efficiencies of the target compound, including factors like the solvents used in the extraction process and the time of extraction. The ion mode, cone voltage, and collision energy of ion pairs within the target compound were optimized using MS parameters. The target compound's chromatographic separation conditions and response intensities, across various mobile phases, were subject to comparison. The experimental data clearly supported direct extraction as the most effective method. Vortexing samples with acetonitrile, followed by ultrasonic extraction exceeding 30 minutes and filtration through a 0.22 µm organic Millipore filter, led to detection using UPLC-MS/MS. Gradient elution, using water and acetonitrile as the mobile phases, allowed for the separation of concentrated extracts on a Waters CORTECS C18 column (150 mm × 21 mm, 27 µm). The target compound was observed using electrospray ionization (ESI+), positive ion scanning, and multiple reaction monitoring (MRM) analysis. Quantitative analysis methodology involved the application of a matrix-matched standard curve. Given optimal conditions, the target compound exhibited a strong linear relationship in the concentration range of 0.09 to 3.7 grams per liter. Within these five various cosmetic matrices, the linear correlation coefficient (R²) exceeded 0.99; the method's quantification limit (LOQ) reached 0.009 g/g, and the detection threshold (LOD) was established at 0.003 g/g. The recovery test was performed at three spiked levels: 1, 2, and 10 times the limit of quantification (LOQ). In these five cosmetic matrices, the tested substance's recovery rate fell between 832% and 1032%, with relative standard deviations (RSDs, n=6) fluctuating between 14% and 56%. To screen cosmetic samples categorized by various matrix types, this method was utilized. Five positive samples were identified, with clobetasol acetate content fluctuating between 11 and 481 g/g. Ultimately, the method demonstrates simplicity, sensitivity, and reliability, proving suitable for high-throughput screening of cosmetic samples, whether qualitative or quantitative, and across diverse matrices. In addition, the process provides vital technical backing and a theoretical basis for creating viable detection criteria for clobetasol acetate in China, as well as for controlling it in cosmetic products. This method offers critical practical value for putting into action management plans to control unauthorized ingredients in cosmetics.
Antibiotics' pervasive and regular use in treating diseases and promoting animal growth has contributed to their persistence and accumulation in water, soil, and sedimentary layers. Antibiotic pollution, a newly emerging environmental concern, is currently a subject of intense research. Trace levels of antibiotics are a common occurrence in water ecosystems. Sadly, pinpointing the diverse types of antibiotics, each possessing unique physicochemical properties, proves a complex undertaking. Hence, the importance of developing pretreatment and analytical techniques to ensure rapid, precise, and sensitive analysis of these emerging contaminants in diverse water matrices is undeniable. Considering the characteristics of the screened antibiotics and the sample matrix, adjustments were made to the pretreatment method, especially regarding the SPE column, water sample pH, and the addition of ethylene diamine tetra-acetic acid disodium (Na2EDTA). Before extraction, a 200-milliliter water sample received 0.5 grams of Na2EDTA, and its pH was adjusted to 3 by using either sulfuric acid or sodium hydroxide solution. LY2157299 cost Using an HLB column, the water sample underwent enrichment and purification processes. A C18 column (100 mm × 21 mm, 35 μm) was used for HPLC separation employing a gradient elution method utilizing a mobile phase mixture of acetonitrile and 0.15% (v/v) aqueous formic acid. LY2157299 cost Qualitative and quantitative analyses were performed on a triple quadrupole mass spectrometer using an electrospray ionization source in multiple reaction monitoring mode. Analysis revealed correlation coefficients surpassing 0.995, signifying strong linear associations. The method detection limits (MDLs) spanned a range from 23 to 107 ng/L, while the limits of quantification (LOQs) ranged from 92 to 428 ng/L. Three different spiked levels of target compounds in surface water resulted in recoveries ranging from 612% to 157%, with corresponding relative standard deviations (RSDs) of 10% to 219%. In wastewater samples spiked with target compounds at three concentrations, the recovery percentages varied from 501% to 129%, with relative standard deviations (RSDs) ranging from 12% to 169%. The simultaneous determination of antibiotics in various water sources—reservoir water, surface water, sewage treatment plant outfall, and livestock wastewater—was achieved using the successful method. Analysis of watershed and livestock wastewater revealed the presence of most antibiotics. Surface water samples, in a count of ten, demonstrated the presence of lincomycin in 90 percent of the cases, while ofloxacin reached a peak concentration of 127 ng/L in livestock wastewater. Hence, this technique achieves remarkably high scores in terms of model decision-making levels and recovery rates, outperforming previously reported strategies. This developed method, distinguished by its capacity for small sample volumes, wide applicability, and rapid analysis, is a promising, rapid, sensitive analytical approach for promptly addressing environmental pollution emergencies.