Current Pharmaceutical Analysis - Volume 19, Issue 10, 2023

Cervical cancer is one of the most prevalent forms of cancer occurring across the world and it has been observed that about 99.7% of cervical cancer cases occur due to infections with the Human papillomavirus (HPV). Over prolonged durations, cervical cancer can lead to complications such as vaginal bleeding, itching, and in more severe instances, even the fatality of the individual. Cervical cancer is an essential cause of death at an early age as it affects young women higher than other populations. The most frequent drugs used in its treatment include antiangiogenic drugs. This review summarizes analytical techniques used for the quantification of anti-angiogenic agents- Bevacizumab, Sunitinib, Pazopanib, Brivanib, and Imatinib. Furthermore, an in-depth description of numerous techniques including NIR (1), HPLC (10), LC-MS (28), and HPTLC (1) approaches used to determine and quantify these agents have been provided in this review. Based on the matrix utilized, the following details were discussed: analytical conditions, detection limits, and solvent used in sample preparation. Our review holds significant importance within the scientific community, offering valuable insights into commonly employed measurement techniques and the latest advancements in these approaches.

Veterinary drug residues in foods pose risks to consumers and promote antimicrobial resistance. Effective detection methods are needed to monitor and control residues. Recent advancements in analytical techniques for veterinary drug residue detection were reviewed. Key sample preparation methods, including QuEChERS, SPE, ASE, and LLE, were summarized. Instrumental analysis techniques including LC-MS/MS, GC-MS, immunoassays, CE and biosensors were examined. Recent trends and future directions were identified. LC-MS/MS and GC-MS provide the highest sensitivity and specificity for veterinary drug residue analysis. However, selectivity remains a challenge, particularly for complex matrices like meat and liver. Multi-residue methods now cover over 100 analytes, but analyzing new and legacy drugs lacking established methods is difficult. Increased sensitivity has been achieved through UHPLC and high resolution MS, but detection limits below 1 μg/kg often remain elusive. sSimplified onsite tests are gaining interest. More selective extraction strategies, data-driven multi-residue methods, microflow LC, and integrated analytical platforms may help address current challenges. Continued advances in sample preparation, instrumentation, data processing, and validation will be needed to fully realize the potential of veterinary drug residue detection and ensure food safety.

Background: N-nitrosodimethylamine (NDMA) are a sort of genotoxic impurities (GTIs) having strong carcinogenic effects and obvious hepatotoxicity. To monitor the NDMA content of metformin hydrochloride sustained-release tablets and enteric capsules in China from 2018 to 2022, a GC-MS/MS method was established and validated.Materials and Methods: The chromatographic column was Agilent VF-WAXms capillary column (30 m.25 mm, 0.25 μm). The GC-MS/MS method was equipped with multiple reaction monitoring (MRM) modes. To assess the quantity of NDMA, the molecular ion at mass-tocharge (m/z) of 74-44 was monitored under the 6 V collision energy, and to assess the quality of NDMA monitoring, the molecular ions at m/z 74-42 were determined. A total of 143 batches of metformin hydrochloride-finished products from 35 enterprises were determined by this method.Results: The linear range of the method was 0.25 ~ 50.00 ng/mL, r = 0.9998, S/N > 10, and the limit of detection and quantitation were 0.06 ng/mL and 0.21 ng/mL, respectively. The average recovery was 98.62%, and the RSD was 4.31%. All batches of enteric capsules met the requirements; 38.21% of the 123 batches sustained-release tablets still exceeded the acceptable daily intake.Conclusion: The presented method is sensitive, accurate, precise, and available for both enteric capsules and sustained-release tablets of metformin hydrochloride, which can provide a reference for their quality control. The over-limit phenomenon of NDMA in metformin hydrochloride products poses new challenges and requirements for both the State Drug Administration and enterprises.

Background: A high-performance liquid chromatography (HPLC) method was developed for the determination of Pantoprazole Sodium (PPZ) in the presence of its degradation products. The degradation of PPZ was studied in simulated intestinal fluid (SIF) and simulated gastric fluids (SGF) in various temperature conditions.Aim: This study aimed to establish a simple, sensitive, and rapid RP HPLC method for in-vitro determination of Pantoprazole Sodium and its degradation products in simulated gastric and intestinal fluids.Objective: Pantoprazole is acid labile drug. In order to determine pantoprazole in various oral dosage forms, the stability-indicating assay of PPZ was performed in phosphate buffer (pH 6.8) representing simulated intestinal fluid (SIF) and in 0.1 molars (M) Hydrochloric acid (HCl) as simulated gastric fluid (SGF) at two different temperature conditions, i.e., 25°C and 0°C, respectively.Methods: Pantoprazole sodium was obtained from the Akums laboratory in Haridwar. The analysis was performed by high-performance liquid chromatography (HPLC), Shimadzu, equipped with two LC-10 AD VP solvent-delivery modules, a SPD-10A UV–-visible detector, and a manual injector valve with 20 μL sample loop. Phenomenex ODS analytical column (150 mm 4.6 mm i.d., 5 μm particles) was done under reversed-phase partition chromatographic conditions. The mobile phase was phosphate buffer and acetonitrile (ACN) of pH 7.4, respectively, optimized in a 70:30 (v/v) ratio followed by filtration through a 0.45 μm membrane filter and degassed by ultrasonicator before use. The mobile phase was delivered at the flow rate of 2 mL/min. The various parameters, such as linearity, accuracy and precision of the analytical method, were studied.Results: The standard curve of PPZ was linear (R2>0.99) over the concentration range of 5-30 μg/mL, and the relative standard deviation (RSD) values for intra-day and inter-day variations were in the range of 1.0-1.8%. The range of RSD was within ±2.Conclusion: The stability of PPZ in aqueous solution was pH dependent. The rate of degradation increases with decreasing pH. The pH stability of pantoprazole was studied at the above-mentioned temperature conditions. The PPZ peaks were analyzed by comparing them with fresh samples and were stable in SIF solution after 24 hours elapsed time at pH 6.8. The obtained degraded peaks in SGF (pH 1) were successfully separated from the PPZ.

Background: Recently, a combination prescription with the main ingredients sitagliptin and dapagliflozin as dipeptidyl peptidase-4 andsodium–glucose cotransporter-2 inhibitors, respectively, for the treatment of type 2 diabetes has widely been issued in hospitals. However, the development of double-layered tablets requires simultaneous quantitative dissolution tests that are significantly efficient and cost-effective.Objective: Individual analysis of the two active pharmaceutical ingredients (APIs) incurs more than twice the time and cost. Consequently, this study aimed to develop a dissolution analysis method that simultaneously quantifies the APIs dapagliflozin and sitagliptin in multi- layered tablets. This simultaneous quantitative dissolution analysis can dramatically reduce analysis time and cost.Methods: For reversed-phase high-performance liquid chromatography (RP-HPLC) analysis using ultraviolet detection, a Zorbax C18 column (4.6 150 mm, 5 μm) was used, and the flow rate was 1.5 mL/min, injection amount 20 μL, and maximum absorption wavelength set to 205 nm. Additionally, the analysis time was set to 1.5 times the retention time of dapagliflozin.Results: The retention times of dapagliflozin and sitagliptin were 11.57 and 2.56 min, respectively. Further, their relative standard deviations were 0.11% and 0.05%, respectively. Quantitative analysis using RP-HPLC confirmed no peak interference between the APIs and excipients. Both APIs exhibited linearity at a 20–120% concentration.Conclusion: The dissolution method developed in this study can quantify both APIs simultaneously, thereby reducing analysis time and cost by more than 50% and increasing efficiency in the pharmaceutical industry.

Background: The liver perfusion method is frequently used in drug pharmacokinetic studies and the various effects of drugs on liver tissue. The aim of this study was to establish and validate an analytical method using high-performance liquid chromatography to determine the simultaneous concentration of losartan and its active metabolite, EXP-3174, in an isolated perfused rat liver study.Method: An HPLC system with isocratic mode was used. Various chromatographic parameters were adjusted to develop and validate a method for determination of losartan and its active metabolite in liver perfusion media.Results: In this study, losartan and its active metabolite, EXP-3174, were separated using a C18 stationary phase, a mobile phase consisting of acetonitrile: phosphate buffer at a flow rate of 1 mL.min-1, and UV detection at 254 nm. Retention times for losartan and the metabolite were 10 and 16 minutes, respectively. Linearity from 25-250 ng.ml-1 was validated with acceptable accuracy and precision. The LOD and LOQ for losartan were 7.0 and 21.1 ng.ml-1, respectively. The LOD and LOQ for metabolite were 7.4 and 22.4 ng.ml-1, respectively. ChromGate® software was used to acquire and process the data.Conclusions: The optimized and validated technique was effectively used to analyze losartan and its active metabolite in isolated perfused rat liver.