Current Pharmaceutical Analysis - Online First

The study emphasizes establishing a stability-indicating RP-UPLC method for concurrent estimation of pregabalin and etoricoxib in combined pharmaceutical formulations, confirming effective separation, sensitivity, and repeatability, validated according to ICH guidelines.

The present research study aims to establish a new stability-indicating RP-UPLC method for concurrently estimating pregabalin and etoricoxib in blended powder and their combined tablet formulation with less run time, high sensitivity, and specificity.

The effective separation of pregabalin and etoricoxib was achieved with HSS column C18 (150x2.1mm,1.8µm), 0.1% orthophosphoric acid:acetonitrile (65:35 v/v) at a flow rate of 0.3mL/min, and isocratic elution at 228nm. The elution of PRB and ETB was noticed at 1.56 and 2.01 minutes, with good resolution and system suitability with the developed approach.

Pregabalin and etoricoxib have shown linear responses from 18.75 to 112.5µg/mL and 15 to 90µg/mL, respectively. The range of the % RSD for intraday and inter-day precision was 0.33 to 0.81. The LOD and LOQ of pregabalin and etoricoxib were computed to be 0.07 µg/mL and 0.21 µg/mL, and 0.01µg/mL and 0.04 µg/mL, respectively, by standard deviation method. The validation method was carried out using ICH standards. The stability-indicating feature of the method was confirmed by the forced degradation studies where degradants generated by stress testing were clearly distinguished from the peaks of analytes.

The shorter elution period and superior sensitivity of both analytes with this method have been found to be appropriate for regular analysis of pregabalin and etoricoxib.

Since the International Olympic Committee (IOC) was established, sports doping control analyses have revealed a high rate of positive cases for cannabinoids. Cannabinoids were banned in all sports where they were used in competition as per the Prohibited List published annually. Further, it was also included in the threshold drug category. Consequently, developing a reliable method for urine Cannabinoids metabolite quantification plays a pivotal role in sports dope testing.

This work aimed to develop and validate a reliable, cost-effective, robust gas chromatography-tandem mass spectrometry method for detecting (−)-11-nor-9-Carboxy-Δ9-THC component in human urine samples, in compliance with ICH and WADA guidelines.

The sample preparation was done by enzymatic hydrolysis for deconjugation, further proceeded with solid phase extraction (SPE), liquid-liquid extraction (LLE), and using an XAD2 column, and N-methyl trimethylsilyl trifluoroacetamide (MSTFA) for derivatization.

The linearity was obtained in a range of 50–300 ng/mL, and the correlation coefficient was found to be higher than 0.99. Throughout the entire validation study, the difference in Retention Time (RT) for the analyte, including the Internal Standard (IS), was shown to be less than 1.0%. The quantification limit (LOQ) was calculated at a level of 50 ng/mL in human urine samples for the 3 most abundant ion transitions. The detection limit (LOD) was established at 4 ng/mL.

The accuracy, precision, linearity, recovery, quantification limit, and selectivity by GC-MS/MS technique were found acceptable and well satisfactory while following the ICH guidelines. The developed method has been proven to be fit for purpose in accordance with the enforced Guidelines of WADA.

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.

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.

Mangiferin shows great promise as a potent drug for a wide variety of diseases. Its low bioavailability and poor water solubility, however, restrict its therapeutic use.

The aim of the study goal was to systematically design a UV-spectroscopy method for mangiferin quantification in analytical samples that is quick, easy, and very sensitive. In order to validate the method, UV spectroscopy was used to check for specificity, accuracy, precision, and linearity. The models were constructed with Design Expert^Ⓡ V.10 and optimised using Box-Behnken Design (BBD), a three-factor and three-level procedure.

The devised method demonstrated good levels of sensitivity, specificity, accuracy, and precision, according to the results. The absorbance and concentration showed a strong linear relationship in the given 5-25 μg/ml range for several wavelengths, with correlation coefficients of 0.989, 0.982, 0.905, and 0.896 at 364.5, 370, 378, and 265nm, respectively. The intraday precision was 0.788 at 364.5 nm, 0.801 at 370 nm, 0.739 at 378 nm, and 0.721 at 256 nm for the concentration of 20 μg/ml. Particle size and entrapment efficiency, two dependent variables in the microspheres formulation, were best suited by the models derived when the observed responses were fitted to the design. Microspheres had a high entrapment efficiency and were microsized. Interestingly, drug-encapsulated microspheres containing mangiferin maintained the spherical shape.

The existence of well-resolved peaks and good recovery of mangiferin in the analytical method for analysis makes it ideal and acceptable for further use.