Analytica, Volume 4, Issue 1 (March 2023) – 7 articles

Among many diseases, allergy appears to be a serious problem for human beings. Various forms of allergic disorders make people tense, leading to some other health issues. Many medications, including nonracemic and racemic ones, are used to treat this problem. It is important to have exact analysis strategies just to see any medication side effects, plasma profiles, and working efficiency. Therefore, efforts are made to review simple and chiral HPLC methods for antiallergic drugs; HPLC is the best analytical technique. The highlights in this article include the world scenario, causes of allergy, the effect of allergy on the economy, the mechanism of allergy in humans, classes of antiallergic drugs, simple drugs, chiral drugs, analysis by HPLC, and the chiral recognition mechanism. Moreover, attempts are also made to highlight the management of allergies and future perspectives. Full article

Human milk provides all the nutrients required by babies during the first six months of their life. Human milk lipids represent the main source of energy, contributing almost 50% of the total energy content. Additionally, fatty acids ensure the correct development of children in the prenatal, postnatal, and infant phases. Docosahexaenoic acid (DHA) is essential for visual and cognitive development, and its presence during childhood can affect long-term health. This study aimed to optimize and validate a methodology for the direct determination of DHA in human milk. We used 20 samples of human milk from lactating women living in the city of Itu, São Paulo, who attended Basic Health Units from September 2019 to September 2020, and a sample of certified reference material from the National Institute of Standards and Technology. The proposed methodology consists of a validated mixed transesterification process without prior lipid extraction, optimized by factorial design. This methodology can be successfully used in human milk samples as it is both precise and accurate. The values of DHA in the sampled milks were similar to those in European countries and lower than those in Asian countries due to diet. Full article

Chromatograms with overlapping peaks and a baseline rise or upset constitute a great challenge for analysts. Such a case regarding the analysis of bupropion hydrochloride and its 5 impurities in a tablet formulation was used as a model. A baseline correction technique for liquid chromatography coupled with diode array detection is described by using Rstudio. The asymmetry least squares (ALS) algorithm was used as implemented in the “baseline” package, with parameters lambda and p set to 4 and 0.05, respectively. Peak deconvolution and subsequent integration and area quantification were accomplished through Fytik software. Chromatographic data from the validation procedure were utilized to demonstrate the feasibility of the suggested method and whether this correction affects the outcome of the validation study. Finally, a robustness study was carried out in order to shed light on the factors that have a more significant influence on the baseline correction, showing the reliability of this procedure through random changes in its parameters. Full article

Fluorescent staining of microplastics as a detection method is consistently gaining importance in microplastics research, as it is fast, easy to use, and requires low technical effort. In this study, a complete procedure was developed, from sample collection to sample processing and detection, to measure microplastics with low cost and time requirements. The developed procedure was tested by measuring the microplastics in the effluent of a German wastewater treatment plant over a period of one year. The results show that the process is especially well suited to investigate temporal variations of microplastic contamination, which requires a large number of samples to be processed. Further, the precision and selectivity of the detection process could be improved by applying newly developed Nile red derivatives for fluorescent staining. A low budget modification of a microscope for fluorescent imaging is compared to a modification with precise optical bandpass filters. A script enabling automated microplastic detection and counting was developed, improving the accuracy and comparability of the process. Full article

Global plastic production and usage has increased annually for decades and microplastic pollutants (≤5 mm) are a growing concern. Microplastics in surface waters can adsorb and desorb harmful chemicals such as per- and polyfluoroalkyl substances (PFAS). Microplastics can accumulate across all tropic levels in the marine food web. The purpose of this research was to analyze the stomach and intestinal contents of stranded (Mississippi coast) bottlenose dolphins and sea turtles for the presence of microplastics and commonly found PFAS, PFOS, PFOA, and GenX. Gut contents were digested (10% KOH in 50% MeOH) and then analyzed for microplastics using pyrolysis gas chromatography-mass spectrometry (Pyro-GC-MS), Nile red microscopy, X-ray photo electron spectroscopy (XPS), and Raman spectroscopy. Digested sample filtrate was pre-concentrated using solid-phase extraction (SPE) before PFAS liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis. The PFOS extraction and analysis had 98.6% recovery when validated with certified pike‒perch fish reference material. The Nile red testing on most samples revealed the presence of microplastics (Table S1). The Pyro-GC-MS results from two samples confirmed the presence of the plasticizer acetamide. The Raman spectroscopy analysis indicated characteristic plastic peaks corresponding to polystyrene in one sample. PFOS (95.5 to 1,934.5 µg/kg) was detected in three dolphin stomach samples. This project is part of a long-term study with the goal of a better understanding of microplastics and PFAS environmental contamination and their impact on bottlenose dolphins and sea turtles. Full article

Levetiracetam (LEV) is a broad spectrum antiseizure medication that is used in various seizure types. There is evidence that therapeutic drug monitoring (TDM) of LEV is of value in selected patient populations, therefore determination of LEV plasma concentrations is essential. Herein we developed and validated a simple, reproducible, and practical method for the quantification of LEV concentrations in human plasma samples using high performance liquid chromatography (HPLC). Plasma samples (0.3 mL) deproteinization was done using acetonitrile. HPLC chromatographic separation of plasma samples was accomplished by reversed phase C18 column. The mobile phase constituted water and acetonitrile (90:10, v/v) ran at flow rate of 1 mL/min. Signal acquisition was conducted at a wavelength of 192 nm. Calibration curves showed excellent linearity (Correlation coefficient r² > 0.99) over a concentration range of 3–80 μg/mL. Both inter and intraday assay accuracy and precision were less than 8% (except for the lowest limit of quantification was within 20%). Elution time was 15 min. The developed method excluded the use of buffers and utilized small volumes of plasma samples with simple mobile phase composition. Therefore, our method could be practically applied to routine TDM. Full article