Current Pharmaceutical Analysis - Volume 20, Issue 8, 2024

Cordyceps sinensis, a renowned traditional Chinese medicinal substance, contains pharmacologically beneficial compounds, including γ-aminobutyric acid (GABA), necessitating efficient analytical methods for quality assessment. This study aims to develop a rapid, cost-effective, and eco-friendly liquid chromatography-tandem mass spectrometry (LC–MS/MS) method for GABA quantification in Cordyceps sinensis and its related species. The objective is to enhance the quality control standards within the Cordyceps sinensis industry and for those of its related species.

The study innovated a swift analytical procedure. Optimal conditions were determined through systematic evaluations of extraction solvents, durations, and chromatographic settings, prioritizing speed and solvent minimization.

The proposed LC–MS/MS method achieved precise quantification of GABA in a reduced time frame and significantly lowered solvent consumption, enhancing method efficiency by 22-fold compared to reported LC methods. The method exhibited robustness and scored the highest blue applicability grade index score, underscoring its suitability for academic and industrial applicaition.

The validated LC–MS/MS approach offers a sustainable avenue for the rapid and accurate measurement of GABA in Cordyceps sinensis and its related species, improving the quality control process and ensuring product authenticity. This method stands out as a model for green analytical chemistry, propelling forward the eco-friendly analytical evaluation of health-related compounds.

The objective of the present work is to develop and validate a novel, specific, precise, and reliable method for the estimation of Calotropis gigantea in bulk and herbal dosage form using the RP-HPLC method.

RP-HPLC analysis was performed using a C18 column of dimension 150×4.6mm, 5 µ. The chromatography system comprised an Agilent 1220 Infinity II LC equipped with a VWD detector and a 1220 Infinity II LC binary pump, wherein the instrument operation was managed through Control Panel software at a flow rate of 0.5 ml/min. Methanol: water in the ratio of 55:45 was used as the mobile phase, and the effluents were analyzed at 275nm. The proposed method was validated for various parameters like linearity, precision, accuracy, robustness, ruggedness, selectivity, limit of detection, limit of quantification, and assay as per the ICH Q2(R1) guidelines.

Linearity was noted over a concentration range of 50-250 µg/ml with a correlation coefficient of 0.999. The limit of detection (LOD) and limit of quantification (LOQ) were determined to be 16.02 and 48.56 µg/mL, respectively. The % RSD for interday and intraday precision studies was less than 2%, which was within the official RSD limit. Recovery analysis performed using marketed formulation was found to be in the range of 97-105%.

The method developed was validated according to the ICH guidelines. Hence, it is evident that the developed method is novel, sensitive, precise, and reliable, and it can be successfully applied to estimate Calotropis gigantea in bulk material and its herbal dosage form.

The in-vitro release test (IVRT) is a tool to measure the amount and the release rate of active pharmaceutical compounds released from topical semisolid dosage forms. The IVRT provides significant information for product performance assessment and evaluation. It is also used to assess the bioequivalence study (biowaivers) for topical semisolid products.

The study aims to develop and validate the IVRT method for qualitative and quantitative estimation of ganciclovir topical products and to demonstrate the similarity between the marketed reference product and the in-house test product of ganciclovir ophthalmic gel.

The method was developed using a vertical diffusion cell with a synthetic cellulose membrane, simulated tear fluid as the receiver media, and UV detection. The IVRT study was performed at 100rpm and 32℃ for 6hr. The marketed formulation containing 0.15%w/w ganciclovir was used as a reference.

The in-house test product of ganciclovir met all characterization criteria. The analytical method was optimized and validated with a concentration range of 2-14μg/ml and a regression coefficient of 0.9997 as per the ICH guideline. The developed IVRT method was simple, economical, linear, robust, reproducible, sensitive, specific, and selective to evaluate the drug release from the formulation. The %recovery at 6hr was found to be 84.43% and 78.68% for reference and test product of ganciclovir ophthalmic gel with correlation coefficient R² 0.9947 and 0.9921, respectively, this value justified the biowaivers between the reference and test formulation.

This method can be utilized to check topical semisolid product quality, product performance, and product uniformity. Additionally, it can also be used to waive the requirement for bioequivalency studies for ganciclovir ophthalmic gel.

N-nitrosamines have recently been discovered in metformin hydrochloride and other generic drugs. To quantify the five N-nitrosamines in metformin hydrochloride, we devised sensitive and reliable multiple reactions monitoring mode-based GC-MS/MS technique, particularly, N-nitrosodiethy amine (NDEA), N-nitroso ethyl isopropylamine (NEIPA), N-nitrosodiisopropylamine (NDIPA), N-nitrosodipropylamine (NDPA), as well as N-nitrosodibutylamine (NDBA).

To develop a sensitive, precise, and accurate MRM mode based GC-MS/MS method for the quantification of five N-nitrosamines in metformin hydrochloride and valídate as per ICH guidelines.

The settings for mass spectrometry and gas chromatography were optimized. With the linearity, sensitivity, specificity, accuracy, and precision of the parameter, the procedure was as per the recommendation of ICH: International Council for Harmonization guidelines.

N-nitrosamines in metformin hydrochloride had detection and quantification limits of 0.001 ppm and 0.004 ppm, correspondingly. The obtained results were within the sensitivity limitations issued by the US Food and Drug Administration. The calibration curve's regression coefficients for five N-nitrosamines were over 0.99, demonstrating the process's good linearity. The retrievals of N-nitrosamines in metformin hydrochloride between 97.1 – 127.4%. The RSD (Relative Standard Deviation) was lower than 10% for both inter-day and intra-day precision studies.

The proposed method exhibited a rapid analysis capability, high accuracy, sensitivity, and precision, making it a trustworthy method for monitoring N-nitrosamines in metformin hydrochloride.