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Applications of Chromatography in Drug Analysis and Development

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A special issue of Processes (ISSN 2227-9717). This special issue belongs to the section "Pharmaceutical Processes".

Deadline for manuscript submissions: closed (15 March 2023) | Viewed by 33501

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Dr. Malgorzata Starek

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Department of Inorganic and Analytical Chemistry, Faculty of Pharmacy, Jagiellonian University Medical College, 9 Medyczna St., 30-688 Kraków, Poland
Interests: chromatographic techniques; methods validation; drug analysis; stability testing; interactions; drug impurities; remediation

Prof. Dr. Monika Dąbrowska

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Special Issue Information

Dear Colleagues,

One of the most common methodologies for pharmaceutical and biomedical analysis is chromatography, both liquid (HPLC, TLC) and gas (GC). HPLC, in particular, has become the most important analytical method used to identify and quantify medicinal substances, both in their active pharmaceutical ingredient and in formulations during the process of their discovery, development, production, quality control, stability, and bioavailability studies. Drug development begins with the discovery of a molecule with therapeutic value, while metabolism and pharmacokinetics are the next stages during which compounds such as drug candidates are tested, most often using combined techniques such as LC-MS or LC-MS/MS, due to their high sensitivity and selectivity.

This Special Issue focuses on different procedures, e.g., method development, validation, compounds separation, physicochemical properties, quality attributes, and provides information for their optimization, environmental and health relations, and sustainability. The new applications of chromatographic operations can be applied in drug development and delivery. Furthermore, applying chromatographic methods and optimization at both the theoretical and practical levels are within the scope of this issue. Original research papers and review articles covering a wide range of all chromatographic procedures are welcome.

Topics include, but are not limited to applications in the following areas:

Design and simulation of a novel or revamped separation processes
Optimization of the chromatographic conditions
Monitoring safety and operational issues in the pharmaceutical industry
Separation of non-enantiomeric compounds and chiral separation mechanisms
Qualitative and quantitative studies of biologically active compounds
Drug impurities analysis
Drug discovery and development
Examination of the physicochemical properties of chemical compounds, such as lipophilicity

Dr. Malgorzata Starek
Dr. Monika Dąbrowska
Guest Editors

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Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Processes is an international peer-reviewed open access monthly journal published by MDPI.

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Keywords

lipophilicity
stability and kinetics
purity testing
drug analysis
stereoisomers analysis
analysis of biological materials
identification of metabolisms products
analysis of phototransformation products

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Published Papers (9 papers)

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Research

13 pages, 927 KiB

Open AccessArticle

Optimizations of the Conditions for Ceftobiprole Determination in a Complex Matrix

by Żaneta Binert-Kusztal, Joanna Żandarek, Małgorzata Starek and Monika Dąbrowska

Processes 2022, 10(11), 2196; https://doi.org/10.3390/pr10112196 - 26 Oct 2022

Cited by 2 | Viewed by 1629

Abstract

A quick and accurate chromatographic–densitometric method for the determination of ceftobiprole in biological material (whole blood and urine) was developed. Preparation of the test sample required extraction of the drug from the matrix and was carried out by testing methanol or acetone as extracting agents, which were successfully used to isolate ceftobiprole from biological material. Under optimization of the procedure, various stationary and mobile phases were tested. Lastly, HPTLC cellulose plates and a mixture containing ethanol, 2-propanol, glacial acetic acid, and water in the ratio 4:4:1:3 (v/v/v/v) were chosen. Densitometric detection was made at a maximum absorbance of 316 nm. The developed method was validated; a linear function of the ceftobiprole concentration was obtained in the range of 2.4–72 µg/mL (r > 0.99) for both methanol and acetone solutions. The average accuracy of the devised method was measured at nearly 100%; nevertheless, the limit of the quantification was at 8.92 for methanol and 9.14 µg/mL for acetone solution. Therefore, the above method can be successfully used to ceftobiprole in biological material. Full article

(This article belongs to the Special Issue Applications of Chromatography in Drug Analysis and Development)

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11 pages, 1094 KiB

Open AccessArticle

Cytochrome P450 3A2 and PGP-MDR1-Mediated Pharmacokinetic Interaction of Sinapic Acid with Ibrutinib in Rats: Potential Food/Herb–Drug Interaction

by Muzaffar Iqbal, Mohammad Raish, Ajaz Ahmad, Essam A. Ali, Yousef A. Bin Jardan, Mushtaq A. Ansari, Mudassar Shahid, Abdul Ahad, Khalid M. Alkharfy and Fahad I. Al-Jenoobi

Processes 2022, 10(6), 1066; https://doi.org/10.3390/pr10061066 - 26 May 2022

Cited by 3 | Viewed by 2932

Abstract

Ibrutinib (IBR) metabolism (primarily by CYP3A enzyme) is the main route of excretion for IBR, which could lead to drug–drug/herb–drug interactions with herbal medicines, nutritional supplements, and other foods. Sinapic acid (SA) is a bioactive phytonutrient that is used as a dietary supplement to treat a variety of illnesses. Pharmacokinetic interactions may occur when IBR interacts with SA, which influences the pharmacokinetic processes such as absorption, distribution, metabolism, and excretion. Therefore, it is obligatory to investigate the safety apprehensions of such parallel usage and to evaluate the possible impact of SA on the pharmacokinetics of IBR and propose a possible interaction mechanism in an animal model. The IBR concentration in plasma samples was determined using a validated UHPLC-MS/MS method after administration of a single oral dosage of IBR (50 mg/kg) in rats with or without SA pretreatment (40 mg/kg p.o. each day for 7 days, n = 6). The co-administration of IBR with SA displayed significant increases in C_max ~18.77%, AUC_0–T ~28.07%, MRT ~16.87%, and K_el ~24.76%, and a significant decrease in the volume of distribution Vz/F_obs ~37.66%, the rate of clearance (Cl/F) ~21.81%, and T_½ ~20.43%, respectively, were observed as compared to rats that were administered IBR alone, which may result in increased bioavailability of IBR. The metabolism of IBR in the liver and intestines is significantly inhibited when SA is given, which may lead to an increase in the absorption rate of IBR. These findings need to be investigated further before they can be used in clinical practice. Full article

(This article belongs to the Special Issue Applications of Chromatography in Drug Analysis and Development)

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32 pages, 6091 KiB

Open AccessArticle

An Experimental and Modeling Combined Approach in Preparative Hydrophobic Interaction Chromatography

by Elena Lietta, Alessandro Pieri, Antonio G. Cardillo, Marco Vanni, Roberto Pisano and Antonello A. Barresi

Processes 2022, 10(5), 1027; https://doi.org/10.3390/pr10051027 - 20 May 2022

Cited by 5 | Viewed by 3061

Abstract

Chromatography is a technique widely used in the purification of biopharmaceuticals, and generally consists of several chromatographic steps. In this work, Hydrophobic Interaction Chromatography (HIC) is investigated as a polishing step for the purification of therapeutic proteins. Adsorption mechanisms in hydrophobic interaction chromatography are still not completely clear and a limited amount of published data is available. In addition to new data on adsorption isotherms for some proteins (obtained both by high-throughput and frontal analysis method), and a comparison of different models proposed in the literature, two different approaches are compared in this work to investigate HIC. The predictive approach exploits an in-house code that simulates the behavior of the component in the column using the model parameters found from the fitting of experimental data. The estimation approach, on the other hand, exploits commercial software in which the model parameters are found by the fitting of a few experimental chromatograms. The two approaches are validated on some bind-elute runs: the predictive approach is very informative, but the experimental effort needed is high; the estimation approach is more effective, but the knowledge gained is lower. The second approach is also applied to an in-development industrial purification process and successfully resulted in predicting the behavior of the system, allowing for optimization with a reduction in the time and amount of sample needed. Full article

(This article belongs to the Special Issue Applications of Chromatography in Drug Analysis and Development)

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15 pages, 4521 KiB

Open AccessFeature PaperArticle

Solubility of Luteolin and Other Polyphenolic Compounds in Water, Nonpolar, Polar Aprotic and Protic Solvents by Applying FTIR/HPLC

by Saša Rajhard, Lucija Hladnik, Filipa A. Vicente, Stanko Srčič, Miha Grilc and Blaž Likozar

Processes 2021, 9(11), 1952; https://doi.org/10.3390/pr9111952 - 30 Oct 2021

Cited by 24 | Viewed by 6252

Abstract

In recent years, flavonoids have become a highly researched topic due to their health beneficial effects. Since flavonoids’ solubility plays a significant role in their use in pharmaceutical, food, biological, and chemical areas, the determination of suitable solvents is crucial. Fourier transform infrared (FTIR) analysis was used to characterize functional groups of several flavonoids and phenolic compounds, namely luteolin, hesperidin, quercetin, naringenin, gallic acid and tannic acid. Concentration dependence on transmittance was evaluated for these compounds in ethanol. Afterwards, luteolin was chosen as a model flavonoid, with its concentration correlated with transmittance using 15 solvents with different polarities. Luteolin solubility was further corroborated with high-performance liquid chromatography (HPLC). These results shed light on using FTIR as a semi-quantitative method for the initial screening of solvents and the solubility of different compounds while saving time and solvents. Hence, HPLC would only be needed as a final step for the most promising solvents. Full article

(This article belongs to the Special Issue Applications of Chromatography in Drug Analysis and Development)

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12 pages, 983 KiB

Open AccessArticle

Highly Sensitive and Ecologically Sustainable Reversed-Phase HPTLC Method for the Determination of Hydroquinone in Commercial Whitening Creams

by Mohammed H. Alqarni, Prawez Alam, Faiyaz Shakeel, Ahmed I. Foudah and Sultan Alshehri

Processes 2021, 9(9), 1631; https://doi.org/10.3390/pr9091631 - 9 Sep 2021

Cited by 7 | Viewed by 2560

Abstract

Hydroquinone (HDQ) is a natural depigmenting agent, which is commonly used in skin-toning preparations. The safety and greenness of analytical methods of HDQ quantification were not considered in previous literature. Therefore, a highly sensitive and ecologically greener reversed-phase high-performance thin-layer chromatography (RP-HPTLC)-based assay was established for HDQ estimation in four different commercial whitening creams (CWCs). The binary ethanol–water (60:40, v·v⁻¹) mixture was utilized as the green solvent system. The estimation of HDQ was carried out at 291 nm. The present RP-HPTLC-based assay was linear in the 20–2400 ng band⁻¹ range. The present analytical method was highly sensitive based on the detection and quantification data. The other validation parameters, such as accuracy, precision, and robustness, were also suitable for the determination of HDQ. Maximum HDQ quantities were obtained in CWC A (1.23% w·w⁻¹) followed by CWC C (0.81% w·w⁻¹), CWC D (0.43% w·w⁻¹), and CWC B (0.37% w·w⁻¹). The analytical GREEnness (AGREE) score for the present analytical method was estimated as 0.91, indicating the excellent greener characteristics of the present RP-HPTLC assay. These results suggest that the present analytical method is highly sensitive and ecologically sustainable for the quantitation of HDQ in its commercial formulations. Full article

(This article belongs to the Special Issue Applications of Chromatography in Drug Analysis and Development)

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18 pages, 2769 KiB

Open AccessFeature PaperEditor’s ChoiceArticle

Development of TLC Chromatographic-Densitometric Procedure for Qualitative and Quantitative Analysis of Ceftobiprole

by Żaneta Binert-Kusztal, Małgorzata Starek, Joanna Żandarek and Monika Dąbrowska

Processes 2021, 9(4), 708; https://doi.org/10.3390/pr9040708 - 16 Apr 2021

Cited by 3 | Viewed by 2581

Abstract

Currently, there is still a need for broad-spectrum antibiotics. The new cephalosporin antibiotics include, among others, ceftobiprole, a fifth-generation gram-positive cephalosporin, active against Staphylococcus aureus methicillin agonist (MRSA). The main focus of the work was to optimize the conditions of ceftobiprole qualitative determination and to validate the developed procedure according to ICH guidelines. As a result of the optimization process, HPTLC Cellulose chromatographic plates as a stationary phase and a mixture consisting of ethanol:2-propanol: glacial acetic acid: water (4:4:1:3, v/v/v/v) as a mobile phase were chosen. The densitometric detection was carried out at maximum absorbance of ceftobiprole (λ = 232 nm). Next, the validation process of the developed procedure was carried out. The relative standard deviation (RSD) for precision was less than 1.65%, which proves the high compatibility of the results, as well as the LOD = 0.0257 µg/spot and LOQ = 0.0779 µg/spot values, which also confirm the high sensitivity of the procedure. The usefulness of the developed method for the stability studies of ceftobiprole was analyzed. Study was carried out under stress conditions, i.e., acid and alkaline environments, exposure to radiation imitating sunlight and high temperature (40–60 °C). It was found that cefotbiprole is unstable in an alkaline environment and during exposure to UV-VIS radiation. Moreover, the lipophilicity parameter, as a main physicochemical property of the biologically active compound, was determined using experimental and computational methods. Full article

(This article belongs to the Special Issue Applications of Chromatography in Drug Analysis and Development)

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12 pages, 1571 KiB

Open AccessFeature PaperArticle

Application of the HPLC Method in Parenteral Nutrition Assessment: Stability Studies of Ondansetron

by Szymon Tomczak, Vera Radwan, Anna Jelińska and Maciej Stawny

Processes 2021, 9(3), 453; https://doi.org/10.3390/pr9030453 - 3 Mar 2021

Cited by 3 | Viewed by 3207

Abstract

Ondansetron (OND) is a serotonin type 3 receptor antagonist that exhibits antiemetic activity. From the clinical point of view, vomiting and nausea prevention is an important task. Anticancer treatment and recovery impact the patient’s overall state by affecting appetite, well-being, and physical activity, and consequently, nutrition quality. Depending on the patient’s indication and condition, parenteral nutrition is administered to meet full nutritional requirements. In addition, antiemetic drugs can be added to the parenteral nutrition (PN) admixture to treat chemo- or radio-therapy-induced nausea and vomiting. However, adding any medication to the PN admixture can result in the instability of the composition in the overall admixture. This study aimed to develop the HPLC method of determination of OND in Lipoflex special, one of the most popular, ready-to-use PN admixtures. The proposed HPLC method and the sample preparation procedure were suitable for analyzing OND in PN admixture stored under various conditions, such as exposure to sunlight and temperature. It was found that the decomposition of OND during the seven-day storage did not exceed 5% and did not depend on external factors. Based on the conducted research, it is recommended to add OND to Lipoflex special, and it is possible to store such an admixture for seven days. Full article

(This article belongs to the Special Issue Applications of Chromatography in Drug Analysis and Development)

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13 pages, 7573 KiB

Open AccessArticle

Chromatographic and Computational Screening of Lipophilicity and Pharmacokinetics of Newly Synthesized Betulin-1,4-quinone Hybrids

by Monika Kadela-Tomanek, Maria Jastrzębska, Elwira Chrobak, Ewa Bębenek and Stanisław Boryczka

Processes 2021, 9(2), 376; https://doi.org/10.3390/pr9020376 - 19 Feb 2021

Cited by 15 | Viewed by 3017

Abstract

Lipophilicity is one of the most important parameters determining the pharmacodynamic and pharmacokinetic properties, as well as the toxicity of many compounds. The subject of the research was to determine the lipophilicity of betulin-1,4-quinone hybrids using thin layer chromatography in reverse phase system and computer programs to calculate its theoretical models. The correlation between the experimental and theoretical values of lipophilicity was analyzed. Lipinski’s and Veber’s rules, as well as penetration through the blood–brain barrier were also determined using computer programs. For all of the analyzed values, a similarity analysis was performed. The dendrograms for the experimental and theoretical lipophilicity show that there is a correlation between them. However, the dendrograms for the experimental lipophilicity and pharmacokinetic parameters indicate that there is no correlation between the structure and the pharmacological properties. Hybrids exhibit a high biological activity against cancer cell lines, with a high level of NAD[P]H-quinone oxidoreductase (NQO1) protein. The enzymatic assay used has shown that these compounds are good NQO1 substrates, as evidenced by the increasing metabolic rates relative to that of streptonigrin. The similarity analysis has also shown that there is no correlation between lipophilicity and biological activity for the tested compounds. Full article

(This article belongs to the Special Issue Applications of Chromatography in Drug Analysis and Development)

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8 pages, 1323 KiB

Open AccessCommunication

Affinity of Fluoroquinolone–Safirinium Dye Hybrids to Phospholipids Estimated by IAM-HPLC

by Krzesimir Ciura, Joanna Fedorowicz, Hanna Kapica, Alicja Adamkowska, Wiesław Sawicki and Jarosław Sączewski

Processes 2020, 8(9), 1148; https://doi.org/10.3390/pr8091148 - 14 Sep 2020

Cited by 7 | Viewed by 2882

Abstract

Nowadays, fluoroquinolones (FQs) constitute one of the most important classes of antibiotics. FQs are used to treat infections caused by Gram-positive and Gram-negative species. A set of fluoroquinolone–Safirinium dye hybrids has been synthesized in our laboratory as potential new dual-action antibacterial agents. In the present study we have evaluated how such a modification influences the affinity of FQs to phospholipids. The immobilized artificial membrane (IAM) high-performance liquid chromatography (IAM-HPLC) was used as a tool for the determination of phospholipids partitioning. The obtained results indicate that the fluoroquinolone–Safirinium dye hybrids, especially the SafiriniumP conjugates, display significantly lower affinity to phospholipids than the parent FQs. Despite the fact that the hybrid structures comprise a quaternary nitrogen atom and hence are permanently charged, the attractive electrostatic interactions between the solutes and negatively charged phospholipids do not occur or occur at a lesser extent than in the case of the unmodified FQs. Since affinity of FQs to phospholipids involves molecular mechanism, which is not entirely determined by lipophilicity, assessment of phospholipid partitioning should be considered at the early stage of the development of new FQ antibiotics. Full article

(This article belongs to the Special Issue Applications of Chromatography in Drug Analysis and Development)

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