Five cosmetic matrices were used to test the substance, which showed recoveries from 832% to 1032% and relative standard deviations (RSDs, n=6) of 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. Furthermore, the method furnishes essential technical support and a theoretical foundation for the creation of practical detection standards for clobetasol acetate in China, as well as for regulating its presence in cosmetic products. This method offers critical practical value for putting into action management plans to control unauthorized ingredients in cosmetics.
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. Environmental research has recently intensified its focus on antibiotics, which are now recognized as an emerging pollutant. Antibiotics are present in detectable, though minute, quantities in aquatic environments. Regrettably, the precise identification and quantification of various antibiotic types, each with differing physicochemical traits, remains a demanding process. Accordingly, the need for methods to rapidly, accurately, and sensitively analyze these emerging pollutants in various water specimens necessitates the development of pretreatment and analytical procedures. The pretreatment procedure was improved, tailored to the specific characteristics of the screened antibiotics and sample matrix, with focus on the SPE column, water sample pH, and ethylene diamine tetra-acetic acid disodium (Na2EDTA) addition. 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. The HLB column was instrumental in achieving the enrichment and purification of the water sample. Gradient elution with a mobile phase containing acetonitrile and 0.15% (v/v) aqueous formic acid was used for HPLC separation on a C18 column (100 mm × 21 mm, 35 μm). 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 correlation coefficients, exceeding 0.995, highlighted robust linear relationships in the results. Limits of quantification (LOQs) were found to fall between 92 and 428 ng/L, and method detection limits (MDLs) were observed to be within the 23 to 107 ng/L range. At three spiked levels, target compounds' recoveries in surface water varied from 612% to 157%, with relative standard deviations (RSDs) ranging from 10% to 219%. Target compound recoveries in wastewater samples, spiked at three concentrations, exhibited a wide range, from 501% to 129%, with relative standard deviations (RSDs) varying from 12% to 169%. The method yielded successful results in the simultaneous determination of antibiotics across multiple water sources: reservoir water, surface water, sewage treatment plant outfall, and livestock wastewater. Antibiotics were predominantly found in watershed and livestock wastewater. A detection frequency of 90% for lincomycin was observed across a collection of 10 surface water samples. Ofloxaccin's concentration peaked at 127 ng/L in livestock wastewater samples. Consequently, the current approach demonstrates superior performance in terms of model decision-making accuracy and recovery rates when compared to previously published methods. With its capacity for small water samples, wide-ranging applicability, and rapid analysis, the newly developed method emerges as a fast, efficient, and sensitive analytical approach, particularly valuable for tracking environmental emergencies. Antibiotic residue standards can be reliably established thanks to the reference provided by this method. Regarding the environmental occurrence, treatment, and control of emerging pollutants, the results offer compelling support and a deepened understanding.
Quaternary ammonium compounds (QACs), a class of cationic surfactants, are commonly found in the formulations of disinfectants. The heightened use of QACs warrants concern due to potential adverse effects on respiratory and reproductive systems, particularly in cases of inhalation or ingestion. QAC exposure in humans is largely driven by eating food and inhaling airborne QACs. The presence of QAC residues poses a serious and substantial threat to the public's health. Recognizing the importance of evaluating potential QAC residue levels within food, a procedure was established for the simultaneous detection of six common QACs and one emerging QAC, Ephemora, in frozen food. The method employed ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), combined with a modified QuEChERS extraction technique. The method's response, recovery, and sensitivity were optimized during sample pretreatment and instrument analysis, focusing on key factors like extraction solvents, adsorbent types and dosages, apparatus conditions, and mobile phases. A 20-minute vortex-shock extraction using 20 mL of methanol-water (90:10, v/v) containing 0.5% formic acid yielded QAC residues from the frozen food. PF-05251749 clinical trial A 10-minute ultrasonic treatment was applied to the mixture, after which it was centrifuged at 10,000 revolutions per minute for a period of 10 minutes. A milliliter of supernatant was transferred to another tube for purification with 100 milligrams of PSA adsorbent material. The purified solution was subjected to analysis after 5 minutes of mixing and centrifugation at 10,000 revolutions per minute. An ACQUITY UPLC BEH C8 chromatographic column (50 mm × 2.1 mm, 1.7 µm), held at a column temperature of 40°C and operated at a flow rate of 0.3 mL/min, was employed for separating the target analytes. A 1-liter injection volume was utilized. A multiple reaction monitoring (MRM) analysis was undertaken in the positive electrospray ionization mode, ESI+. Employing the matrix-matched external standard technique, seven QACs were measured. The optimized chromatography-based method facilitated a complete and thorough separation of the seven analytes. Consistent linear relationships were found for all seven QACs, spanning a concentration range from 0.1 to 1000 ng/mL. The correlation coefficient r² was observed to fall between 0.9971 and 0.9983. Quantification limits, at 0.15 g/kg to 0.30 g/kg, and detection limits, at 0.05 g/kg to 0.10 g/kg, were established, respectively. Six replicate determinations, using salmon and chicken samples spiked with 30, 100, and 1000 grams per kilogram of analytes, confirmed accuracy and precision, in accordance with the current legal standards. The seven QACs exhibited recovery rates that averaged between 101% and 654%. PF-05251749 clinical trial Relative standard deviations (RSDs) exhibited a variation spanning from 0.64% to 1.68%. Matrix effects on analytes in salmon and chicken samples, after purification with PSA, spanned a range from -275% to 334%. To determine the presence of seven QACs in rural samples, the developed method was employed. In only one sample were QACs observed; the levels measured fell short of the stipulated residue limit prescribed by the European Food Safety Authority. The detection method's high sensitivity, coupled with its good selectivity and stability, guarantees precise and trustworthy results. A rapid and simultaneous determination of seven QAC residues is achievable in frozen food using this. Future risk assessment studies focusing on this compound class will benefit significantly from the insights provided by these results.
While vital for safeguarding food crops, the widespread use of pesticides in agricultural areas often has an adverse impact on both ecological balance and human health. The pervasive nature of pesticides in the environment, coupled with their toxic properties, has engendered substantial public concern. China's position as a major pesticide user and producer is prominent on the global stage. Unfortunately, there is a limited amount of information on pesticide exposure in humans, which underscores the need for a method to quantify pesticide levels in human samples. To quantify two phenoxyacetic herbicides, two organophosphate pesticide metabolites, and four pyrethroid pesticide metabolites in human urine, a sensitive and comprehensive method was both developed and validated in this study. This method relied upon 96-well plate solid-phase extraction (SPE) coupled with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The chromatographic separation conditions and MS/MS parameters were subjected to a systematic optimization process for this application. Through an optimization process, six solvents were selected to effectively extract and clean human urine samples for further analysis. The human urine samples' targeted compounds achieved complete separation within 16 minutes during a single analytical run. A 1 mL sample of human urine was mixed with 0.5 mL of 0.2 M sodium acetate buffer and then processed overnight at 37°C via -glucuronidase enzyme hydrolysis. Methanol was used to elute the eight targeted analytes after their extraction and cleaning procedure using the Oasis HLB 96-well solid phase plate. Separation of the eight target analytes was accomplished using a UPLC Acquity BEH C18 column (150 mm × 2.1 mm, 1.7 μm) with a gradient elution method involving 0.1% (v/v) acetic acid in acetonitrile and 0.1% (v/v) acetic acid in water. PF-05251749 clinical trial Using isotope-labeled analogs, the quantity of analytes was determined after their identification via multiple reaction monitoring (MRM) in the negative electrospray ionization (ESI-) mode. Para-nitrophenol (PNP), 3,5,6-trichloro-2-pyridinol (TCPY), and cis-dichlorovinyl-dimethylcyclopropane carboxylic acid (cis-DCCA) demonstrated good linearity between 0.2 and 100 g/L. In comparison, 3-phenoxybenzoic acid (3-PBA), 4-fluoro-3-phenoxybenzoic acid (4F-3PBA), 2,4-dichlorophenoxyacetic acid (2,4-D), trans-dichlorovinyl-dimethylcyclopropane carboxylic acid (trans-DCCA), and 2,4,5-trichlorophenoxyacetic acid (2,4,5-T) displayed linearity from 0.1 to 100 g/L, with all correlation coefficients exceeding 0.9993.