Background Irritable bowel syndrome (IBS) is considered an anxious disease leading to undesirable pain. Phloroglucinol (PHG) and Trimethylphloroglucinol (TMG) are co-formulated as spasmolytic medication that is considered to be effective in reducing smooth muscle spasm. Dichloroaniline (DCL) is a specified PHG pharmacopoeial impurity which is needed to be monitored to avoid its toxic effects. Objective Different smart approaches were presented as a challenge to provide simple, reliable and economic spectrophotometric methods able to resolve the severe overlapping in the spectra of PHG and TMG in their pure and pharmaceutical forms, in addition to their estimation in the presence of DCL as PHG toxic impurity without any need for initial separation. Methods The presented work include univariate methods; Derivative ratio (DR), Ratio difference (RD), Mean centering (MC) and Deconvulated Fourier method (DF) which were able to determine PHG and TMG simultaneously in their binary mixture after DCL was estimated in the zero order, where the two drugs have zero absorption at 247.0 nm, and its contribution was eliminated by applying ratio subtraction method. Multivariate chemometric PLS and PCR models were also applied to determine PHG and TMG simultaneously in presence of DCL impurity. Results Univariate methods were applied in the range of 5.0–30.0, 2.5–25.0, and 1.0–12.0 µg/mL for PHG, TMG and DCL, respectively. The proposed chemometric models were used in the range of 6.0–14.0, 5.0–25.0 and 2.0–10.0 µg/mL for PHG, TMG and DCL, respectively. These analytical approaches succeeded in estimating the cited drugs in their pharmaceutical formulation and assessing content uniformity of dosage units. The methods were statistically compared with a reported HPLC method, and the results revealed no significance statistical difference. Conclusion This work provides for the first time univariate and multivariate PLS and PCR methods succeeded to assess PHG and TMG in presence of DCL as toxic impurity along with content uniform testing of dosage units. Highlights Comparative univariate and multivariate spectrophotometric analytical approaches was presented, for the first time, for estimation of spasmolytic formulation of PHG and TMG in the presence of Dichloroaniline (DCL) as PHG toxic impurity. Successful application to content uniformity testing of Stopspasm® dosage form. Statistical study including t-test and one way ANOVA was conducted.

Aim: Helicobacter pylori infection is a prevalent global bacterial infection that can potentially exaggerate symptoms of other serious infections like SARS-CoV-2 (COVID-19). Methodology: Herein, an efficient, accurate and cost-effective high-performance liquid chromatography-diode array detector method was developed and validated for determination of the novel triple therapy combination of tinidazole (TD), clarithromycin (CLR) and lansoprazole (LAN) in different analytical matrices (pharmaceutical formulation, dissolution media and spiked human plasma). Results: Successful chromatographic separation was achieved using Agilent Microsorb-MV 100–5 CN column (250 × 4.6 mm, 5 μm) and a mobile phase consisted of acetonitrile and 10.0 mM phosphate buffer, pH 7.5 ± 0.1 at flow rate of 1 ml/min via gradient elution. UV-detection was accomplished at 210.0 nm for CLR and 290.0 nm for TD and LAN. Conclusion: The developed method clearly provides a reliable, beneficial and cost-effective tool for quality control, dissolution testing and biological applications of the mentioned drugs.

No abstract

Nowadays, Green Analytical Chemistry is widely applied to provide various analytical methods with eco‐friendly procedures employing the least toxic, harmful reagents on humans and the environment without affecting the efficacy of the determination. Accordingly, two eco‐friendly, accurate, and reliable high‐performance thin‐layer chromatography‐densitometry and high‐performance liquid chromatographic methods were established for the determination and separation of two antispasmodic drugs, namely phloroglucinol and trimethylphloroglucinol in their pure, combined dosage form along with phloroglucinol toxic impurity, 3,5‐dichloroaniline. For high‐performance thin‐layer chromatography‐densitometry, efficient separation was developed via utilizing the stationary phase of high‐performance thin‐layer chromatography silica gel 60 F254 plates and developing a system comprising of ethyl acetate‐butanol‐ammonia in the ratio of 8.0:2.0:0.2, by volume and scanning of the developed bands at 210.0 nm. The subsequent method is isocratic high‐performance liquid chromatography with diode array detection in which separation was successively attained using XTerra RP‐C18 (250 × 4.6 mm, 5 μm) column as stationary phase and methanol‐10.0 mM phosphate buffer, pH 3.7 ± 0.1 as mobile phase in the ratio of 75.0:25.0, v/v at flow rate 1.0 ml/min and scanning at 220.0 nm. The developed liquid chromatography methods were validated according to the International Council for Harmonization guidelines, and all results acknowledged their efficacy. Additionally, the proposed methods worked well for assessing the cited drugs in binary combined commercially available pharmaceutical formulation. The greenness profile of the present methods was assessed and estimated using various assessment tools, namely; Green Analytical Procedure Index, analytical eco‐scale method, National Environmental Method Index in addition to Analytical GREEnness tool to evaluate the greenness of the provided methods with a statistical comparison between them to assess the more green ones.

Background Mitiglinide (MTG) is one of meglitinides group which are used for treatment of type two diabetes mellitus. Objective Mitiglinide (MTG) is a novel oral hypoglycemic drug. The present work adopts two stability-indicating chromatographic methods for determination of MTG after being exposed to forced degradation using 4 M methanolic HCl for 12 h. Methods The first method is HPTLC/densitometry using methanol:chloroform:acetic acid (5:2.5:0.3 by volume) as the eluting system and silica gel 60 GF254 as the stationary phase; the separated bands were then scanned at 220 nm. The second method is HPLC/UV in which acetonitrile:methanol:0.05 M potassium dihydrogen orthophosphate (pH 3.5) (40:25:35 by volume) was used as the mobile phase and a Zorbax SB-C8 (250 × 4.6 mm, 5 µm) column as a stationary phase, at a flow rate of 1 mL/min and UV detection at 220 nm. Results As a result of acid hydrolysis, two degradants were obtained. The first one was benzyl succinic acid to which this study was performed. The second one lacked configuration and was unreadable using UV spectrometry. Linearity was in the range of 8–48 µg/band MTG for HPTLC and 10–80 µg MTG for HPLC. LOD and LOQ values were 1.85 and 5.62 µg/band for the HPTLC method and 2.14 and 6.49 µg/mL for the HPLC method, respectively. The Recovery % was 100.03 ± 1.464 and 99.61 ± 1.44 using the HPTLC and HPLC methods, respectively. The relative standard deviations (RSD, %) for intra- and inter-day assays were 1.111 and 1.430 for the HPTLC method, respectively, and those for the HPLC method were 1.377 and 0.866, respectively. The RSD, %, for robustness testing was 1.162 (saturation time of mobile phase) and 1.592 (change in ratio of methanol content) for the HPTLC method and 1.377 (mobile phase composition), 1.713 (detector wavelength) and 1.770 (mobile phase flow rate) for the HPLC method. Conclusions The adopted methods were successfully applied for the determination of MTG in its pure form, in presence of its acid degradant and in its tablet dosage form. Highlights Statistical comparison between the results obtained from the developed methods and those obtained by the reported HPLC method showed no significance difference.