The mobile phase consisted of a 0.1% (v/v) aqueous solution of formic acid, along with 5 mmol/L ammonium formate, and acetonitrile also containing 0.1% (v/v) formic acid. Electrospray ionization (ESI) in positive and negative modes ionized the analytes, which were then detected by multiple reaction monitoring (MRM). The target compounds were quantified via the external standard method. For optimal performance, the method displayed a high degree of linearity between 0.24 and 8.406 g/L, with correlation coefficients consistently exceeding 0.995. Quantification limits (LOQs), for plasma samples, varied between 168 and 1204 ng/mL; urine sample LOQs were between 480 and 344 ng/mL. Compound recoveries, averaged across the board, demonstrated a considerable range, from 704% to 1234% when spiked at levels of 1, 2, and 10 times the lower limit of quantification (LOQ). Intra-day precisions fluctuated from 23% to 191%, while inter-day precisions showed a range between 50% and 160%. AZD-5153 6-hydroxy-2-naphthoic cell line Using the established protocol, the target compounds were detected in the plasma and urine of mice following intraperitoneal exposure to 14 shellfish toxins. Analysis of the 20 urine and 20 plasma samples showed the presence of all 14 toxins, with concentrations ranging from 1940 to 5560 g/L in urine and 875 to 1386 g/L in plasma. Requiring only a small sample, the method is both straightforward and highly sensitive. Thus, it is a very appropriate technique for the prompt detection of paralytic shellfish toxins in both plasma and urine.
A novel solid-phase extraction (SPE) coupled with high-performance liquid chromatography (HPLC) method was developed for the quantification of 15 carbonyl compounds, including formaldehyde (FOR), acetaldehyde (ACETA), acrolein (ACR), acetone (ACETO), propionaldehyde (PRO), crotonaldehyde (CRO), butyraldehyde (BUT), benzaldehyde (BEN), isovaleraldehyde (ISO), n-valeraldehyde (VAL), o-methylbenzaldehyde (o-TOL), m-methylbenzaldehyde (m-TOL), p-methylbenzaldehyde (p-TOL), n-hexanal (HEX), and 2,5-dimethylbenzaldehyde (DIM), in soil samples. Soil extraction, using ultrasonic waves and acetonitrile, was followed by the derivatization of the extracted samples with 24-dinitrophenylhydrazine (24-DNPH), forming stable hydrazone compounds. Derivatized solutions were cleaned using an SPE cartridge, specifically a Welchrom BRP, which was filled with a copolymer composed of N-vinylpyrrolidone and divinylbenzene. Separation was performed using an Ultimate XB-C18 column (250 mm x 46 mm, 5 m) with isocratic elution, employing a 65:35 (v/v) acetonitrile-water mobile phase. Detection was carried out at a wavelength of 360 nm. The 15 carbonyl compounds in the soil were subsequently measured using an external standard methodology. By leveraging high-performance liquid chromatography, the proposed method for carbonyl compound determination in soil and sediment surpasses the procedures detailed in the environmental standard HJ 997-2018. The optimal conditions for soil extraction, as determined by a series of experiments, involved using acetonitrile as the solvent, maintaining a 30-degree Celsius temperature, and employing a 10-minute extraction time. The purification effect exhibited by the BRP cartridge was markedly superior to that of the conventional silica-based C18 cartridge, as determined through the results. The fifteen carbonyl compounds displayed a good degree of linearity, with all correlation coefficients exceeding 0.996. AZD-5153 6-hydroxy-2-naphthoic cell line Recovery percentages ranged from a high of 1159% down to 846%, the relative standard deviations (RSDs) from 0.2% to 5.1%, and the lowest to highest detection limits were 0.002 and 0.006 mg/L respectively. The 15 carbonyl compounds in soil, as identified in HJ 997-2018, can be analyzed quantitatively with a method that is simple, sensitive, and suitable for accurate determinations. Consequently, the enhanced methodology furnishes dependable technical assistance for examining the residual state and ecological comportment of carbonyl compounds within the soil.
From the Schisandra chinensis (Turcz.) plant, a kidney-shaped, reddish fruit emerges. The Schisandraceae family encompasses Baill, a prominent ingredient in traditional Chinese medicine. AZD-5153 6-hydroxy-2-naphthoic cell line In the realm of English plant names, the Chinese magnolia vine stands out. 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. This is a consequence of the broad spectrum of bioactive components, encompassing lignans, essential oils, triterpenoids, organic acids, polysaccharides, and sterols. These constituents can, in some circumstances, affect the plant's pharmacological efficiency. Lignans, specifically those with a dibenzocyclooctadiene-type structure, are the principal constituents and active compounds found in abundance within Schisandra chinensis. However, the compound complexity within Schisandra chinensis makes the extraction of lignans a process with significantly lower yields. Practically, in sample preparation procedures, the pretreatment methods employed deserve particular attention in ensuring the quality of traditional Chinese medicines. The method of matrix solid-phase dispersion extraction (MSPD) involves a comprehensive sequence of steps including destruction, extraction, fractionation, and purification A minimal sample and solvent requirement defines the straightforward MSPD method, which bypasses the need for specialized instruments or equipment, rendering it applicable for the preparation of liquid, viscous, semi-solid, and solid samples. A novel methodology integrating matrix solid-phase dispersion extraction with high-performance liquid chromatography (MSPD-HPLC) was developed for the simultaneous determination of five lignans, including schisandrol A, schisandrol B, deoxyschizandrin, schizandrin B, and schizandrin C, within Schisandra chinensis. The target compounds were separated on a C18 column via gradient elution. Mobile phases consisted of 0.1% (v/v) formic acid aqueous solution and acetonitrile. Detection was carried out at a wavelength of 250 nm. A study was conducted to assess the performance of 12 adsorbents, encompassing silica gel, acidic alumina, neutral alumina, alkaline alumina, Florisil, Diol, XAmide, Xion, and the inverse adsorbents C18, C18-ME, C18-G1, and C18-HC, in optimizing the extraction yield of lignans. The extraction efficiency of lignans was studied considering the parameters of adsorbent mass, eluent type, and eluent volume. Schisandra chinensis lignan analysis via MSPD-HPLC employed Xion as the adsorbent. Optimization of extraction parameters for lignans from Schisandra chinensis powder (0.25 g) demonstrated the effectiveness of the MSPD method, using Xion (0.75 g) as the adsorbent and methanol (15 mL) as the elution solvent. Methods for the analysis of five lignans found in Schisandra chinensis were created, with results displaying a highly linear relationship (correlation coefficients (R²) consistently above 0.9999 for each analyte). The quantification limits, varying from 0.00267 to 0.00882 g/mL, and the detection limits, varying from 0.00089 to 0.00294 g/mL, were, respectively, found. Different concentrations of lignans, specifically low, medium, and high, were used in the tests. The average recovery rate was found to be between 922% and 1112%, and the relative standard deviations were situated between 0.23% and 3.54%. Intra-day and inter-day precision figures failed to surpass the 36% threshold. MSPD, contrasting with hot reflux extraction and ultrasonic extraction techniques, offers advantages in combined extraction and purification, requiring less time and solvent. Finally, the optimized methodology was successfully applied to the examination of five lignans in Schisandra chinensis samples collected from seventeen cultivation locations.
Currently, illicit additions of novel restricted substances are increasingly prevalent in cosmetic products. Classified as a novel glucocorticoid, clobetasol acetate is not included in the current national standards, and is structurally similar to clobetasol propionate. To determine clobetasol acetate, a new glucocorticoid (GC), in cosmetics, a method based on ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was implemented. The new methodology demonstrated compatibility with five typical cosmetic matrices: creams, gels, clay masks, lotions, and face masks. A study compared four pretreatment methods: direct acetonitrile extraction, PRiME pass-through column purification, solid-phase extraction (SPE), and QuEChERS purification. Moreover, an inquiry was conducted into the effects of different extraction efficiencies of the target compound, specifically examining the range of solvents and the time required for extraction. Optimization procedures were performed on the MS parameters of the target compound's ion pairs, including ion mode, cone voltage, and collision energy. A comparison was made of the chromatographic separation conditions and response intensities of the target compound, as observed in diverse mobile phases. From the experimental data, the optimal extraction technique was ascertained as direct extraction. This process consisted of vortexing samples with acetonitrile, subjecting them to ultrasonic extraction lasting more than 30 minutes, filtering them through a 0.22 µm organic Millipore filter, and subsequently employing UPLC-MS/MS detection. The concentrated extracts were separated using a Waters CORTECS C18 column (150 mm × 21 mm, 27 µm), employing water and acetonitrile as the mobile phases for gradient elution. The multiple reaction monitoring (MRM) mode, coupled with electrospray ionization and positive ion scanning (ESI+), detected the target compound. Quantitative analysis was executed by leveraging the matrix-matched standard curve. Optimal conditions allowed the target compound to demonstrate a good linear fit within the concentration interval of 0.09 to 3.7 grams per liter. Across these five unique cosmetic matrices, the linear correlation coefficient (R²) demonstrated a value greater than 0.99; the method's limit of quantification (LOQ) was 0.009 g/g, and the limit of detection (LOD) was 0.003 g/g. The recovery test was executed using spiked levels of 1, 2, and 10 times the limit of quantification, denoted as LOQ.