Analytical Methods最新文献

Peroxide-mediated oxidation of drug molecules is a known challenge faced throughout the pharmaceutical development pathway—from early-stage stability studies to manufacturing processes. During the initial development stage, the major source of peroxide is the formulation excipients, whether they are pre-loaded or generated in situ due to slow degradation, and in the late phase, peroxides can be introduced during sanitization processes or generated via cavitation. In essence, a control strategy for peroxide mitigation often becomes a critical quality attribute for successful drug development. To this end, quantitation of peroxide is essential to monitor the peroxide level to ensure product quality and proposed shelf-life. However, methods for reliable and robust quantitation to detect trace levels of peroxide in a complex drug product matrix become increasingly challenging. This article discusses three high-throughput assays based on absorbance, fluorescence and chemiluminescence measurements to detect peroxide at a low level and compares the methods through validation studies in water. Selected methods have also been tested to understand the forced degradation of model peptide drug products with spiked hydrogen peroxide. Peptide degradation profiles and residual peroxide levels are presented to provide an understanding of the suitability of the quantitation methods and their performance.

Test protocols for airborne clearance of asbestos abatement sites define the collection, imaging and quantification of asbestos with transmission electron microscopy (TEM). Since those protocols were developed 35 years ago, scanning electron microscope (SEM) capabilities have significantly improved and expanded, with improvements in image spatial resolution, elemental analysis, and transmission electron diffraction capabilities. This contribution demonstrates transmission electron imaging and diffraction using NIST Asbestos Standard Reference Materials and a conventional SEM to provide comparable identification and quantification capabilities in the SEM as the current regulatory methods based on TEM techniques. In particular, we demonstrate that the 0.53 nm layer line spacing that is characteristic of asbestos can be quantified using different detection methods, and that other identifying diffraction signatures of chrysotile are readily obtained. The results demonstrate a viable alternative to the current TEM-based methods for asbestos identification and classification.

While polycyclic aromatic hydrocarbons (PAHs) are well-known for their potential carcinogenic and mutagenic effects, the health implications of exposure to oxygenated PAHs (OPAHs), which are significant substitutes with increased persistence and bioaccumulation, are less understood. In this work, we compared the background levels of liquid–liquid, solid-phase, and supported-liquid extraction for the determination of serum PAHs and OPAHs. Liquid–liquid extraction demonstrated minimal background interference and was validated and used for human biomonitoring of PAHs and OPAHs in 240 participants using gas chromatography coupled with tandem mass spectrometry. We observed significant positive correlations between these compounds using Spearman correlation analysis. Furthermore, we investigated the concentration levels and compositions of PAHs and OPAHs among different demographic characteristics, including gender, age, and body mass index. Linear regression analysis demonstrated a weak but significant correlation between total concentrations of PAHs and OPAHs and age and body mass index. A multivariate linear regression analysis was then conducted to examine the association of exposure to individual PAHs and OPAHs with the body mass index. Naphthalene exposure and body mass index showed a statistically significant positive correlation, suggesting that higher levels of naphthalene exposure are associated with higher body mass index values. This study establishes a robust method for biomonitoring PAHs and OPAHs in serum, evaluating the exposure levels of these compounds in healthy adults and highlighting their associations with demographic characteristics.

In this work, two types of optical sensors were prepared for the quantification of potassium: the bulk optode (BO) and nano-optode (NO). The BO was prepared using three main components: the ionophore valinomycin, the ion exchanger tetrakis(4-chlorophenyl) potassium borate (K-TCPB), and the chromoionophore ETH 5294 (CHI). The optimal composition was found to be in a ratio of [1 : 1 : 1]. The NO was prepared by miniaturizing the BO through sonication in surfactant Pluronic F-127. The working range for the linear calibration model of BO was from 10⁻⁶ to 1.0 M K⁺ with a LOD_BO = 0.31 μM, meanwhile for NO was from 10⁻⁴ to 1.0 M K⁺ with a LOD_NO = 30.3 μM. Both optodes were tested for selectivity towards K⁺ in the presence of alkaline and alkaline earth ions, with a selectivity coefficient > 1.0. Furthermore, precision and stability studies of BO and NO were performed for three levels of K⁺ concentrations, 10⁻⁶, 10⁻³, 1.0 M for BO and 10⁻⁴, 10⁻², 1.0 M for NO, showing a good homogeneity of the NO in the whole concentration range. However, an excessive variability was obtained for BO at 1.0 M K⁺. Therefore, the NO represents a potential tool for quantification of K⁺.

The detection of anions using carbon dots (CDs) has received less attention compared to cations. Therefore, the present study aimed to develop a fluorescence sensor based on carbon dots (CDs) capable of detecting S²⁻ in real water samples. The CDs were successfully prepared from the residues of a traditional Chinese herb, Gardenia, which emitted green photoluminescence (PL) under ultraviolet light irradiation. The as-prepared CDs were quasi-spherical in shape and ranged in size from 10 to 30 nm. Different detailed analyses proved that the CDs had good morphology, various functional groups, high water solubility, great optical features, and excellent stability under diverse environmental conditions. The ion detection showed that only Ag⁺ had the strongest fluorescence quenching effect on the CDs, however, the addition of S²⁻ could recover their fluorescence. Based on these results, an “off–on” fluorescence sensor was achieved to selectively detect the concentration of S²⁻ in real water samples with a limit of detection (LOD) of 39 μM, which further expanded the application of residues from traditional Chinese herbal medicine.

Intelligent technology can assist in the diagnosis and treatment of disease, which would pave the way towards precision medicine in the coming decade. As a key focus of medical research, the diagnosis and prognosis of cancer play an important role in the future survival of patients. In this work, a diagnostic method based on nano-resolution imaging was proposed to meet the demand for precise detection methods in medicine and scientific research. The cell images scanned by AFM were recognized by cell feature engineering and machine learning classifiers. A feature ranking method based on the importance of features to responses was used to screen features closely related to categorization and optimization of feature combinations, which helps to understand the feature differences between cell types at the micro level. The results showed that the Bayesian optimized back propagation neural network has accuracy rates of 90.37% and 92.68% on two cell datasets (HL-7702 & SMMC-7721 and GES-1 & SGC-7901), respectively. This provides an automatic analysis method for identifying cancer cells or abnormal cells, which can help to reduce the burden of medical or scientific research, decrease misjudgment and promote precise medical care for the whole society.