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Sensitivity Enhancement Approaches to the Separation Techniques for Pharmaceutical Analysis and Therapeutic Drug Monitoring

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A special issue of Separations (ISSN 2297-8739). This special issue belongs to the section "Analysis of Natural Products and Pharmaceuticals".

Deadline for manuscript submissions: closed (30 September 2023) | Viewed by 7911

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Prof. Dr. Samy Emara

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Faculty of Pharmacy, Misr International University, Cairo, Egypt
Interests: automation in liquid chromatography; capillary electrophoresis; mass spectrometry; flow injection analysis; therapeutic drug monitoring; quality control of pharmaceuticals; green chemistry

Prof. Dr. Randa Abdel-Salam

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Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Suez Canal University, Ismailia 41522, Egypt
Interests: HPLC; LC-MS; environmental analytical chemistry; green chemistry technology; chromatographic method development; sample preparation; quality control for analysis of drugs in dosage forms and/or in biological fluids
Special Issues, Collections and Topics in MDPI journals

Prof. Dr. Ibrahim Darwish

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Department of Pharmaceutical Chemistry, College of Pharmacy, King Saud University, Riyadh, Saudi Arabia
Interests: HPLC; LC-MS; capillary electrophoresis; immune analytical methods and Immunosensors; quality control for analysis of drugs in dosage forms or/and in biological fluids

Special Issue Information

Dear Colleagues,

Several separation techniques are available for pharmaceutical and biomedical analysis, but when these techniques are utilized alone, where it is essential to quantify the analytes at the lowest possible concentrations, the success rates are not very encouraging. This could imply that even robust routine separation techniques that provide reliable specificity and validity at the usual working concentrations can fail at low concentration levels of pharmaceuticals. This poses significant problems for investigating product purity and drug monitoring in bio-fluid samples. Sensitivity enhancement approaches are consequently required to maximize the performance of separation procedures. This issue focuses on potential strategies for enhancing sensitivity as they can be applied to current separation techniques for pharmaceutical analysis and therapeutic drug monitoring.

Prof. Dr. Samy Emara
Prof. Dr. Randa Abdel-Salam
Prof. Dr. Ibrahim Darwish
Guest Editors

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Keywords

pharmaceutical analysis
biomedical analysis
therapeutic drug monitoring
separation techniques
sensitivity enhancement

Published Papers (4 papers)

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Research

17 pages, 3238 KiB

Open AccessArticle

Optimization of Chromatographic Conditions with QbD for Method Development and Validation of Bosutinib by HPLC: Applications in Dosage Forms and Rat Plasma Analysis

by Asim Najmi, Zia ur Rehman, Hassan Ahmed Alhazmi, Mohammed Mofarreh Albratty, Nasser Hassan Majrashi, Khalid Mohammed Hakami, Naif Ali Najmi and Ammar Abdullah Mobarki

Separations 2023, 10(6), 346; https://doi.org/10.3390/separations10060346 - 07 Jun 2023

Cited by 2 | Viewed by 2111

Abstract

Aim: Bosutinib (BST) is an anti-cancer medicine that is used to treat a variety of different types of cancer. Using the HPLC method of analysis and the Quality by Design (QbD) strategy, the study aimed to precisely quantify the drug in tablet form and in rat plasma. Methodology: For the developed method’s validation, the chromatographic settings were fine-tuned by making use of the Box–Behnken Design (BBD). In the BBD, two dependent variables and three independent variables were selected. Isocratically, samples were eluted, having eluent phase composition of ammonium acetate (CH₃COONH₄) buffer pH 3.0 and acetonitrile (CH₃CN) (60:40% v/v), in Raptor C-18 column at temperature 25

^{\circ}

C with a flow rate of 1 mL/min for 5 min. The wavelength of detection was set at 260 nm. In this study, encorafenib (ENC) was employed as an internal standard. Result: A sharp and resolved peak of BST and ENC at a retention time of 1.92 min and 4.01 min, respectively, was observed by the developed method. The limits of quantification and detection of the newly established method were found to be 1.503

μ

g/mL⁻¹ and 0.496

μ

g/mL⁻¹. The calibration curve’s observed linearity range was between 2 and 20

μ

g/mL⁻¹, with an r² of 0.999. The developed and optimized method was verified in compliance with the ICH guidelines. The results of all validation parameters were within the acceptable range, for example, % RSD of system suitability (0.63–4.46), % RSD of linear regression (1.659), interday and intraday precision % RSD value (1.723–1.892), and (1.762–1.923), respectively, and accuracy (1.476–1.982). Conclusion: The quantity of BST in tablet dosage form and in rat plasma samples was determined using a simple, quick, and robust method that was devised and validated. Full article

(This article belongs to the Special Issue Sensitivity Enhancement Approaches to the Separation Techniques for Pharmaceutical Analysis and Therapeutic Drug Monitoring)

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15 pages, 3289 KiB

Open AccessArticle

Experimental Design Approach for Development of HPLC Method for Simultaneous Analysis of Triamcinolone, Nystatin, and Gramicidin in Industrial Wastewater

by Loubna Elsharkawy, Maha A. Hegazy, Ahmed E. Elgendy and Rasha M. Ahmed

Separations 2023, 10(6), 342; https://doi.org/10.3390/separations10060342 - 01 Jun 2023

Cited by 1 | Viewed by 1560

Abstract

This study used an experimental design approach to optimize an HPLC method for the simultaneous determination of three pharmaceutical residues (triamcinolone, nystatin, and gramicidin) in industrial wastewater samples. The goal of using an experimental design approach was to maximize the method performance through separation enhancement and shortening the time of analysis and/or minimizing the environmental effects through the reduction in wastes and sample treatment. To achieve this goal, two steps were performed: a full factorial screening design for the three chromatographic variables, and optimization design using central composite design to select the optimum conditions that accomplished the highest resolution between adjacent peaks within a minimum run time of less than 5 min. The optimal chromatographic conditions derived from Minitab software using the desirability function were applied. Separation was carried out on a Zorbax C18 column (250 mm × 4.6, 5 μm) with gradient elution of a mobile phase composed of methanol and 0.25 M potassium dihydrogen phosphate buffer (pH 3.6) at different UV detections. For the validation of the developed HPLC method, ICH guidelines were followed, and the obtained results were found to be in compliance with the acceptance criteria. Linearity was over the concentration range of 1.00–25.00 μg/mL for triamcinilone and nystatin and 10.00–50.00 µg/mL for gramicidin. The proposed method was successfully applied to quantify the three studied pharmaceutical compounds in rinsing wastewater samples. Full article

(This article belongs to the Special Issue Sensitivity Enhancement Approaches to the Separation Techniques for Pharmaceutical Analysis and Therapeutic Drug Monitoring)

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14 pages, 1999 KiB

Open AccessArticle

Application of Quality by Design Approach in the Optimization and Development of the UPLC Analytical Method for Determination of Fusidic Acid in Pharmaceutical Products

by Mohamed Ibrahim, Nasser Ali Alhabib, Doaa Alshora, Mounir M. Salem Bekhit, Ehab Taha, Wael A. Mahdi and Abdulelah M. Harthi

Separations 2023, 10(5), 318; https://doi.org/10.3390/separations10050318 - 19 May 2023

Cited by 3 | Viewed by 1188

Abstract

Background: Analytical techniques are a crucial method used in quality control procedures. Fusidic acid (FU), an antibacterial drug, is available on the market in a semisolid dosage form. This work aimed to develop a simple, sensitive, and robust UPLC assay for FU. Method: The effect of the formic acid concentration (X1 (1%, 0.55%, and 0.1%)), and column temperature (X2 (40, 32.5, and 25 °C)) on the retention time, peak area, and peak height were determined. Results: The results show that a long retention time of 1.18 min can be achieved with a low column temperature and a low to medium concentration of formic acid. A good peak height resolution was obtained with a low concentration of formic acid at different temperature settings. The optimized condition was suggested by the software program to analyze the drug in a mobile phase, consisting of 72% acetonitrile and 28% water containing 0.1% formic acid with a column temperature adjusted to 40 °C. Conclusion: The method was validated in terms of linearity, accuracy, precision, and robustness. In addition, the stability degradation study determined that the method can separate the drug from other degradation production. The method was applicable to determine the drug content in the marketed product. Full article

(This article belongs to the Special Issue Sensitivity Enhancement Approaches to the Separation Techniques for Pharmaceutical Analysis and Therapeutic Drug Monitoring)

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14 pages, 1785 KiB

Open AccessArticle

Highly Sensitive In-Capillary Derivatization and Field Amplified Sample Stacking to Analyze Narcotic Drugs in Human Serum by Capillary Zone Electrophoresis

by Monika Malak, Hager Ebrahim, Heba Sonbol, Ahmed Ali, Yasmine Aboulella, Ghada Hadad and Samy Emara

Separations 2023, 10(1), 58; https://doi.org/10.3390/separations10010058 - 15 Jan 2023

Cited by 5 | Viewed by 1846

Abstract

An in-capillary derivatization (in-CAP-D) integrated with field amplified sample stacking (FASS) has been developed for the determination of morphine (MOR) and its metabolite, morphine-6-glucuronide (MOR-6-G) in human serum using capillary zone electrophoresis (CZE) and fluorescence detection (in-Cap-D-FASS-CZE). Acetonitrile was employed in removing proteins and extracting MOR and MOR-6-G into the clear supernatant containing codeine (COD) as an internal standard (IS). The derivatization was achieved in an in-capillary mode by introducing the acetonitrile-treated samples into a running electrolyte containing an oxidizing agent of potassium ferricyanide, whereas MOR, MOR-6-G and COD were oxidized into dimer derivatives with highly fluorescent intensity. The effectiveness and sensitivity of the in-Cap-D-FASS-CZE method were affected by many parameters, and the following conditions were found to be optimal: 70 m Mdisodium tetraboratedecahydrate (pH, 10.5), 0.30 mM ferrricyanide and a separation voltage of 10 kV. In order to perform the FASS, samples were electrokinetically injected for 20 s at 20 kV into the capillary that was pre-field with a 4 s water plug. Analysis was performed at ambient temperature (22 ± 1 °C). The method’s validation revealed good linearity with respect to peak area ratios of MOR and MOR-6-G with the IS and the corresponding concentrations over the ranges of 1–2000 and 1.2 to 2000 ng/mL, respectively. Following one oral dose of controlled-release MOR sulphate tablet, the validated in-Cap-D-FASS-CZE method successfully enabled the determination of MOR and MOR-6-G in clinical serum samples. Full article

(This article belongs to the Special Issue Sensitivity Enhancement Approaches to the Separation Techniques for Pharmaceutical Analysis and Therapeutic Drug Monitoring)

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