What is the role of current mass spectrometry in pharmaceutical analysis?

The role of mass spectrometry (MS) has become more important in most application domains in recent years. Pharmaceutical analysis is specific due to its stringent regulation procedures, the need for good laboratory/manufacturing practices, and a large number of routine quality control analyses to be carried out. The role of MS is, therefore, very different throughout the whole drug development cycle. While it dominates within the drug discovery and development phase, in routine quality control, the role of MS is minor and indispensable only for selected applications. Moreover, its role is very different in the case of analysis of small molecule pharmaceuticals and biopharmaceuticals. Our review explains the role of current MS in the analysis of both small-molecule chemical drugs and biopharmaceuticals. Important features of MS-based technologies being implemented, method requirements, and related challenges are discussed. The differences in analytical procedures for small molecule pharmaceuticals and biopharmaceuticals are pointed out. While a single method or a small set of methods is usually sufficient for quality control in the case of small molecule pharmaceuticals and MS is often not indispensable, a large panel of methods including extensive use of MS must be used for quality control of biopharmaceuticals. Finally, expected development and future trends are outlined.

Enantioselective separation and determination of ibuprofen: Stereoselective pharmacokinetics, pharmacodynamics and analytical methods.

Ibuprofen (IBP), the 29th most prescribed drug in the United States in 2019, is a widely used nonsteroidal anti-inflammatory drug (NSAID) comprising two enantiomers, (R)-IBP and (S)-IBP, collectively known as (RS)-IBP. This critical review examines analytical techniques for the enantioselective separation and determination of IBP enantiomers, crucial for pharmaceutical and clinical applications. The review focuses on state-of-the-art methods, including chromatographic techniques including high-performance liquid chromatography, gas chromatography, liquid chromatography-tandem mass spectrometry, and some other techniques. This review addresses pharmacokinetics, pharmacology, and side effects of each enantiomer, ensuring safe drug usage. By consolidating diverse analytical methods and their applicability in different matrices, this review serves as a valuable resource for researchers, analysts, and practitioners in pharmaceutical analysis, pharmacology, and clinical studies.

Characterization of Prototype Gummy Formulations Provides Insight into Setting Quality Standards.

Gummy formulations are considered suitable alternatives to traditional oral dosage forms like tablets and capsules due to their merits that include chewability, softness/flexibility, improved drug release, administration without water, appealing organoleptic properties, better patient compliance, easy preparation and usefulness for persons of different ages (e.g. children). Though there is increasing interest in gummy formulations containing drugs, measurable parameters, and specification limits for evaluating their quality are scarce. Quality check forms an essential part of the pharmaceutical development process because drug products must be distributed as consistently stable, safe, and therapeutically effective entities. Consequently, some quality parameters that could contribute to the overall performance of typical gummy formulations were investigated employing six brands of non-medicinal gummies as specimens. Accordingly, key physicochemical and micromechanical characteristics namely adhesiveness (0.009 - 0.028 mJ), adhesive force (0.009 - 0.055 N), chewiness (2.780 - 6.753 N), cohesiveness (0.910 - 0.990), hardness (2.984 - 7.453 N), springiness (0.960 - 1.000), and resilience (0.388 - 0.572), matrix firmness - compression load (2.653 - 6.753 N) and work done (3.288 - 6.829 mJ), rupture (5.315 - 29.016 N), moisture content (< 5%), weight uniformity (< 2.5 g; < 7.5% deviation), and intraoral dissolution pH (≥ 3.5 ≤ 6.8) were quantified to identify measures that may potentially function as specification limits and serve as prospective reference points for evaluating the quality of gummy formulations. Findings from this work contribute to ongoing efforts to standardize the quality control strategies for gummy formulations, particularly those intended for oral drug delivery.

LC-MS/MS Investigation of nitrosamine impurities in certain Sartan group medicinal products available in Istanbul, Türkiye.

Nitrosamines (NAs) are molecules that include the nitroso functional group. In 2018, the US Food and Drug Administration (FDA) received its first report of NAs in pharmaceuticals. The fact that NA impurities are likely human carcinogens is relevant to these compounds. Furthermore, prolonged exposure to NA contaminants above safe limits may raise the risk of cancer. The goal of this article was to assess the amounts of six different NAs in Sartan group medicines purchased from formal pharmacies in Istanbul, Türkiye, using a validated LC-MS/MS assay. An LC-MS/MS-based analytical assay was undertaken. The separation was performed with a HR ODS 150mm×3.0mm and 5-analytical columns, providing effective separation of major peaks from NA impurities. In mobile phase A, formic acid was 0.10% in water, while in mobile phase B, formic acid was 0.10% in methanol. The flow rate was 0.4mL/minute, and the total runtime was 18minutes with the gradient elution mode. The validation was conducted in line with ISO/IEC 17025 requirements. Up to 100µg/L, linearity was determined using correlation coefficients (r2>0.995) for all NAs. The limit of quantification values for all NAs analyses were below 1.0µg/L. The mean recovery value obtained during the spike experiment was 95.18%, demonstrating the accuracy of the procedure. In addition, the accuracy was shown by a certified reference analysis, which yielded relative standard deviation and relative error values of 1.82% and 3.34%, respectively. During the intermediate precision testing, bias and relative standard deviation were 0.96 and 2.87%, respectively. Of the 75 study samples involving Sartan group medical products, no nitrosamine impurities were detected, demonstrating that pharmaceutical companies have adequate medication safety precautions in place in accordance with FDA and European Medicines Agency (EMA) regulations published to prevent NA contaminants in human medicinal products.

Smart and sensitive nanomaterial-based electrochemical sensor for the determination of a poly (ADP-ribose) polymerase (PARP) inhibitor anticancer agent.

In this research, we propose a novel approach for constructing a sensitive and selective electrochemical sensor utilizing high-quality multi-walled carbon nanotubes functionalized with amino groups (MWCNT-NH2) for the detection of Talazoparib (TLZ), a poly (ADP-ribose) polymerase (PARP) enzyme inhibitor, in real samples. The MWCNT-NH2-based sensor exhibited remarkable performance characteristics, including excellent repeatability, reproducibility, and high selectivity against various interferences. Under optimized conditions, the sensor demonstrated a wide linear concentration range of 1.0-5.0 µM, with a low limit of detection (LOD) of 0.201 µM. Substantiated by rigorous analysis of pharmaceutical and biological matrices, our methodology emerges as a paragon of reliability, boasting recovery rates within the satisfactory bracket of 96.38-105.25%. The successful application of the MWCNT-NH2-based sensor in practical sample analysis highlights its potential for implementation in clinical and pharmaceutical settings. This research not only advances the application of MWCNT-NH2 in electrochemical sensing but also opens new avenues for the development and monitoring of innovative anticancer treatments. The insights gained from our study have far-reaching implications, pointing toward a future where precision and innovation converge to improve patient care and treatment outcomes.

Magnetic molecularly imprinted polymer based on dynamically established metal-mediated binding sites for the determination of trace captopril in rat plasma.

Therapeutic drug monitoring of captopril, which is a commonly used antihypertensive agent in clinical practice, is necessary. However, matrix effect-induced pretreatment is the bottleneck for determination. Metal-mediated molecularly imprinted polymers, an essential branch of molecularly imprinted polymers with better specificity and selectivity, have been used to separate/enrich analytes from complex matrices. In this work, Cu2+ was introduced to dynamically establish the binding sites of metal-mediated molecularly imprinted polymer towards captopril. All evidence demonstrated that the metal-mediated molecularly imprinted polymer based on Cu2+ coordination obtained a higher adsorption capacity (81.23 mg/g), faster adsorption rate (adsorption equilibrium within 50 min), and better selectivity (with the unrecognized analog). Subsequently, the Cu2+ -mediated molecularly imprinted polymer was used as dispersive molecularly imprinted solid-phase extraction to successfully establish an analytical platform for the determination of trace captopril in rat plasma. The enrichment factor was up to 20, the detection limit was as low as 0.16 µg/ml, and the average recovery was in the range of 87.51%-98.28% with a relative standard deviation of less than 3.29%. This study provides a promising reference for the preparation of selective adsorbents to improve pretreatment.

Advanced porous organic materials for sample preparation in pharmaceutical analysis.

The development of novel sample preparation media plays a crucial role in pharmaceutical analysis. To facilitate the extraction and enrichment of pharmaceutical molecules in complex samples, various functionalized materials have been developed and prepared as adsorbents. Recently, some functionalized porous organic materials have become adsorbents for pharmaceutical analysis due to their unique properties of adsorption and recognition. These advanced porous organic materials, combined with consequent analytical techniques, have been successfully used for pharmaceutical analysis in complex samples such as environmental and biological samples. This review encapsulates the progress of advanced porous materials for pharmaceutical analysis including pesticides, antibiotics, chiral drugs, and other compounds in the past decade. In addition, we also address the limitations and future trends of these porous organic materials in pharmaceutical analysis.

Environmentally friendly protocol for the determination of sitagliptin phosphate in pharmaceutical preparations and biological fluids using l-tyrosine as a fluorescence probe.

A responsive spectrofluorometric method was developed for the determination of sitagliptin phosphate using l-tyrosine as a fluorescence probe. The fluorescence intensity of l-tyrosine was quenched with sitagliptin phosphate. The fluorescence intensity was recorded at 307 nm using a 272 nm excitation wavelength. The calibration plot between fluorescence intensity and the concentration of drug was linear in the range of 0.1 to 2.0 mM with a good correlation value of 0.997. The limit of detection and quantification were established to be 3.7 × 10-4 and 1.23 × 10-3  mM, respectively. Commonly used excipients did not interfere with sitagliptin phosphate measurement. The proposed method was used to measure the sitagliptin phosphate in its standard type, dosage form, and biological samples. The percent recovery ranged from 97.41-103.36%. The static quenching was shown to be responsible for quenching as indicated by the Stern-Volmer plot. The method was validated using ICH guidelines and profitably applied for the content uniformity test, resulting in a high percent recovery and small relative standard deviation. The proposed approach is effortless, susceptible, selective, economic, and provides a high precision and accuracy, and can be used to determine sitagliptin phosphate in the pharmaceutical industry.

Electrochemical sensor based on 3D-printed substrate by masked stereolithography (MSLA): a new, cheap, robust and sustainable approach for simple production of analytical platforms.

The development of miniaturized, sustainable and eco-friendly analytical sensors with low production cost is a current trend worldwide. Within this idea, this work presents  the innovative use of masked stereolithography (MSLA) 3D-printed substrates for the easy fabrication of pencil-drawn electrochemical sensors (MSLA-3D-PDE). The use of a non-toxic material such as pencil (electrodes) together with a biodegradable 3D printing resin (substrate) allowed the production of devices that are quite cheap (ca. US$ 0.11 per sensor) and with low environmental impact. Compared to paper, which is the most used substrate for manufacturing pencil-drawn electrodes, the MSLA-3D-printed substrate has the advantages of not absorbing water (hydrophobicity) or becoming crinkled and weakened when in contact with solutions. These features provide more reproducible, reliable, stable, and long-lasting sensors. The MSLA-3D-PDE, in conjunction with the custom cell developed, showed excellent robustness and electrochemical performance similar to that observed of the glassy carbon electrode, without the need of any activation procedure. The analytical applicability of this platform was explored through the quantification of omeprazole in pharmaceuticals. A limit of detection (LOD) of 0.72 µmol L-1 was achieved, with a linear range of 10 to 200 µmol L-1. Analysis of real samples provided results that were highly concordant with those obtained by UV-Vis spectrophotometry (relative error ≤ 1.50%). In addition, the greenness of this approach was evaluated and confirmed by a quantitative methodology (Eco-Scale index). Thus, the MSLA-3D-PDE appears as a new and sustainable tool with great potential of use in analytical electrochemistry.

Advances in Ultra-High-Resolution Mass Spectrometry for Pharmaceutical Analysis.

Pharmaceutical analysis refers to an area of analytical chemistry that deals with active compounds either by themselves (drug substance) or when formulated with excipients (drug product). In a less simplistic way, it can be defined as a complex science involving various disciplines, e.g., drug development, pharmacokinetics, drug metabolism, tissue distribution studies, and environmental contamination analyses. As such, the pharmaceutical analysis covers drug development to its impact on health and the environment. Moreover, due to the need for safe and effective medications, the pharmaceutical industry is one of the most heavily regulated sectors of the global economy. For this reason, powerful analytical instrumentation and efficient methods are required. In the last decades, mass spectrometry has been increasingly used in pharmaceutical analysis both for research aims and routine quality controls. Among different instrumental setups, ultra-high-resolution mass spectrometry with Fourier transform instruments, i.e., Fourier transform ion cyclotron resonance (FTICR) and Orbitrap, gives access to valuable molecular information for pharmaceutical analysis. In fact, thanks to their high resolving power, mass accuracy, and dynamic range, reliable molecular formula assignments or trace analysis in complex mixtures can be obtained. This review summarizes the principles of the two main types of Fourier transform mass spectrometers, and it highlights applications, developments, and future perspectives in pharmaceutical analysis.

Development of Green and High Throughput Microplate Reader-Assisted Universal Microwell Spectrophotometric Assay for Direct Determination of Tyrosine Kinase Inhibitors in Their Pharmaceutical Formulations Irrespective the Diversity of Their Chemical Structures.

This study discusses the development and validation of a universal microwell spectrophotometric assay for TKIs, regardless of the diversity in their chemical structures. The assay depends on directly measuring the native ultraviolet light (UV) absorption of TKIs. The assay was carried out using UV-transparent 96-microwell plates and the absorbance signals were measured by a microplate reader at 230 nm, at which all TKIs had light absorption. Beer's law correlating the absorbances of TKIs with their corresponding concentrations was obeyed in the range of 2-160 µg mL-1 with excellent correlation coefficients (0.9991-0.9997). The limits of detection and limits quantitation were in the ranges of 0.56-5.21 and 1.69-15.78 µg mL-1, respectively. The proposed assay showed high precision as the values of the relative standard deviations for the intra- and inter-assay precisions did not exceed 2.03 and 2.14%, respectively. The accuracy of the assay was proven as the recovery values were in the range of 97.8-102.9% (±0.8-2.4%). The proposed assay was successfully applied to the quantitation of all TKIs in their pharmaceutical formulations (tablets) with reliable results in terms of high accuracy and precision. The assay greenness was evaluated, and the results proved that the assay fulfils the requirements of green analytical approach. The proposed assay is the first assay that can analyse all TKIs on a single assay system without chemical derivatization or modifications in the detection wavelength. In addition, the simple and simultaneous handling of a large number of samples as a batch using micro-volumes of samples gave the assay the advantage of high throughput analysis, which is a serious demand in the pharmaceutical industry.

Quantification of quetiapine fumarate based on electrochemical analysis by reduced graphene oxide modified nano-silica functionalized with polydopamine and gold nanostars: A novel pharmaceutical analysis strategy.

Quetiapine fumarate (QF) is an antipsychotic drug that has been most widely prescribed as an antipsychotic. In this regard, sensitive recognition of QF in bodily fluids must be done accurately. In this work, an electrochemical sensor for QF detection was fabricated, using GNSs-PDA@SiO2 modified rGO stabilized on glassy carbon electrode. According to the electrical nature of gold nanoparticles (GNPs), polydopamine (PDA), and its composition with nano-silica, the proposed hybrid material is able to enhance the electro-oxidation signals of QF toward its sensitive detection in complex biological media. The morphology of synthesized polymeric nanocomposites and various surfaces of electrodes were investigated using Field Emission Scanning Electron Microscopy and Energy-Dispersive X-Ray Spectroscopy methods. Using the square wave voltammetry technique, the fabricated electrochemical sensor could detect QF in the linear range of 500 µM to 3 mM, which low limit of quantification was obtained as 500 µM, indicating the sensor's appropriate sensitivity. For the first time, the application of novel hybrid material (GNSs-PDA@SiO2 ) for pharmaceutical analysis in human plasma was studied using electrochemical sensor technology. Based on the obtained analytical results, engineered nano-surface led to entrapment and oxidation of QF in real samples. So, a novel and efficient method for the analysis of QF was designed and validated, which opens a new horizon for pharmaceutical analysis and therapeutic drug monitoring.

Enantiomeric separation of bupropion by liquid chromatography on derivatized cyclofructan chiral stationary phase.

High-performance liquid chromatography (HPLC) is an ideal tool for enantiomeric separations of different drugs. In this study, the direct enantioseparation of bupropion, an atypical antidepressant structurally related to cathinone, was explored by using five chiral columns, including three based on derivatized cyclofructans, macrocyclic glycopeptide teicoplanin, and an immobilized amylose derivative under multimodal elution conditions. Baseline enantioseparation was obtained on the LarihcShell CF6-RN column, with derivatized cyclofructan 6, in the polar organic mode. The effects of the mobile-phase composition, type and content of major components, the nature and the amount of mobile-phase additives, and the column temperature on the retention, selectivity, and resolution were investigated to optimize enantioseparation. The calibration curve was linear in the range of 10-125 µg/ml for each enantiomer. The limits of detection and quantification were 0.1 and 0.3 µg/ml for both enantiomers of bupropion. The chiral recognition was controlled especially by H bonds, π-π, dipole-dipole interactions, and steric effects. Finally, the developed method was applied to the determination of bupropion in the commercially available drug.

Orthophthaldehyde as a fluorescent probe for the feasible and sensitive assay of heptaminol: application to dosage forms and real human plasma.

The antihypotensive drug heptaminol was determined using a spectrofluorimetric method and ortho-phthaladehyde as a fluorescence probe. The drug was mixed with the reagent in the presence of 2-mercaptoethanol and the reaction was carried out in slightly alkaline aqueous solution containing 0.1 M sodium hydroxide. The resulting product exhibited high fluorescence activity that was measured at 451 nm after excitation at 334 nm. The linearity range of the method was 5-100 ng ml-1 with a lower detection limit of 1.8 ng ml-1 . The procedure was evaluated according to the International Council of Harmonization guidelines. The proposed method was applied to analyze the drug in pharmaceutical tablets and oral drops. In addition, the present study represents the first spectrofluorimetric method for the determination of the cited drug in real human plasma. The method provided high recovery percentages without any interference from coexisting pharmaceutical excipients or the components of human plasma.

Resonance Rayleigh scattering approach based on association complex formation with erythrosine B for determination of venlafaxine, application to the dosage form and spiked human plasma.

The interaction of venlafaxine hydrochloride (VLX) with erythrosine B was investigated using a resonance Rayleigh scattering (RRS) spectroscopic technique. In acetate buffer (pH 3.4), erythrosine B reacted with VLX to form a 1:1 ion-pair complex with concomitant enhancement in RRS intensity that was measured at 330 nm. In addition, the stability constant and the change in free energy of the reaction were estimated. Based on this interaction a new method was developed for a sensitive VLX analysis using erythrosine B as a probe. The results indicated that this method had good selectivity in the presence of coexisting compounds. The scattering intensity (ΔIRRS ) was linearly dependent on VLX concentration over the range 0.04-1.0 µg ml-1 with a determination coefficient (r) of 0.9998. The limit of detection and limit of quantitation were 0.01 and 0.03 µg ml-1 , respectively. This method could be suitably used for analysis of VLX in pharmaceutical capsules and human plasma.

Facile spectrofluorimetric quantitation of octreotide, a synthetic peptide, in its pure form and pharmaceutical formulation; evaluation of the method's greenness.

A new, rapid, highly sensitive, and affordable spectrofluorimetric approach has been constructed and validated for the determination of octreotide in its authentic form and pharmaceutical dosage form. Octreotide is an important synthetic analog of the naturally occurring somatostatin hormone. The developed spectrofluorimetric approach is actually dependent on the measurement of octreotide native fluorescence at emission wavelength of 342 nm after excitation at 218 nm. At optimal reaction conditions, the calibration curve has been constructed over the concentration range 200-2000 ng ml-1 , with excellent linearity. The limits of detection and quantitation values were found to be 55 and 169 ng ml-1 , respectively. The developed approach has been effectively used to determine octreotide in its pharmaceutical ampoules, without interference from the excipients in the dosage form. The developed approach is simple, time-saving, and does not require multiple pretreatment steps for samples, costly apparatus, or dangerous materials. As a result, it can be used to detect and quantify octreotide acetate in quality control laboratories.

3D-printed electrochemical pestle and mortar for identification of falsified pharmaceutical tablets.

Falsified medicines and healthcare supplements provide a major risk to public health and thus early identification is critical. Although a host of analytical approaches have been used to date, they are limited, as they require extensive sample preparation, are semi-quantitative and/or are inaccessible to low- and middle-income countries. Therefore, for the first time, we report a simple total analysis system which can rapidly and accurately detect falsified medicines and healthcare supplements. We fabricated a poly-lactic acid (PLA) pestle and mortar and using a commercial 3D printer, then made carbon black/PLA (CB/PLA) electrodes in the base of the mortar using a 3D printing pen to make an electrochemical cell. The pestle and mortar were able to crush and grind the tablets into a fine powder to the same consistency as a standard laboratory pestle and mortar. Using melatonin tablets to characterise the device, the 3D-printed pestle and mortar was able to detect the concentration of melatonin in the presence of insoluble excipients. The calibration plot showed a linear response from 37.5 to 300 µg/mL, where the limit of detection was 7 µg/mL. Electrochemical treatment was able to regenerate the CB/PLA working electrode allowing for repeated use of the device. In a blinded study, the device was able to accurately determine falsified melatonin tablets with recovery percentages between 101% and 105%. This was comparable to HPLC measurements. Overall, these findings highlight that our 3D-printed electrochemical pestle and mortar is an accessible and effective total analysis system that can have the ability to identify falsified medicines and healthcare supplements in remote locations.

Voltammetric Sensor Based on SeO2 Nanoparticles and Surfactants for Indigo Carmine Determination.

Indigo carmine is a widely used colorant in the food and pharmaceutical industry a high concentration of which can lead to a wide range of negative effects on human health. Therefore, colorant contents have to be strictly controlled. SeO2-nanoparticle-modified glassy carbon electrodes (GCE) have been developed as a voltammetric sensor for indigo carmine. Various types and concentrations of surfactants have been used as reagents for the stabilization of SeO2 nanoparticle dispersions and as electrode surface co-modifiers. An amount of 1.0 mM cationic cetylpyridinium bromide (CPB) provides the best response of the indigo carmine on the modified electrode. The electrodes were characterized by cyclic voltammetry, chronoamperometry, and electrochemical impedance spectroscopy (EIS). SeO2 nanoparticle-CPB-modified electrodes show 4.2-fold higher electroactive area vs. GCE as well as a dramatic 5043-fold decrease in the electron transfer resistance indicating effectivity of the modifier developed. The surface-controlled electrooxidation of indigo carmine proceeds irreversibly (αa = 0.46) with the participation of two electrons and two protons. A linear dynamic range of 0.025-1.0 and 1.0-10 µM of indigo carmine were obtained with the detection and quantification limits of 4.3 and 14.3 nM, respectively. The practical applicability of the sensor was successfully shown on the pharmaceutical dosage forms.

Multifunctional Eco-Friendly Synthesis of ZnO Nanoparticles in Biomedical Applications.

This work describes an environmental-friendly preparation of ZnO nanoparticles using aqueous oat extract. The advanced electrochemical and optical features of green synthesized ZnONPs displayed excellent antibacterial activity and exhibited an important role in pharmaceutical determinations. The formation of nanoscale ZnO was confirmed using various spectroscopic and microscopic investigations. The formed nanoparticles were found to be around 100 nm. The as-prepared ZnONPs were monitored for their antibacterial potential against different bacterial strains. The inhibition zones for ZnONPs were found as Escherichia coli (16 mm), Pseudomonas aeruginosa (17 mm), Staphylococcus aureus (12 mm) and Bacillus subtilis (11 mm) using a 30-µg mL-1 sample concentration. In addition, ZnONPs exhibited significant antioxidant effects, from 58 to 67%, with an average IC50 value of 0.88 ± 0.03 scavenging activity and from 53 to 71% (IC50 value of 0.73 ± 0.05) versus the scavenging free radicals DPPH and ABTS, respectively. The photocatalytic potential of ZnONPs for Rhodamine B dye degradation under UV irradiation was calculated. The photodegradation process was carried out as a function of time-dependent and complete degradation (nearly 98%), with color removal after 120 min. Conclusively, the synthesized ZnONPs using oat biomass might provide a great promise in the future for biomedical applications.

Employing molecularly imprinted polymers in the development of electroanalytical methodologies for antibiotic determination.

Antibiotics, although being amazing compounds, need to be monitored in the environment and foodstuff. This is primarily to prevent the development of antibiotic resistance that may make them ineffective. Unsurprisingly, advances in analyticalsciences that can improve their determination are appreciated. Electrochemical techniques are known for their simplicity, sensitivity, portability and low-cost; however, they are often not selective enough without recurring to a discriminating element like an antibody. Molecular imprinting technology aims to create artificial tissues mimicking antibodies named molecularly imprinted polymers (MIPs), these retain the advantages of selectivity but without the typical disadvantages of biological material, like limited shelf-life and high cost. This manuscript aims to review all analytical methodologies for antibiotics, using MIPs, where the detection technique is electrochemical, like differential pulse voltammetry (DPV), square-wave voltammetry (SWV) or electrochemical impedance spectroscopy (EIS). MIPs developed by electropolymerization (e-MIPs) were applied in about 60 publications and patents found in the bibliographic search, while MIPs developed by other polymerization techniques, like temperature assisted ("bulk") or photopolymerization, were limited to around 40. Published works covered the electroanalysis of a wide range of different antibiotics (ß-lactams, tetracyclines, quinolones, macrolides, aminoglycosides, among other), in a wide range of matrices (food, environmental and biological).