Current Analytical Chemistry - Volume 19, Issue 7, 2023

Food safety has received increasing attention, and pesticide contamination is one of the primary issues. Many toxicological endpoints have been established to evaluate the hazards of pesticides. However, the sensitivity of toxic endpoints is dominated by analytical methods. The risks of pesticides may be underestimated when using insensitive analytical methods to establish the toxicological endpoints. Therefore, it is necessary to find highly sensitive analytical approaches to develop a toxicological endpoint. Recently, metabolomics has been widely applied for investigating the toxicological mechanism of environmental pollutants in animals and plants with higher sensitivity. However, metabolomics has not been utilized to establish toxicological endpoints. Herein, the potential of metabolomics for toxicological endpoint establishment is briefly discussed.

Nilotinib hydrochloride is a tyrosine kinase inhibitor licensed to treat chronic myelogenous leukemia in patients with the Philadelphia Chromosome (Ph+). Researchers at Novartis Pharmaceuticals discovered novel inhibitors that are effective against imatinib-resistant BCR-ABL mutations. As a consequence, Nilotinib was discovered. Several analytical approaches were employed to address the quantitative as well as qualitative assessment of Nilotinib from diverse biological and pharmaceutical matrices during the development of Nilotinib. The literature search was conducted by evaluating publications reporting on nilotinib analytical methodologies from 2006 to 2022. This review briefly summarizes the drug profile, viz. stereochemistry, mechanism of action, resistance, pharmacokinetics, pharmacodynamics, side effects, and several analytical techniques used to assess Nilotinib in dosage form, bulk, and biological fluids. The determination of Nilotinib using analytical methods is important for therapeutic drug monitoring, optimizing dosage, ensuring safety and efficacy, and conducting comparative studies. A variety of techniques are gathered and examined, including spectroscopy, electrophoresis, voltammetry, Raman spectroscopy, differential scanning calorimetry, X-ray diffraction, chromatography, and hybrid techniques. They are also useful for studying the pharmacokinetics of the drug. These methods play a crucial role in the effective and personalized treatment of patients with chronic myeloid leukemia and other conditions where Nilotinib is used.

Background: Sufentanil, an opioid analgesic, is used as an induction agent for general anesthesia during surgery. Sufentanil is more active than other anesthetics and has a narrow therapeutic range. Therefore, a precise dosage regimen is necessary when administering sufentanil.Objective: This study aimed to develop a bioanalytical method for the determination of sufentanil within the sensitive concentration range more than that in a previous study utilizing protein precipitation (PP) and determine the plasma concentration of sufentanil.Methods: A method for quantitating sufentanil was developed using ultra-high performance liquid chromatography coupled with mass spectrometry (UPLC-MS/MS) and detection by electrospray ionization (ESI). The internal standard was sufentanil-d5. Chromatographic separation was performed using an Acquity UPLC HSS T3 column (50x 2.1 mm, 1.8 μm) from Waters (Milford, MA, USA). Protein precipitation (PP) was used for sample preparation, and gradient elution was conducted using a mobile phase consisting of 1 mL of 2M ammonium acetate in 99% formic acid in 1 L of water or in 1 L of acetonitrile. The total run time for the analysis was 5 min, and the flow rate was 0.4 mL/min.Results: Standard curves were linear over ranges of 0.025-30 ng/mL for sufentanil with a correlation coefficient (r²) greater than 0.9998. The lower limit of quantification (LLOQ) was 0.025 ng/mL. The intra- and inter-day accuracies were 97.66%-108.8% and 101.25%-103.17%, respectively, and the precision did not exceed 15% for sufentanil.Conclusion: This study developed a validated, simple, sensitive, and convenient UPLC-MS/MS method for quantifying sufentanil in human plasma. This method was applied to determine sufentanil concentration in the plasma of patients undergoing surgery. The bioanalytical method using PP showed a sufficiently sensitive concentration range. This method could be applied to various pharmacokinetic studies of sufentanil.

Background: Initially synthesized as an antidepressant and potentially rapid onset of action, flibanserin (FLB) was approved by the Food and Drug Administration (FDA) in August 2015 with a warning to dispense the drug through a dedicated risk management program, despite the removal of HSDD from the DSM-5TM. The drug is the first noteworthy FDA-approved drug for treating premenopausal women with acquired, generalized HSDD.Objective: In literature, studies are plasma analyses or metabolite determinations to meet pharmacokinetic analyses and some analytical targets. For this reason, in this thesis, a new method has been developed for analysing FLB from pharmaceutical preparations, which is our target, providing all optimization conditions and method validity parameters.Method: The chromatographic separation was also investigated using Chromolith^® and Ascentis^® Express models with a total of six stationary phases. The mobile phase mixture was acetonitrile:ammonium formate (0.020 M, pH 6.0) and was used at the ratio (60:40, v/v). The optimum column temperature was chosen as 40.0±0.1°C, and the autosampler thermostat temperature was chosen as 15±0.1°C. The sample injection volume is optimized to be 1 μL.Results: The developed method is linear in the range of 2.63-105.0 ng/mL, and the regression coefficient is 0.999 intraday and 0.986 interday. In the method, LOD and LOQ were obtained as 128 pg/mL and 384 pg/mL, respectively. In addition, the ANOVA P values were calculated as 0.586 and 0.914, respectively, in the validation studies conducted intraday and interday.Conclusion: FLB chromatographic behaviors were studied and compared in detail with six different stationary phases. The developed method was fully validated according to the ICH Q2 (R1) guideline, and its pseudo-pharmaceutical formulation was analyzed.

Background: Green synthesis of nanomaterials is promising as a biological source for treating different diseases without side effects.Methods: In the present study, marine Streptomyces sp. was used to biosynthesize silver nanoparticles, which were then characterized and evaluated for various therapeutic activities and A 549 breast cancer cell line for cytotoxic evaluation.Results: The Surface Plasmon Resonance exhibited a peak at 434 nm, and the FT-IR spectrum of St- AgNPs revealed the presence of secondary metabolites, which were used for stabilization and capping processes. The St-AgNPs showed an agglomerated spherical shape with a diameter of 10-35 nm. The elemental composition was silver (60.0%), oxygen (14.9%), sodium (14.9%), and carbon (15.0%). The St-AgNPs exhibited significant antioxidant activity in terms of DPPH 62.2 ± 2.1, H2O2 57.76 ± 2.4%, TAA 64.3±2.7, and NO 64.3 ± 2.7 at 100 μ/mL. The cytotoxic activity using A 549 Breast cancer cell line was found to be only 20 % of viable cells at 100μ concentration. St-AgNPs revealed good antibacterial efficacy against Streptococcus mutants, Klebsiella Sp. and Staphylococcus aureus (MRSA).Conclusion: The St-AgNPs may be a good choice for antibacterial, antioxidant and cytotoxic agents in the future with further relevant study and may be used in the field of nano biomedicine.

Background: Nigella sativa is a traditional plant with several ethno-medicinal activities. There have been several health advantages associated with Nigella sativa (Ns) L. oil, which has a high concentration of bioactive compounds.Method: This research aimed to examine the fatty acid methyl ester profiles, microbiological profiles, and aflatoxin profiles of cold-pressed Ns oils acquired from Turkish herbalists. For this, the fatty acids methyl esters (FAMEs) content and microbiological purity of 10 different Ns oils were examined.Results: The principal FAME components in Ns seed oils were linoleic (C18:2), oleic (C18:1), and palmitic acid (C16:0), with relative percentages of 34.17-57.54%, 19.41-30.52%, and 7.05-12.54%, respectively. The quantity of total saturated fatty acids (SFA) in all investigated oils ranged from 11.47 to 18.69%, while the amount of total unsaturated fatty acids ranged from 80.94 to 88.53%. Six of ten products (0.35-1.49%) were found to contain cis-11 eicosenoic acid, a chemical unique to Ns oil.Conclusion: Although no Aflatoxin was found in any of the samples, Enterobacteriaceae levels were exceptionally low, and yeast mold concentrations surpassed the Turkish Food Codex's permissible limit values.