In the realm of English plant names, the Chinese magnolia vine stands out. Throughout the history of Asia, this method of treatment has been applied to various health conditions, ranging from chronic coughs and shortness of breath, to frequent urination, diarrhea, and diabetes. This is due to the wide array of bioactive components, like lignans, essential oils, triterpenoids, organic acids, polysaccharides, and sterols. These constituents can, in some circumstances, affect the plant's pharmacological efficiency. The primary bioactive components and major constituents of Schisandra chinensis are lignans possessing a dibenzocyclooctadiene framework. While Schisandra chinensis is rich in potential lignans, its complex composition yields a proportionally lower extraction amount of these substances. Consequently, meticulous examination of pretreatment techniques in sample preparation is crucial for ensuring the quality of traditional Chinese medicine. Matrix solid-phase dispersion extraction, or MSPD, is a thorough process encompassing destruction, extraction, fractionation, and purification steps. The MSPD method is a simple method for preparing liquid, viscous, semi-solid, and solid samples, requiring only a small number of samples and solvents, and circumventing the need for any specialized equipment or instruments. Employing a method combining matrix solid-phase dispersion extraction (MSPD) and high-performance liquid chromatography (HPLC), this study determined five lignans—schisandrol A, schisandrol B, deoxyschizandrin, schizandrin B, and schizandrin C—in Schisandra chinensis simultaneously. 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. Regarding lignan extraction yields, the effects of adsorbent mass, the type of eluent, and the volume of eluent were investigated. Schisandra chinensis lignan analysis via MSPD-HPLC employed Xion as the adsorbent. Analysis of the extraction process parameters revealed the MSPD method's efficiency in extracting lignans from Schisandra chinensis powder (0.25 g), utilizing Xion (0.75 g) as an adsorbent and methanol (15 mL) as an eluting solvent. 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). Ranging from 0.00089 to 0.00294 g/mL, and then from 0.00267 to 0.00882 g/mL, respectively, were the detection and quantification limits. The levels of lignans examined were categorized as low, medium, and high. In terms of average recovery rates, the values spanned from 922% to 1112%, correlating to relative standard deviations between 0.23% and 3.54%. Both intra-day and inter-day measurements demonstrated precision values less than 36%. PMX-53 manufacturer The advantages of MSPD over hot reflux extraction and ultrasonic extraction lie in its combined extraction and purification process, making it more efficient, faster, and requiring fewer solvents. Lastly, the optimized technique proved successful in investigating five lignans within Schisandra chinensis samples originating from seventeen cultivation sites.
The illicit incorporation of recently banned substances into cosmetics is on the rise. Newly developed glucocorticoid clobetasol acetate is excluded from the current national standards and is structurally analogous to clobetasol propionate. In cosmetic products, a novel method was developed, using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), to determine the presence and concentration of clobetasol acetate, a novel glucocorticoid (GC). This new method was demonstrably effective with five prevalent cosmetic matrices: creams, gels, clay masks, masks, and lotions. Four different pretreatment methods were evaluated: direct extraction with acetonitrile, PRiME pass-through column purification, solid-phase extraction (SPE), and QuEChERS purification. Additionally, the consequences stemming from diverse extraction efficiencies of the target compound, such as the variety of extraction solvents and the duration of the extraction process, were studied. To enhance performance, the MS parameters, specifically ion mode, cone voltage, and ion pair collision energy of the target compound, were optimized. An examination of chromatographic separation conditions and the target compound's response intensities, across various mobile phases, was conducted. 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. The concentrated extracts were separated on the Waters CORTECS C18 column (150 mm × 21 mm, 27 µm), a gradient elution technique employing water and acetonitrile as mobile phases. The target compound was observed using electrospray ionization (ESI+), positive ion scanning, and multiple reaction monitoring (MRM) analysis. A matrix-matched standard curve facilitated the performance of quantitative analysis. Under the most favorable conditions, the target compound showed good linearity in the range between 0.09 and 3.7 grams per liter. The linear correlation coefficient (R²) exceeded 0.99, the quantification limit (LOQ) of the procedure reached 0.009 g/g, and the detection limit (LOD) stood at 0.003 g/g for these five distinct cosmetic samples. A recovery test was implemented at three spiked levels, 1, 2, and 10 times the limit of quantification (LOQ). Across five cosmetic matrices, the tested substance demonstrated recoveries fluctuating between 832% and 1032%, corresponding with relative standard deviations (RSDs, n=6) spanning from 14% to 56%. A variety of cosmetic samples from diverse matrices were screened using this method. A total of five positive samples were detected, indicating clobetasol acetate concentrations ranging from 11 to 481 g/g. Finally, the method's simplicity, sensitivity, and reliability make it suitable for high-throughput qualitative and quantitative screening, as well as the analysis of cosmetics with various matrix compositions. Moreover, this method supplies vital technical support and a theoretical premise for developing applicable detection standards for clobetasol acetate in China, and for managing its presence within cosmetics. For the successful implementation of management plans to address illegal additions in cosmetics, this method is practically significant.
Repeated and broad usage of antibiotics for treating illnesses and augmenting animal development has caused their permanence and buildup in water, soil, and sediment layers. As a newly identified environmental contaminant, antibiotics have taken center stage in recent years, demanding substantial research efforts. The water environment frequently has antibiotics present at negligible levels. Unfortunately, the task of ascertaining the presence and quantities of diverse antibiotic types, each with distinct physicochemical characteristics, continues to pose a significant challenge. Therefore, the creation of pretreatment and analytical procedures to rapidly, accurately, and sensitively analyze these emerging contaminants within various water samples is imperative. Antibiotic screening and sample composition guided the optimization of the pretreatment method, specifically addressing the SPE column selection, water sample pH level, and the incorporation of ethylene diamine tetra-acetic acid disodium (Na2EDTA) into the water sample. In preparation for extraction, 0.5 grams of Na2EDTA was added to a 200 mL water sample, and the resultant solution's pH was subsequently adjusted to 3 employing either sulfuric acid or sodium hydroxide solution. PMX-53 manufacturer An HLB column facilitated the enrichment and purification of the water sample. A gradient elution technique using a C18 column (100 mm × 21 mm, 35 μm) and a mobile phase consisting of acetonitrile and a 0.15% (v/v) aqueous formic acid solution was employed for the HPLC separation process. PMX-53 manufacturer Analyses of both qualitative and quantitative natures were performed on a triple quadrupole mass spectrometer using a multiple reaction monitoring mode with electrospray ionization. The data showed correlation coefficients exceeding 0.995, confirming a strong linear association. Regarding the method detection limits (MDLs), they were found within the range of 23 to 107 ng/L, and the limits of quantification (LOQs) were observed in the 92 to 428 ng/L interval. The recoveries of target compounds in surface water samples, at three spiked levels, fluctuated between 612% and 157%, while their relative standard deviations (RSDs) ranged between 10% and 219%. The percentage recovery of target compounds in wastewater, across three spiked levels, varied from 501% to 129%, while the relative standard deviations (RSDs) spanned a range from 12% to 169%. A successful application of the method provided the capability to simultaneously analyze antibiotics in samples from reservoir water, surface water, sewage treatment plant outfall, and livestock wastewater. The watershed and livestock wastewater samples exhibited the presence of a large quantity of the detected antibiotics. Of the 10 surface water samples, 90% showcased the presence of lincomycin. Ofloxaccin, conversely, exhibited the highest concentration (127 ng/L) in livestock wastewater. Consequently, the current approach demonstrates superior performance in terms of model decision-making accuracy and recovery rates when compared to previously published methods. The developed method's strengths lie in its small sample requirements, broad applicability, and speedy analysis, positioning it as a rapid, efficient, and highly sensitive method for responding to critical environmental pollution situations.