Current Pharmaceutical Analysis - Volume 19, Issue 3, 2023

Cell phones are like a notepad PC with their own working framework, processor, interior memory, and top-notch camera focal points. Cell phones are more open and less expensive than versatile analytical devices. The quantity of cell phone users overall outperformed 2 billion in 2016 and it addresses more than a fourth of the worldwide population. There have been numerous new articles on the utilization of cell phones as versatile detectors, bioanalytical equipment, and instrument interfaces. The utilization of cell phones has opened doors for prognostic, diagnostic, detection, observing, quantification, control, or making versatile applications, since it can be very well utilized to run routine tests. Moreover it does not require a trained personnel and it is convenient and considered a minimal-expense gadget. The development of analytical methods is crucial in drug development. Improvement of existing and execution of new methodologies are essential for the present-day analytical chemistry of drugs. Recently published studies focussed on some of the applications of smartphone-based analytical methodologies in the last few years for the determination of drugs in different matrices. The aim of the presented review was to enhance the visibility of one of the fast and novel applications of smartphone technology. This will help scientists and researchers to understand the recent developments and explore new possibilities in this field.

Background: For the development of robust analytical methods, Analytical-Qualityby- Design (AQbD)-based testing methods have been found to be more suited than other one factorial approaches. By creating a Method Operable Design Space, this strategy selects the optimal method conditions using the appropriate Design of Experiments. Objective: To impart knowledge to the researchers producing methods using this technique, this review seeks to provide an overview of the Analytical Quality-by-Design technique, experimental designs used, and a survey on methods developed using this technique in various analytical instruments. Methods: The following parts must typically be accomplished for the method to be developed utilizing the Analytical Quality by Design technique: analytical target profile, scouting and risk assessment, experimental runs, selection of Method Operable Design Region, robustness testing, and validation. To optimize the risk parameters, suitable designs for the experiment were chosen based on the number of variables that needed to be optimized. Conclusion: By establishing a relationship between the high-risk factors and target profiles utilizing multidimensional design space, robustness and other critical quality attributes in techniques were attained with a minimum of experimental runs, analytical time, and energy. So, it stands to reason that the Analytical Quality by Design technique will soon be widely used and highly advantageous in several industries.

Background: A reversed-phase high-performance liquid chromatographic method for determining thrombin activity is described. The improved method can provide a high resolution between substrate Nα-P-toluenesulfonyl-L-arginine methyl ester (TAME) and the product of enzyme reaction, Nα-P-toluenesulfonyl-L-Arginine (TA). Methods: When the substrate concentration was 5 mg/mL, the Michaelis equation approached the zero-order reaction, and the thrombin enzyme activity must have a good linear relationship with the consumption of TAME or the yield of TA. Results: The method is suitable for quantitatively analyzing thrombin activity in formulation or serum. Conclusion: Three batches of thrombin lyophilized preparations were determined for activity.

Background: Knee osteoarthritis (KOA) is a clinically common degenerative joint disease that is not fatal but has a high prevalence. Synovitis ointment (HMYG) is a traditional Chinese medicine formula that has been clinically proven to treat KOA; however, its therapeutic targets remain unknown. Objective: This study aimed to identify metabolites and potential targets of synovitis ointment alleviation in rats with KOA using ultra-high-performance liquid-chromatography–mass spectrometry (UHPLC-MS) metabolomics. Methods: The meniscus on each side of the knee was removed to model KOA in rats. The synovitis ointment treatment was provided for 4 weeks. The lateral diameter of the knee was measured once a week, and after 4 weeks, serum was collected to observe changes in the knee through a metabolomic analysis. Results: Synovitis ointment reduced the lateral diameter of the knee joint, relieved knee swelling, and improved knee volume. In total, 28 differential metabolites, which were mainly involved in arginine and proline metabolism and apoptosis, were identified in the Con and HMYG groups. 15-Deoxy-d-12, 14-PGJ2 and fomepizole were found to be the key metabolites after the HMYG treatment of KOA. Compared with known drugs (diclofenac diethylamine emulsion and Jin Huang San), 2-(SGlutathionyl) acetyl glutathione, daidzein, pelargonic acid, and sulfamethoxazole increased in the HMYG, and the metabolic pathways included the oxytocin signaling pathway, platelet activation, olfactory transduction, phototransduction, and cGMP-PKG signaling pathway. The expression levels of cleaved-caspase-3, Bcl-2, PIK3a, TP53, TGFB1, and NFKB1 were reversed after HMYG treatment. Conclusion: It has been observed that synovitis ointment relieves KOA. UHPLC-MS can analyze the potential mechanism of action of the herbal compound of the synovitis ointment.

Objective: The aim of this study was to propose an easy, fast, and precise method, which can be satisfactorily applied to the simultaneous determination of the drugs in pharmaceutical dosage forms instead of the high-performance liquid chromatography (HPLC) method. Methods: Complicated and costly instruments, as well as spending a lot of time for analysis are the limitations of the chromatography method. Hence, UV spectrophotometric technique based on net analyte signal (NAS) and partial least squares (PLS) was proposed and validated for the simultaneous determination of vitamin A and vitamin D in binary mixtures and commercial skin ointment. The chromatographic technique was implemented to compare with the proposed approach for the simultaneous analysis of drugs. Results: The NAS method was able to determine vitamin A and vitamin D in the concentration range of 1–7 and 2-13 μg mL^-1 at λmax= 323 and λmax= 261, respectively. The limit of detection (LOD) and limit of quantification (LOQ) related to the NAS method were found to be 0.092, 0.053 μg/mL and 0.214, 0.170 μg/mL for vitamin A and vitamin D, respectively. The root mean square error (RMSE) of the test series was 0.0607 and 0.0547 for vitamins A and D, respectively. Recoveries by the PLS method were found in the range of 99.98%-100.49% and 99.57%- 100.88% for vitamins A and D, respectively. The results obtained from the NAS and PLS procedures were statistically compared with the reference method (HPLC) via analysis of variance (ANOVA) test, where no significant difference was observed. Conclusion: The spectrophotometry along with NAS and PLS methods are proper, rapid, and economic for the determination of pharmaceutical components in quality control laboratories.

Background: As an external medicine, policresulen solution didn't get much attention throughout the world. From the paper which had been published yet, there has been no report concerning other unknown impurities in the policresulen solution. Four known components had been identified as well as quantified, however, as long as people’s concern for drug safety increased rapidly, there still remain impurities to be studied. Objective: This paper focuses on the separation and characterization of the impurities in the policresulen solution, which is critical for controlling the production of this drug. Methods: The components and impurities in the policresulen solution were separated and characterized using HPLC coupled with to Q-TOF mass spectrometry. An ACE EXCEL 5 C18-PFP column (4.6 mm×250 mm, 5 μm) was used, and the mobile phases were 0.01 M ammonium acetate solution and methanol. Results: 21 previously unknown impurities were separated and characterized in a policresulen solution, and the structures were proposed based on the MS/MS fragmentation data. Conclusion: Based on the characterization of impurities, this study showed that there remain lots of oligomers in the policresulen solution, apart from four known components. This study could be used for further analytical analysis of the policresulen solution, which could improve the quality control of the policresulen solution and other preparations recommended in pharmacopoeias.

Background: Successful drug extraction from biological fluids is challenging due to interfering factors and the trace levels of the target analytes. Objective: We aimed to provide a suitable and sensitive method to increase the efficiency of methotrexate extraction from biological fluids. Methods: Chitosan-based nanogel synthesized by the ionic gelation method was used for solidphase microextraction of methotrexate from aqueous and plasma media. The nanogel was characterized in vitro in terms of morphological characteristics (transmission electron microscopy), particle size, polydispersity index (PDI), and zeta potential. High-performance liquid chromatography was used to determine the methotrexate concentrations and extraction yield. Results: A nanogel with an average size of 135.6 nm and PDI of 0.14 was used for the nanoextraction of methotrexate in this study. The methotrexate concentration, nanogel amount, and extraction time affected the extraction yield. Maximum recovery percentages of 75% and 69% were achieved when extracting methotrexate from aqueous and plasma media, respectively. Conclusion: The high extraction yields in both studied media indicate that using chitosan-based nanogel as a sorbent during the solid-phase microextraction of methotrexate is a promising prospect, with potential uses for other drugs in different media. It seems that using nanogels can be an excellent way to improve the extraction of drugs from biological environments.