High-performance Liquid Chromatographic Method Research Articles

LITERATURE REVIEW ON HPLC METHODS FOR ESTIMATION OF EMTRICITABINE AND TENOFOVIR DISOPROXIL FUMARATE TABLETS

Emtricitabine and Tenofovir Disoproxil Fumarate (TDF) are essential components of antiretroviral therapy (ART) for HIV infection. Accurate quantification of these drugs in pharmaceutical formulations is crucial for ensuring therapeutic efficacy and patient safety. High-Performance Liquid Chromatography (HPLC) is a widely used analytical technique for this purpose. Several validated HPLC methods have been developed, employing diverse chromatographic conditions and detection techniques. These methods typically utilize reversed-phase C18 columns and UV detection at 260 nm or 270 nm. Key considerations for method development include selectivity, sensitivity, accuracy, precision, linearity, and robustness. Additionally, other analytical techniques such as UltraHigh Performance Liquid Chromatography (UHPLC), Thin-Layer Chromatography (TLC), Fourier Transform Infrared Spectroscopy (FTIR), and Ultraviolet-Visible (UV-Vis) Spectroscopy have been explored for the analysis of Emtricitabine and TDF. However, HPLC remains the preferred method due to its versatility, sensitivity, and reliability.

Study of the Acidic, Basic, and Thermal Degradation Kinetics of Three Antihypertensive Drugs-Individually and in Combination.

The importance of fixed-dose combinations (FDCs) for the treatment of hypertension is well established. However, from a stability perspective, FDCs present a challenge since the degradation of one active pharmaceutical ingredient (API) can be affected by the presence of another API. The aim of this study was to compare the degradation behaviors and evaluate the degradation kinetics of three antihypertensive drugs, perindopril tert-butylamine (PER), amlodipine besylate (AML), and indapamide (IND). The degradation processes were studied using the previously developed reverse phase high-performance liquid chromatographic (RP-HPLC) method after exposing each drug individually, as well as the combinations of two/three drugs, to different stress factors, such as light, oxidation, acidic, basic, or neutral pH values at different temperatures. The results show that PER is most unstable under basic conditions and that AML displays a negative, while IND displays a positive effect, on PER stability when combined. AML is most affected by basic conditions and oxidation, and its stability is affected by both drugs positively; IND undergoes extreme photolysis, which is positively affected by AML but negatively by PER. Great care must be taken when formulating FDCs with these three drugs, as well as solutions or oral suspensions adjusted for geriatric or pediatric populations, since the stability of all three drugs is greatly affected by pH conditions, as well as light or oxidation factors and their interactions.

Identification of lu’an Guapian at different picking periods by using excitation–emission matrix fluorescence spectroscopy coupled with chemometrics

Lu’an Guapian (LAGP) is a renowned green tea, with its price significantly higher when picked before the Qingming Festival compared to after, posing risks of confusion and counterfeiting. This study proposed using an excitation-emission matrix (EEM) fluorescence method combined with chemometrics for rapid identification of tea picked before and after Qingming Festival. Firstly, the differences among the EEM fingerprints of different tea samples were analyzed using the alternating trilinear decomposition (ATLD) algorithm. To determine the differences between LAGP before and after Qingming Festival, the total contents of ten main components in tea were detected, and their effects on the EEM fluorescence fingerprint of tea were analyzed using correlation heatmaps. Finally, two chemometric algorithms, partial least squares discriminant analysis (PLS-DA) and k-nearest neighbor (k-NN), were used to classify LAGP before and after Qingming Festival, achieving a classification accuracy of 100% for the training set, test set, and prediction set. To further explore the potential of this method, LAGP was further classified in detail according to four detailed picking periods, achieving an accuracy of over 83%. The same chemometric algorithm was used to classify the data based on the high-performance liquid chromatography (HPLC) method, yielding results comparable to those of the EEM-based method, though slightly inferior. Variable importance projection (VIP) analysis shows that catechin analogs are the main contributors to the classification of LAGP. The results demonstrated the EEM method’s significant potential in identifying the picking time of green tea.

Development of a liquid chromatography method for the analysis of oil extract of artemisia cina

Introduction. The problem of development and implementation of own drugs in Kazakhstan today is acute and urgent. The solution to this problem is possible through the use of own resources – domestic medicinal plant raw materials. A promising medicinal raw material is Artemisia cina – an endemic medicinal plant of the of the Turkestan region of Kazakhstan.Aim. Designing a liquid chromatography methodology to analyze the oil extract obtained from Artemisia cina.Materials and methods. Standard sample (SS) of santonin, Artemisia cina’s oil extract. The substance was identified and quantitatively determined using an Agilent Technologies 1200 liquid chromatograph (USA) equipped with ChemStation software.Results and discussion. The main active substance of the oil extract was analyzed using high-performance liquid chromatography (HPLC) method. Choosing the separation conditions for the column involves determining the best composition of the mobile phase and the rate of elution. There were used a reversed-phase system with sorbent C18 and a mobile phase consisting of acetonitrile and a phosphate buffer with a pH of 6.8. Chromatographic studies of the substance were carried out in a gradient mode at an analytical wavelength of 237 nm. The retention time of the standard sample (SS) of santonin matched the retention time (tR) of santonin isolated from the oil extract of Artemisia cina and amounted to 14.3 minutes.Conclusion. A liquid chromatography method has been established for the identification and quantitative determination of the oil extract, focusing on the main active substance, santonin.

LITERATURE REVIEW ON HPLC METHODS FOR ESTIMATION OF EMTRICITABINE AND TENOFOVIR DISOPROXIL FUMARATE TABLETS

Emtricitabine and Tenofovir Disoproxil Fumarate (TDF) are essential components of antiretroviral therapy (ART) for HIV infection. Accurate quantification of these drugs in pharmaceutical formulations is crucial for ensuring therapeutic efficacy and patient safety. High-Performance Liquid Chromatography (HPLC) is a widely used analytical technique for this purpose. Several validated HPLC methods have been developed, employing diverse chromatographic conditions and detection techniques. These methods typically utilize reversed-phase C18 columns and UV detection at 260 nm or 270 nm. Key considerations for method development include selectivity, sensitivity, accuracy, precision, linearity, and robustness. Additionally, other analytical techniques such as Ultra-High Performance Liquid Chromatography (UHPLC), Thin-Layer Chromatography (TLC), Fourier Transform Infrared Spectroscopy (FTIR), and Ultraviolet-Visible (UV-Vis) Spectroscopy have been explored for the analysis of Emtricitabine and TDF. However, HPLC remains the preferred method due to its versatility, sensitivity, and reliability.

A Pharmacokinetic Study of the Interaction Between Regorafenib and Paracetamol in Male Rats.

Background: In clinical practice, the prevalent problem of polypharmacy could result in increased risks of drug-drug interactions. Regorafenib (REG) is commonly co-administered with paracetamol (PA) as a treatment protocol in cancer patients with pain therapy. Purpose: This study aimed to demonstrate the effect of paracetamol on the pharmacokinetic parameters of regorafenib and its metabolites following a single administration of both substances in rats. Additionally, the influence of REG and its metabolites on the pharmacokinetics of paracetamol was also determined. Methods: Twenty-four rats were divided randomly into three groups: REG group (IIREG, regorafenib 20 mg/kg, n = 8), PA group (IIIPA, paracetamol 100 mg/kg, n = 8), and REG+PA co-administration group (IREG+PA, REG 20 mg/kg and PA 100 mg/kg, n = 8). The concentrations of regorafenib, regorafenib-N-oxide (M-2), and N-desmethyl-regorafenib-N-oxide (M-5) were determined using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The plasma concentrations of PA and its glucuronide (GPA) and sulfate (SPA) metabolites were measured using the validated high-performance liquid chromatography method with ultraviolet detection (HPLC-UV). The pharmacokinetic parameters were calculated using a non-compartmental model. The statistical evaluation was performed in the SAS program. Results: After the administration of PA, the Cmax and AUC0-∞ of REG increased by 890% and 1140%, respectively; for M-2, they increased by 220% and 170%, and for M-5, by 2130% and 1730% (Cmax and AUC0-∞, respectively). A difference in the ratio of M-2/REG for AUC0-∞ and Cmax between the groups was observed, but not for M-5/REG. The AUC0-∞ for PA and GPA decreased by 20.7% and 51.1%, respectively, when PA was co-administered with REG. But the AUC0-∞ for SPA increased by 91.35% in the IREG+PA group. A difference in the ratio of GPA/PA for Cmax and for SPA/PA for AUC0-t and AUC0-∞ between the groups was observed. Conclusions: Paracetamol increased the plasma exposure of regorafenib, M-2, and M-5, which may exacerbate the drug's side effects. In contrast, REG reduced paracetamol exposure and contributed to its faster elimination, which may reduce the analgesic and antipyretic effects of paracetamol. These findings suggest clinical relevance for oncology patients requiring analgesic treatment.

Fabrication of a molecularly imprinted poly(methyl methacrylate) decorated graphite electrode for detection of aloe emodin in Aloe vera

In this work, the authors represent a comprehensive approach for the development and validation of a novel graphite-supported molecularly imprinted poly(methyl methacrylate) electrode for the selective and sensitive detection of aloe emodin (AE) in aloe-based cosmetic products. The electrocatalytic activity of the electrode was evaluated using cyclic voltammetry and differential pulse voltammetry techniques in phosphate buffer saline. Surface morphology, structural characteristics, and imprinting endorsement were investigated using field emission scanning electron microscopy, Fourier-transform infrared spectroscopy, and UV-Vis spectroscopy. Under the optimal conditions, the electrode showed an oxidative differential pulse voltammetry peak at -0.2931±0.011 V (vs. Ag/AgCl, saturated KCl). The current was increased linearly with increasing concentrations of AE from 0.0005 to 350 µM, with a low detection limit of 0.0003 µM. The voltammetric analysis has been validated by reverse-phase high-performance liquid chromatography (RP-HPLC) methods. A partial least square regression model was developed to correlate the results obtained from the proposed system with the reference values obtained by RP-HPLC. The model showed a high prediction accuracy of 95.95 % for the detection of AE in cosmetic samples. The developed electrode provides a low-cost, rapid, easy, and convenient method for the detection of AE in cosmetic products, offering potential benefits for quality control and safety assessment in the cosmetic industry.

Assessment of miligram(Mg) content of some notable analgesics used by residents of Maiduguri Metropolis: evidence from high performance liquid chromatographic technique

Diclofenac sodium and paracetamol are Over the counter (OTC) medications used as analgesic and antipyretic agents to relieve pains, fever and headaches. The aim of this work was determine the mg content of paracetamol and diclofenac sodium in selected samples across the Maiduguri metropolis using High Performance liquid chromatography (HPLC) method. For paracetamol samples an intersil ODS-3V column (150 mm × 4.6 mm; 5 μm pore size) was used at the temperature of 35oC the mobile phase was methanol: water (20:80) using isocratic elution at the flow rate of 2 mL/min, injection volume of 10 μL and a diode array detector. For diclofenac sodium samples, the chromatographic conditions were the same except the mobile phase which was methanol: water (63:37), flow rate of 0.8 mL min, injection volume of 20 μL and column temperature was set at 30 oC. A total of 45 samples were analysed; which comprised of paracetamol tablet, paracetamol syrup and diclofenac sodium tablet which were randomly selected from three different sources; hospital pharmacy, community pharmacy and drug patent stores. The percentage mg content for paracetamol tablets ranged from 48 to 83 % while that of the paracetamol syrups ranged from 72 to 120 % and finally diclofenac sodium tablets ranged from 73 to 174 %. Adopting the United State Pharmacopoeia (USP) as reference for assessment tool, it was observed that all the paracetamol tablet samples failed, 4 out of 15 paracetamol syrup samples failed, and 11 out of 15 diclofenac sodium tablet samples failed. There was statistical significance (p< 0.05) between class of drug and percentage mg content but there was no significance (p< 0.05) between source of drug and percentage constituent. HPLC technique was used successfully for quantitative determination of paracetamol and diclofenac sodium dosage forms.

Determination of 3-hydroxyanthranilic acid in the sweat of healthy older adults

3-Hydroxyanthranillic acid (3HAA) is one of the key metabolites from the tryptophan (TRP) metabolism pathway and is associated with aging, age-associated diseases, and healthy lifespan extension. This study aims to detect 3HAA in the sweat of healthy older adults using simple, high-performance liquid chromatography (HPLC) method. Chromatographic separation using 20 mmol/L sodium acetate, 3 mmol/L zinc acetate, and 7% (v/v) acetonitrile as mobile phase is possible to simultaneous detect 3HAA, KYN, and TRP with UV and fluorescence detection, respectively, under 6 min. This method demonstrated excellent linearity with coefficient of determination (r2) greater than 0.998 for all analytes. The linear range were 0.05–6 µg/mL for TRP, 0.1–6 µg/mL for KYN and 0.2–6 µg/mL for 3HAA. Percentage recoveries from spiked in human sweat ranged from 90 ± 7–101 ± 3 for TRP, 86 ± 1–92 ± 3 for KYN, and 96 ± 1–103 ± 4 for 3HAA. The precision (%RSD) of repeatability and reproducibility is less than 3% and 6%, respectively. This method was used in a cross-sectional study with 81 participants aged 50–79 years, selected randomly from a local primary healthcare hospital’s sampling frame. A detectable amount of 3HAA was observed in all sweat samples, marking the first report of 3HAA presence in human sweat. Additionally, the results revealed that the 3HAA sweat levels increased with age analyzed in three different age groups ranging from 50–59, 60–69, and 70–79. These findings enhance our understanding of sweat profiles and their correlation with aging, potentially further improving early diagnosis, disease monitoring, and development of customized treatment programs for older adults.

Salivary glycated albumin could be as reliable a marker of glycemic control as blood glycated albumin in people with diabetes

AimsMeasurements of diabetes-related biomarkers are necessary to assess glycemic control. The commonly used finger-prick blood glucose and HbA1c measurements are invasive, as is blood glycated albumin (GA) measurement. Therefore, we developed a non-invasive method, namely, measurement of the salivary GA with high accuracy using a high-performance liquid chromatography (HPLC) method. MethodsWe recruited participants with diabetes mellitus admitted to The University of Tokyo Hospital. Blood and saliva samples were collected at three time points (fasting and 2-hour postprandial at admission and fasting at discharge). After partial purification using an antibody-based column, the samples were subjected to GA measurement by HPLC method. ResultsAmong the 56 participants with diabetes mellitus enrolled in the study, there was a correlation between the GA levels measured in blood and saliva at the three time points described above (n = 45, R2 = 0.985, P < 0.001; n = 48, R2 = 0.973, P < 0.001; n = 51, R2 = 0.979, P < 0.001). Multiple regression analysis revealed the associations were maintained even after adjustments for age, BMI, and nephropathy stage. ConclusionsThis exploratory research revealed that the salivary GA levels by this method were accurate and might be able to replace blood GA measurement. The home salivary GA measurement is expected to be developed that may reduce the burden and complications in people with diabetes mellitus and improve the quality of life.

Developing and Validation of a High-Performance Liquid Chromatography Method for the Determination of Combined Perindopril, Indapamide and Amlodipine from Pharmaceutical Preparations

High Performance Liquid Chromatographic method was developed and validated for the analysis of a pharmaceutical preparation (TRIPLIXAM®) consist of Perindopril (PRN), İndapamide (IND) and Amlodipine (AML) which are used for the control of hypertension in patients with high blood pressure. In this developed HPLC method, ACE 5 C18 analytical column (12.5 x 4.6 mm) was used for the analysis of PRN, IND and AML. Acetonitril and 50 mM phosphate buffer mixture (40:60 v/v) was used as mobile phase. Measurements were obtained at 215 nm wavelength using UV detector. Retention times of PRN, AML and IND were 2.22, 3.48 and 5.05 min. respectively, at selected chromatographical conditions. The developed HPLC method was validated in terms of stability, accuracy, sensitivity, linearity, precision, specificity, ruggedness and robustness in accordance with ICH analytical method. Linear calibration curves were obtained in the range of 1.0-25.0 ppm; 1.0-8.0 ppm and 1.0-40.0 ppm for PRN, IND and AML, respectively. In this HPLC method the limit of dedection values (LOD) for PRN, IND and AML were 0.25 ppm, 0.10 ppm and 0.15 ppm while limit of quantification values (LOQ) were 0.50 ppm, 0.25 ppm and 0.40 ppm, respectively.

Bioconversion of mango peels into itaconic acid through submerged fermentation and statistical optimization of parameters through response surface methodology.

Itaconic acid is an industrially crucial organic acid due to its broad range of applications. The main hurdle in itaconic acid production is the high cost of the substrate, i.e., pure glucose, required for the fermentation process. Pakistan annually produces about 1.7 to 1.8 million metric tonnes of mango fruit. Keeping this in view, the potential of a sugar-rich fruit by-product, i.e., mango peels, was analyzed to be used as a substrate for the biosynthesis of itaconic acid using Aspergillus niger by submerged fermentation. Different physicochemical parameters (incubation period, temperature, agitation rate, inoculum size, and pH) were optimized using the central composite design (CCD) design of response surface methodology (RSM). The maximum production of itaconic acid, i.e., 4.6 g/L, was analyzed using 10% mango peels w/v (water hydrolysate), 3 mL inoculum volume after 5 days of fermentation period at pH 3, and a temperature of 32 °C when the media was kept at a 200-rpm agitation speed. The itaconic acid extraction from mango peels was done using the solvent extraction method using n-butanol. The identification and quantification of itaconic acid produced in the study were done using the Fourier Transform Infrared Spectroscopy (FTIR) spectrum and the High-Performance Liquid Chromatography (HPLC) method. According to HPLC analysis, 98.74% purity of itaconic acid was obtained in the research. Hence, it is concluded from the results that sugar-rich mango peels can act as a promising substrate for the biosynthesis of itaconic acid. Further conditions can be optimized at the bioreactor level to meet industrial requirements.

Quality control analyses of selected honey samples from Serbia based on their mineral and flavonoid profiles, and the invertase activity

Abstract Nowadays, climate changes induce deviations in the composition of honey varieties characteristic of a specific geographic region. Therefore, according to Codex Alimentarius for honey, the slight variations in values of determined parameters cannot be strictly regarded as a sign of its adulteration. Here, modified methods are presented for preparing honey samples for inductively coupled plasma-optical emission spectroscopy (ICP-OES) analysis and the high-performance liquid chromatography (HPLC) method to use them as fast and reliable methods in the food industry. ICP-OES analysis suggested that all analysed honey samples are natural, and HPLC-DAD (diode-arrray detection) analysis on the flavonoids showed that one sample is probably not natural. Invertase activity showed an overlap with this HPLC-DAD finding but suggested more samples as possibly adulterated, which can be neglected due to possible thermal treatment of those natural samples, causing a decrease in invertase activity. Therefore, results obtained from the analyses of investigated honey samples based on the mineral content, number, and quantity of flavonoids, together with the invertase activity, indicated that the combination of analyses could be a reliable tool for determining the quality of honey samples.

Validation of chromatographic methods, TLC and HPLC, to quantify known radiochemical impurities and the radiochemical purity the radiopharmaceutical [177Lu]Lu-PSMA I&T

The Energy and Nuclear Research Institute (IPEN) is studying the production of the radiopharmaceutical [177Lu]Lu-PSMA I&T, in accordance with the good manufacturing practices recommended by the National Health Surveillance Agency (ANVISA), to be used in the therapy of prostate cancer. This work aims to validate chromatographic methods, Thin-Layer Chromatographic (TLC) and high-performance liquid chromatography (HPLC), to determine the radiochemical purity (RCP) of the product. The entire validation process of this work was based on ANVISA's RDC 166, 2017 and the Guide 10, version 1, 2017, guided the statistical treatments adopted. With the selectivity study we can observe that the presence of impurities or excess excipients in the sample does not interfere with the quantification of the product. The proposed methods were linear with linear correlation coefficients (r) above 0.99. The precision and repeatability presented relative standard deviation values lower than specified (RSD <5 %). The small controlled variations in the method suggested for the robustness test also did not affect the radiochemical purity of the product. In view of the results and in accordance with the criteria established by the National Health Surveillance Agency (ANVISA), the two chromatographic methods were validated in accordance with RDC 166, 2017, proving to be selective, precise, linear and robust. The validation of TLC and HPLC methods enables their application in the batch release routine of the new radiopharmaceutical at Radiopharmacy Center of IPEN.

Multitarget Phytocomplex: Focus on Antibacterial Profiles of Grape Pomace and Sambucus ebulus L. Lyophilisates Against Extensively Drug-Resistant (XDR) Bacteria and In Vitro Antioxidative Power.

Objectives: This study was conceived with the aim of translating the experience and knowledge of the research group into the design and creation of multi-active phytocomplex cocktails from lyophilised winery by-products (Grape Pomace-GP) and weeds (Sambucus ebulus L., Dwarf Elder-DE). Methods: Quantification of bioactive molecules was performed by high-performance liquid chromatography (HPLC) method. Results: In the extract obtained from lyophilised GP, the most dominant component that was quantified was petunidin-3-glucoside. Prominent compounds that were quantified in DE extract were cyanidin derivatives. The total number of microorganisms in lyophilisates is low, but some of them still survive lyophilisation. Antibacterial activity was determined by microdilution, the minimum inhibitory concentration (MIC) of the tested bacteria ranged from 0.78 mg/mL to 25.00 mg/mL. Antibacterial susceptibility testing (AST) revealed that Klebsiella spp. and Acinetobacter baumannii complex are extensively drug-resistant (XDR). Conclusions: The GP + DE cocktail showed very strong AB power against both tested XDR bacteria. The total phenolic content and antioxidative effect (determined spectrophotometrically) indicate their linear correlation.

Swertia cincta and its main active ingredients regulate the PPAR-α pathway in anti-cholestatic liver injury

Ethnopharmacological relevanceSwertia cincta is a traditional remedy for cholestasis commonly utilised in Yunnan, China. Despite its widespread use, the specific active components and underlying mechanisms of action remain poorly understood. Aim of this studyThis study aimed to investigate the therapeutic properties, mechanisms, and active compounds of Swertia cincta in an animal model of cholestasis induced by alpha-naphthylisothiocyanate (ANIT). Materials and methodsUHPLC/Q-TOF-MS and high-performance liquid chromatography (HPLC) were utilised to analyse the blood components of Swertia cincta. An ANIT-induced cholestatic liver injury animal model was established, and metabolomics was employed to explore the potential mechanisms of Swertia cincta in treating cholestatic liver injury. Hepatocellular injury induced by taurochenodeoxycholic acid was evaluated in vitro, and key bioactive components of Swertia cincta for cholestatic liver injury treatment were identified and confirmed using the ANIT-induced mouse model. ResultsThe established HPLC method demonstrates good specificity and reproducibility, enabling the simultaneous determination of six components in Swertia cincta. Results from serum biochemical indicators and liver pathology analysis indicated that Swertia cincta exhibits promising anti-cholestasis liver injury effects. Specifically, gentiopicroside, loganic acid, and isoorientin were identified as key active ingredients in treating cholestatic liver injury. Their mechanism of action primarily involves regulating PPAR-α, FXR, CYP3A4, NTCP, CAR, and CPT2. By modulating PPAR-α and bile acid metabolism-related proteins, reducing pro-inflammatory factors, enhancing bile acid transport, and promoting fatty acid oxidation to reduce lipid accumulation, Swertia cincta exerts protective and therapeutic effects against cholestatic liver injury. Notably, gentian bitter glycosides appear to be the most critical components for this effect. ConclusionSwertia cincta may improve cholestatic liver injury by activating the peroxisome proliferator-activated receptor alpha pathway, and the key active compounds were gentiopicroside, loganic acid, and isoorientin.

An Integrated Strategy for Chemical Profile Establishment of Premna Microphylla Turcz. leaves and Metabolites in Vivo.

Premna microphylla Turcz. (PMT) is a traditional food and medicinal plant, which has been used to treat cure hemostasis, rheumatism and dysentery. However, it still lacks a clear understanding about chemical profile of PMT and metabolites in vivo. To establish a rapid and efficient analytical method for the identification of phytochemical in PMT and metabolites in vivo. Firstly, the fingerprint of PMT was established by high-performance liquid chromatography (HPLC) with methodology validation. Then, the phytochemical composition in PMT leaves were identified using ultra-performance liquid chromatography tandem quadruple time-of-flight mass spectrometry (UPLC-QTOF-MS/MS). Finally, the prototype and correlated metabolites were detected after oral administration in mice to understand the absorption and metabolism of phytochemical in vivo. The result showed established HPLC method for fingerprints evaluation of PMT has good precision, repeatability and stability. Additionally, a total of 103 phytochemicals were identified in PMT, mainly including flavonoids and terpenoids. Then, 37 prototype components and 20 derived metabolites in vivo were detected. In this study, we constructed a fingerprint method which has good stability, precision and repeatability, and the fingerprint of PMT was established. Then the chemical profile of PMT in vitro and in vivo was performed. The result showed that flavonoids and terpenoids were the main phytochemicals in PMT, and methylation, sulfonation, dihydroxylation were the main metabolic pathway in vivo. The present study provided the phytochemical basis for the subsequent study of pharmacological activity.

Recent Advances in Monitoring Microbial Toxins in Food Samples by HPLC-Based Techniques: A Review

This study examines the significant impact of bacterial, algal, and fungal toxins on foodborne illnesses, and stresses the importance of advanced detection techniques, such as high-performance liquid chromatography (HPLC)-based methodologies. It emphasizes the urgent need for further advancements in these techniques to ensure food safety, as they offer significant benefits, including low detection limits and the ability to be combined with other techniques to detect a wide range of toxins. In this regard, HPLC has emerged as a versatile and sensitive analytical technique for this purpose. Various HPLC methods, often enhanced with detectors such as ultraviolet (UV), fluorescence (FD), and mass spectrometry (MS), have been developed to identify and quantify microbial toxins in a wide variety of food samples. Recent advancements include HPLC-FD methods that utilize the natural fluorescence of certain aflatoxins, improving detection sensitivity. HPLC-MS/MS and UHPLC-MS/MS techniques offer high selectivity and sensitivity, making them suitable for detecting a wide range of toxins in trace quantities. The adaptability of HPLC, combined with innovative detection technologies and sample preparation methods, holds significant potential for enhancing food safety monitoring and reducing the global burden of foodborne diseases.

Development, Validation, and Greenness Assessment of Eco-Friendly Analytical Methods for the Determination of Abiraterone Acetate in Pure Form and Pharmaceutical Formulations

This study presents the development and validation of environmentally friendly analytical methods for quantifying Abiraterone Acetate (AA) in both its pure form and commercial pharmaceutical formulations. An optimized High-Performance Liquid Chromatography (HPLC) method was developed using an Agilent Extend C18 column (250 mm × 4.6 mm, 5 μm) at 25 °C. The mobile phase consisted of formic acid and ethanol in isocratic mode, with a flow rate of 1.0 mL min−1, and detection was performed at 253 nm. The spectrophotometric method involved a comprehensive evaluation of AA’s spectral properties in various solvents, with ultrapure water providing the most suitable spectra for analysis at 253 nm. Both methods were validated according to ICH guidelines, demonstrating selectivity, linearity, accuracy, precision, detection and quantification limits, and robustness, with correlation coefficients exceeding 0.999 across the 5–30 μg mL−1 concentration range. Comparative statistical analysis using Student’s t-test and Fisher’s F-test showed no significant differences between the two methods. The environmental impact of both methods was assessed using AGREE and GAPI software, confirming their sustainability. These validated methods offer reliable and eco-friendly approaches for the quantitative analysis of AA in tablet formulations, promoting safer and greener laboratory practices in pharmaceutical analysis.

Simple simultaneous analysis of various cardiovascular drug mixtures with vincamine: comparative eco-friendly assessment

The development of two eco-friendly analytical methods for the simultaneous determination of eight cardiovascular drugs; hydrochlorothiazide (HCT), captopril (CPL), lisinopril (LSP), valsartan (VAL), atorvastatin (ATR), bisoprolol (BSL), amlodipine (AML) and carvedilol (CVL); alongside with the nutraceutical vincamine (VIC) is essential for sustainable pharmaceutical analysis. This study explores the application of Micellar Electro Kinetic Chromatography (MEKC) and High-Performance Liquid Chromatography (HPLC) for this purpose. In MEKC method, the separation was done using fused silica capillary (41.5 cm × 50 µm id) and a back ground electrolyte consisting of 50 mM borate buffer (pH 9) containing 50 mM sodium lauryl sulphate (SLS) and 10% organic modifier (Acetonitrile). In HPLC method, separation was performed on a ZORBAX Extend-C18 (4.6 × 250 mm, 5 µm) column, using a gradient mobile phase consisting of 50 mM phosphate buffer pH 3 and methanol. Both methods attained good linearity (r ≥ 0.9996) with low values of LOD and LOQ. Both methods were successfully applied in the determination of co-administered single, binary and ternary dosage form of the studied drugs. Moreover, application of various combinations of co-administered dosage forms was achieved in rat plasma, confirming the applicability of these methods in different matrices. The use of micellar solutions in MEKC enhances separation efficiency while reducing the need for organic solvents, aligning with green chemistry principles. HPLC methods were optimized using environmentally benign solvents, ensuring reduced toxicity and waste production. The methodologies were evaluated through green, white, and blue metrics to ensure comprehensive sustainability, considering ecological impact, safety, and practical efficiency. These methods were not only cost-effective and time-saving but achieved high efficiency, sensitivity, and reproducibility making them ideal for routine use in pharmaceutical analysis.