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Bioanalysis and Biological Matrix Sampling

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A special issue of Molecules (ISSN 1420-3049). This special issue belongs to the section "Analytical Chemistry".

Deadline for manuscript submissions: closed (31 January 2021) | Viewed by 46135

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Special Issue Editors

Dr. Roberto Mandrioli

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Department for Life Quality Studies, Alma Mater Studiorum—Università di Bologna, 47921 Rimini, Italy
Interests: drug analysis; toxicological analysis; HPLC; capillary electrophoresis; method development; microsampling; sample preparation; antioxidants; biological matrices
Special Issues, Collections and Topics in MDPI journals

Dr. Laura Mercolini

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Guest Editor

Research group of Pharmaco-Toxicological Analysis (PTA Lab), Department of Pharmacy and Biotechnology (FaBiT), Alma Mater Studiorum - University of Bologna, Via Belmeloro 6, 40126 Bologna, Italy
Interests: bioanalysis; liquid chromatography; mass spectrometry; method validation; microsampling; sample treatment; central nervous system drugs; drugs of abuse; doping agents; natural products
Special Issues, Collections and Topics in MDPI journals

Dr. Michele Protti

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Guest Editor

Research group of Pharmaco-Toxicological Analysis (PTA Lab), Department of Pharmacy and Biotechnology (FaBiT), Alma Mater Studiorum-University of Bologna, Via Belmeloro 6, 40126 Bologna, Italy
Interests: HPLC; UHPLC; MS; HRMS; automation; biological matrix; miniaturized sample collection and pretreatment; CNS drugs; metabolites; biomarkers
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Bioanalysis is one of the most stimulating and complicated fields of analytical, medicinal, and biomedical chemistry. The high complexity of matrices coming from living beings is hardly matched, and most analytes, be they endogenous or exogenous, are found in these heterogeneous matrices at extremely low levels. The intrinsic instability and ease of degradation of biomatrices only adds to the difficulty of the endeavour.

As a consequence, bioanalysis requires cutting-edge levels of sensitivity, selectivity, reproducibility, and overall reliability together with top-level throughput. To tackle these challenges effectively, a huge array of sampling, sample preparation, and analysis combinations and workflows have been devised, tested, and applied.

The results have been nothing less than amazing. Material and instrumental advances, coupled to automation, miniaturisation, and to the ingenuity and expertise of thousands of researchers, have made this field one of the most advanced, attractive, and vibrant of all analytical chemistry.

In this Special Issue, we invite researchers to contribute innovative, original research articles and reviews papers related to the state of the art of all facets of biomatrix sampling, pretreatment, and analysis. Forensic, toxicological, anti-doping, and drug analyses are among the most important, but definitely not the only, aspects of the Special Issue. Proposals including all kinds of instrumental setups, endogenous and exogenous analytes, and biological matrices are welcome.

Potential topics include, but are not limited to the following:

Anti-doping analysis
Clinical analysis
Drug analysis
Forensic analysis
High-throughput or high-capacity analysis
Innovation in sampling
Sampling and microsampling
Toxicological analysis
Workflow and sample prep automation

Prof. Roberto Mandrioli
Prof. Dr. Laura Mercolini
Dr. Michele Protti
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. Molecules is an international peer-reviewed open access semimonthly journal published by MDPI.

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Keywords

anti-doping
automation
bioanalysis
biological matrix
drug analysis
forensic analysis
sample preparation
sampling and microsampling
toxicological analysis

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Published Papers (14 papers)

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20 pages, 4564 KiB

Open AccessArticle

Promising Antidiabetic and Antimicrobial Agents Based on Fused Pyrimidine Derivatives: Molecular Modeling and Biological Evaluation with Histopathological Effect

by Fatma Bassyouni, Mohammad Tarek, Abeer Salama, Bassant Ibrahim, Sawsan Salah El Dine, Nemat Yassin, Amina Hassanein, Maysa Moharam and Mohamed Abdel-Rehim

Molecules 2021, 26(8), 2370; https://doi.org/10.3390/molecules26082370 - 19 Apr 2021

Cited by 33 | Viewed by 3326

Abstract

Diabetes is the most common metabolic disorder in both developing and non-developing countries, and a well-recognized global health problem. The WHO anticipates an increase in cases from 171 million in 2000 to 366 million by 2030. In the present study, we focus on the preparation of pyrimidine derivatives as potential antidiabetic and antimicrobial agents. Thein vivoeffect on total serum glucose concentration, cholesterol and antioxidant activity was assessed in adult male albino Wister rats and compared to the reference drug glimperide. Promising results were observed for compound 5. The histopathological study confirms that compound 5 results in significant activity with liver maintenance. The antimicrobial activities were evaluated against several bacterial strains such as Salmonella typhimurium ATCC 25566, Bacillus cereus, Escherichia coli NRRN 3008, Pseudomonas aeruginosa ATCC 10145, Staphylococcus aureus ATCC 6538and fungi such as Rhizopus oligosporus, Mucor miehei and Asperillus niger. Compounds 4 and 5 showed a good inhibition of the bacterial zone compared to the reference drug cephradine. Finally, we suggest protein targets for these drugs based on computational analysis, and infer their activities from their predicted modes of binding using molecular modeling. The molecular modeling for compounds 4 and 5 resulted in improved docking scores and hydrogen bonding. The docking studies are in good agreement with the in vitro and in vivo studies. Full article

(This article belongs to the Special Issue Bioanalysis and Biological Matrix Sampling)

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18 pages, 2320 KiB

Open AccessArticle

A Rapid Nano-Liquid Chromatographic Method for the Analysis of Cannabinoids in Cannabis sativa L. Extracts

by Lucie Žampachová, Zeineb Aturki, Francesca Mariani and Petr Bednář

Molecules 2021, 26(7), 1825; https://doi.org/10.3390/molecules26071825 - 24 Mar 2021

Cited by 15 | Viewed by 3400

Abstract

Cannabis sativa L. is an herbaceous plant belonging to the family of Cannabaceae. It is classified into three different chemotypes based on the different cannabinoids profile. In particular, fiber-type cannabis (hemp) is rich in cannabidiol (CBD) content. In the present work, a rapid nano liquid chromatographic method (nano-LC) was proposed for the determination of the main cannabinoids in Cannabis sativa L. (hemp) inflorescences belonging to different varieties. The nano-LC experiments were carried out in a 100 µm internal diameter capillary column packed with a C18 stationary phase for 15 cm with a mobile phase composed of ACN/H₂O/formic acid, 80/19/1% (v/v/v). The reverse-phase nano-LC method allowed the complete separation of four standard cannabinoids in less than 12 min under isocratic elution mode. The nano-LC method coupled to ultraviolet (UV) detection was validated and applied to the quantification of the target analytes in cannabis extracts. The nano-LC system was also coupled to an electrospray ionization–mass spectrometry (ESI-MS) detector to confirm the identity of the cannabinoids present in hemp samples. For the extraction of the cannabinoids, three different approaches, including dynamic maceration (DM), ultrasound-assisted extraction (UAE), and an extraction procedure adapted from the French Pharmacopeia’s protocol on medicinal plants, were carried out, and the results achieved were compared. Full article

(This article belongs to the Special Issue Bioanalysis and Biological Matrix Sampling)

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17 pages, 546 KiB

Open AccessArticle

Assessing Adherence to Antihypertensive Medication by Means of Dose-Dependent Reference Plasma Concentration Ranges and Ultra-High Performance Liquid Chromatography-Ion Trap Mass Spectrometry Analysis

by Lea Wagmann, Aline C. Vollmer, Lucas Lauder, Felix Mahfoud and Markus R. Meyer

Molecules 2021, 26(5), 1495; https://doi.org/10.3390/molecules26051495 - 9 Mar 2021

Cited by 7 | Viewed by 2909

Abstract

Poor adherence to antihypertensive drug therapy is a well-recognized problem and can be assessed by mass spectrometry-based analyses of body fluids. However, contrary statements exist whether drug quantification in blood or qualitative screening in urine is more suitable. The present pilot study aimed to further elucidate the power of blood plasma drug concentrations for adherence monitoring by developing and validating a quantification procedure for nine antihypertensive drugs (amlodipine, bisoprolol, candesartan, canrenone, carvedilol, metoprolol, olmesartan, torasemide, and valsartan) in blood plasma using liquid–liquid extraction and an ultra-high-performance liquid chromatography-ion trap mass spectrometry analysis. The procedure should then be used for an adherence assessment and compared with the results of an established qualitative urine screening. Selectivity, carryover, matrix effect, accuracy, precision, dilution integrity, and stability were successfully validated, except for amlodipine. The applicability was demonstrated by analyzing 19 plasma samples containing 28 antihypertensive drugs and comparing the measured concentrations with calculated dose-dependent reference plasma concentration ranges. The interpretation of plasma concentrations was found to be more sophisticated and time-consuming than that of urine screening results, and adherence could not be assessed in two cases (10%) due to measured plasma concentrations below the lower limit of quantification. However, 14 out of 19 subjects were classified as adherent (75%) and three as nonadherent (15%), in contrast to 19 (100%) that were claimed to be adherent based on the results of the qualitative urine screening. Nevertheless, further data is needed to estimate whether plasma quantification is superior in terms of assessing adherence to antihypertensive medication. Full article

(This article belongs to the Special Issue Bioanalysis and Biological Matrix Sampling)

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12 pages, 1699 KiB

Open AccessArticle

Rp-HPLC Determination of Quercetin in a Novel D-α-Tocopherol Polyethylene Glycol 1000 Succinate Based SNEDDS Formulation: Pharmacokinetics in Rat Plasma

by Osama A. A. Ahmed, Hany M. El-Bassossy, Heba M. El-Sayed and Soad S. Abd El-Hay

Molecules 2021, 26(5), 1435; https://doi.org/10.3390/molecules26051435 - 6 Mar 2021

Cited by 16 | Viewed by 4131

Abstract

Despite its proven efficacy in diverse metabolic disorders, quercetin (QU) for clinical use is still limited because of its low bioavailability. D-α-Tocopherol polyethylene glycol 1000 succinate (TPGS) is approved as a safe pharmaceutical adjuvant with marked antioxidant and anti-inflammatory activities. In the current study, several QU-loaded self-nanoemulsifying drug delivery systems (SNEDDS) were investigated to improve QU bioavailability. A reversed phase high performance liquid chromatography (RP-HPLC) method was developed, for the first time, as a simple and sensitive technique for pharmacokinetic studies of QU in the presence of TPGS SNEDDS formula in rat plasma. The analyses were performed on a Xterra C₁₈ column (4.6 × 100 mm, 5 µm) and UV detection at 280 nm. The analytes were separated by a gradient system of methanol and phosphate buffer of pH 3. The developed RP-HPLC method showed low limit of detection (LODs) of 7.65 and 22.09 ng/mL and LOQs of 23.19 and 66.96 ng/mL for QU and TPGS, respectively, which allowed their determination in real rat plasma samples. The method was linear over a wide range, (30–10,000) and (100–10,000) ng/mL for QU and TPGS, respectively. The selected SNEDDS formula, containing 50% w/w TPGS, 30% polyethylene glycol 200 (PEG 200), and 20% w/w pumpkin seed oil (PSO), showed a globule size of 320 nm and −28.6 mV zeta potential. Results of the pharmacokinetic studies showed 149.8% improvement in bioavailability of QU in SNEDDS relative to its suspension. The developed HPLC method proved to be simple and sensitive for QU and TPGS simultaneous determination in rat plasma after oral administration of the new SNEDDS formula. Full article

(This article belongs to the Special Issue Bioanalysis and Biological Matrix Sampling)

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15 pages, 24973 KiB

Open AccessArticle

Sensitive, High-Throughput Liquid Chromatography-Tandem Mass Spectrometry Analysis of Atorvastatin and Its Pharmacologically Active Metabolites in Serum for Supporting Precision Pharmacotherapy

by Gellért Balázs Karvaly, István Vincze, István Karádi, Barna Vásárhelyi and András Zsáry

Molecules 2021, 26(5), 1324; https://doi.org/10.3390/molecules26051324 - 2 Mar 2021

Cited by 4 | Viewed by 2161

Abstract

The antihyerlipidemic drug atorvastatin (ATR) is used worldwide as part of the strategy to prevent cardiovascular events. The high prevalence of patient nonadherence remains an important challenge which could be addressed efficiently by precision pharmacotherapy based on therapeutic drug monitoring (TDM). ATR is metabolized to pharmacologically active metabolites, and evidence shows that the sums of ATR acid and lactone form concentrations (ATR + ATRL), or of ATR and hydroxylated metabolites (ATR + MET) should be assayed. A method is presented for the analysis of these substances in serum. Method validation included the estimation of the quantitative relationship between the concentrations and the standard deviations (SD), which supports the optimal incorporation of TDM results into nonparametric pharmacokinetic models. The concentrations of the analytes were evaluated in human subjects receiving ATR. The method’s performance improved by taking the sums of acid and lactone concentrations into account. The concentration–SD relationship was linear, and we recommend applying Theil’s regression for estimating the assay error. All analytes could be detected by 2 h post dose in the samples of human subjects. The changes in metabolite/parent drug concentration ratios in time depended on the dose. The method is suitable for the TDM of ATR with a focus on precision pharmacotherapy. Full article

(This article belongs to the Special Issue Bioanalysis and Biological Matrix Sampling)

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19 pages, 2704 KiB

Open AccessArticle

Rapid MALDI-MS Assays for Drug Quantification in Biological Matrices: Lessons Learned, New Developments, and Future Perspectives

by Margaux Fresnais, Esra Yildirim, Seda Karabulut, Dirk Jäger, Inka Zörnig, Julia Benzel, Kristian W. Pajtler, Stefan M. Pfister, Jürgen Burhenne, Walter E. Haefeli and Rémi Longuespée

Molecules 2021, 26(5), 1281; https://doi.org/10.3390/molecules26051281 - 26 Feb 2021

Cited by 10 | Viewed by 3460

Abstract

Matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) has rarely been used in the field of therapeutic drug monitoring, partly because of the complexity of the ionization processes between the compounds to be quantified and the many MALDI matrices available. The development of a viable MALDI-MS method that meets regulatory guidelines for bioanalytical method validation requires prior knowledge of the suitability of (i) the MALDI matrix with the analyte class and properties for ionization, (ii) the crystallization properties of the MALDI matrix with automation features, and (iii) the MS instrumentation used to achieve sensitive and specific measurements in order to determine low pharmacological drug concentrations in biological matrices. In the present hybrid article/white paper, we review the developments required for the establishment of MALDI-MS assays for the quantification of drugs in tissues and plasma, illustrated with concrete results for the different steps. We summarize the necessary parameters that need to be controlled for the successful development of fully validated MALDI-MS methods according to regulatory authorities, as well as currently unsolved problems and promising ways to address them. Finally, we propose an expert opinion on future perspectives and needs in order to establish MALDI-MS as a universal method for therapeutic drug monitoring. Full article

(This article belongs to the Special Issue Bioanalysis and Biological Matrix Sampling)

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11 pages, 1126 KiB

Open AccessArticle

Simultaneous Quantification of 3′- and 6′-Sialyllactose in Rat Plasma Using Liquid Chromatography-Tandem Mass Spectrometry and Its Application to a Pharmacokinetic Study

by Seok-In Jang, Han Young Eom, Jeong Ho Hwang, Lila Kim and Jong-Hwa Lee

Molecules 2021, 26(4), 1177; https://doi.org/10.3390/molecules26041177 - 22 Feb 2021

Cited by 4 | Viewed by 2419

Abstract

Sialyllactose (SL), an acidic oligosaccharide, has immune-protective effects against pathogens and helps with the development of the immune system and intestinal microorganisms. To elucidate the pharmacokinetic characterization after oral administration to rats, the simultaneous quantification method for 3′-SL and 6′-SL in rat plasma was validated, using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in an electrospray ionization (ESI) mode. Several types of columns [C18, amide, and hydrophilic interaction liquid chromatography (HILIC) phase] were used to separate the peaks of 3′-SL and 6′-SL, which improved chromatographic selectivity. Ultimately, the HILIC phase column had a good peak shape and quick resolution, with a mobile phase comprising ammonium acetate buffer and acetonitrile obtained by gradient elution. In addition, the simultaneous quantification of 3′-SL and 6′-SL in rat plasma samples were adequately applied to pharmacokinetic study. Full article

(This article belongs to the Special Issue Bioanalysis and Biological Matrix Sampling)

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6 pages, 224 KiB

Open AccessCommunication

Optimized Extraction of Amikacin from Murine Whole Blood

by Roccaldo Sardella, Styliani Xiroudaki, Laura Mercolini, Samuele Sabbatini, Claudia Monari, Stefano Perito, Federica Ianni, Anna Vecchiarelli and Stefano Giovagnoli

Molecules 2021, 26(3), 665; https://doi.org/10.3390/molecules26030665 - 27 Jan 2021

Viewed by 1890

Abstract

Amikacin (Amk) analysis and quantitation, for pharmacokinetics studies and other types of investigations, is conventionally performed after extraction from plasma. No report exists so far regarding drug extraction from whole blood (WB). This can represent an issue since quantification in plasma does not account for drug partitioning to the blood cell compartment, significantly underrating the drug fraction reaching the blood circulation. In the present work, the optimization of an extraction method of Amk from murine WB has been described. The extraction yield was measured by RP-HPLC-UV after derivatization with 1-fluoro-2,4-dinitrobenzene, which produced an appreciably stable derivative with a favorable UV/vis absorption. Several extraction conditions were tested: spiked Amk disulfate solution/acetonitrile/WB ratio; presence of organic acids and/or ammonium hydroxide and/or ammonium acetate in the extraction mixture; re-dissolution of the supernatant in water after a drying process under vacuum; treatment of the supernatant with a solution of inorganic salts. The use of 5% (by volume) of ammonium hydroxide in a hydro-organic solution with acetonitrile, allowed the almost quantitative (95%) extraction of the drug from WB. Full article

(This article belongs to the Special Issue Bioanalysis and Biological Matrix Sampling)

16 pages, 6635 KiB

Open AccessArticle

Simultaneous Determination of Cortisol, Cortisone, and Multiple Illicit Drugs in Hair among Female Drug Addicts with LC-MS/MS

by Cailing Duan, Yan Wu, Jin Yang, Shenghuo Chen, Yun Pu and Huihua Deng

Molecules 2021, 26(2), 516; https://doi.org/10.3390/molecules26020516 - 19 Jan 2021

Cited by 7 | Viewed by 3596

Abstract

Long-term dependence of illicit drugs impairs the function of the hypothalamic-pituitary-adrenal (HPA) axis, which regulates the secretion of endogenous steroids, cortisol, and cortisone. Thus, the present study aimed to develop a sensitive method for simultaneous determination of the multiple illicit drugs and two steroids in hair to monitor the status of illicit drug exposure and the physiological and psychological health of drug addicts. The target analytes were extracted from hair by incubation with 1 mL methanol for 24 h at 40 °C and then determined with LC-APCI⁺-MS/MS. The validated method showed acceptable linearity (R² > 0.99) in the range of 1.25–250 pg/mg for cortisol and cortisone, 2.5–125 pg/mg for heroin, 2.5–1250 pg/mg for ketamine, 2.5–5000 pg/mg for methamphetamine (MAM), 2.5–250 pg/mg for 3, 4-methylenedioxymethamphetamine (MDMA), morphine, and 6-monoacetylmorphine (6-AM). Limits of quantification were 1.6, 1.2, 1.6, 1.0, 1.4, 0.3, 2.1, and 1.2 pg/mg for cortisol, cortisone, heroin, ketamine, MAM, MDMA, morphine, and 6-AM, respectively. Method recoveries were from 90–115% for all analytes. Inter-day and intra-day coefficients of variation were within 10%. Finally, this method was successfully applied to detect the aforementioned analytes in hair among female drug addicts who self-reported to be MAM abuser, heroin abuser, ketamine abuser, and abuser of mixture drugs of MAM and heroin. MAM abusers with current MAM use showed significantly higher concentrations of cortisol, MAM, and MDMA than controls with drug withdrawal. Full article

(This article belongs to the Special Issue Bioanalysis and Biological Matrix Sampling)

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16 pages, 1018 KiB

Open AccessArticle

LC-MS/MS Quantification of Nevirapine and Its Metabolites in Hair for Assessing Long-Term Adherence

by Haoran Yang, Liuxi Chu, Yan Wu, Wei Wang, Jin Yang, Quan Zhang, Shan Qiao, Xiaoming Li, Zhiyong Shen, Yuejiao Zhou, Shuaifeng Liu and Huihua Deng

Molecules 2020, 25(23), 5692; https://doi.org/10.3390/molecules25235692 - 2 Dec 2020

Cited by 5 | Viewed by 2590

Abstract

The adherence assessment based on the combination of nevirapine (NVP) and its two metabolites (2-hydroxynevirapine and 3-hydroxynevirapine) would more comprehensively and accurately reflect long-term adherence than that of a single prototype. This study aimed to develop a specific, sensitive and selective method for simultaneous detection of the three compounds in hair and explore whether there was consistency among the three compounds in assessing long-term adherence. Furthermore, 75 HIV-positive patients who were taking the NVP drug were randomly recruited and divided into two groups (high-and low-adherence group). All participants self-reported their days of oral drug administration per month and provided their hair strands closest to the scalp at the region of posterior vertex. The concentrations of three compounds in the hair were determined using a developed LC-MS/MS method in multiple reaction monitoring. This method showed good performances in limit of quantification and accuracy with the recoveries from 85 to 115% and in precision with the intra-day and inter-day coefficients of variation within 15% for the three compounds. The population analysis revealed that patients with high-adherence showed significantly higher concentrations than those with low-adherence for all three compounds. There were significantly moderate correlations of nevirapine with 2-hydroxynevirapine and 3-hydroxynevirapin and high correlation between 2-hydroxynevirapine and 3-hydroxynevirapin. The two NVP’s metabolites showed high consistency with NVP in evaluating long-term adherence. Full article

(This article belongs to the Special Issue Bioanalysis and Biological Matrix Sampling)

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15 pages, 2592 KiB

Open AccessArticle

Ultrasound–Vortex-Assisted Dispersive Liquid–Liquid Microextraction Combined with High Performance Liquid Chromatography–Diode Array Detection for Determining UV Filters in Cosmetics and the Human Stratum Corneum

by Fang-Yi Liao, Yu-Lin Su, Jing-Ru Weng, Ying-Chi Lin and Chia-Hsien Feng

Molecules 2020, 25(20), 4642; https://doi.org/10.3390/molecules25204642 - 12 Oct 2020

Cited by 9 | Viewed by 3529

Abstract

This study explores the amounts of common chemical ultraviolet (UV) filters (i.e., avobenzone, bemotrizinol, ethylhexyl triazone, octocrylene, and octyl methoxycinnamate) in cosmetics and the human stratum corneum. An ultrasound–vortex-assisted dispersive liquid–liquid microextraction (US–VA–DLLME) method with a high-performance liquid chromatography–diode array detector was used to analyze UV filters. A bio-derived solvent (i.e., anisole) was used as the extractant in the US–VA–DLLME procedure, along with methanol as the dispersant, a vortexing time of 4 min, and ultrasonication for 3 min. The mass-transfer rate of the extraction process was enhanced due to vortex-ultrasound combination. Various C18 end-capped columns were used to investigate the separation characteristics of the UV filters, with XBridge BEH or CORTECS selected as the separation column. Calibration curves were constructed in the 0.05–5 μg/mL (all filters except octocrylene) and 0.1–10 μg/mL (octocrylene) ranges, and excellent analytical linearities with coefficients of determination (r²) above 0.998. The developed method was successfully used to analyze sunscreen. Moreover, experiments were designed to simulate the sunscreen-usage habits of consumers, and the cup method was used to extract UV filters from the human stratum corneum. The results suggest that a makeup remover should be employed to remove water-in-oil sunscreens from skin. Full article

(This article belongs to the Special Issue Bioanalysis and Biological Matrix Sampling)

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11 pages, 2510 KiB

Open AccessArticle

Enhanced Extraction Technique of Omarigliptin from Human Plasma—Applied to Biological Samples from Healthy Human Volunteers

by Shereen Mowaka, Nermeen Ashoush, Mariam Tadros, Noha El Zahar and Bassam Ayoub

Molecules 2020, 25(18), 4232; https://doi.org/10.3390/molecules25184232 - 15 Sep 2020

Cited by 3 | Viewed by 2267

Abstract

Enhancing drug extraction from human plasma is a challenging approach that critically affects pharmacokinetic and any further clinical studies based on the drug C_min and C_max values. It also has a serious impact on the sensitivity and the lower limit of quantification (LLOQ) value of the bio-analytical methods. An advanced liquid chromatography tandem mass spectrometry (LC-MS/MS) bio-analytical method of omarigliptin (25–1000 nM) was established in human plasma using one-step liquid-liquid extraction. Alogliptin was used as an internal standard (IS) to attain good recovery and reproducibility while reducing the effects of the matrix. Enhanced plasma extraction of omarigliptin was successfully achieved with tertiary butyl methyl ether—diethyl ether (TBME-DEE) mixture as the extracting solvent, while using acetonitrile as the diluent solvent for the IS to effectively decrease the formed emulsion. Multiple Reaction Monitoring (MRM) of the transition pairs of m/z 399.2 to 153.0 for omarigliptin and m/z 340.2 to 116.0 for alogliptin was employed in positive Electro Spray Ionization (ESI) mode. Human plasma samples were collected after 1.5 h (t_max) of Marizev^® (12.5 mg) tablets administration to healthy human volunteers showing average concentration of 292.18 nM. Validation results were all satisfactory including successful stability studies with bias below 12%. The proposed study will be valuable for ethnicity comparison studies that will be commenced on omarigliptin in Egypt by the authors in prospective study, following the FDA recommends, to evaluate possible sub-group dissimilarities that include pharmacokinetic parameters. Full article

(This article belongs to the Special Issue Bioanalysis and Biological Matrix Sampling)

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18 pages, 1865 KiB

Open AccessFeature PaperArticle

Dried Urine Microsampling Coupled to Liquid Chromatography—Tandem Mass Spectrometry (LC–MS/MS) for the Analysis of Unconjugated Anabolic Androgenic Steroids

by Michele Protti, Camilla Marasca, Marco Cirrincione, Angelo E. Sberna, Roberto Mandrioli and Laura Mercolini

Molecules 2020, 25(14), 3210; https://doi.org/10.3390/molecules25143210 - 14 Jul 2020

Cited by 17 | Viewed by 4499

Abstract

Testing and monitoring anabolic androgenic steroids in biological fluids is a key activity in anti-doping practices. In this study, a novel approach is proposed, based on dried urine microsampling through two different workflows: dried urine spots (DUS) and volumetric absorptive microsampling (VAMS). Both techniques can overcome some common drawbacks of urine sampling, such as analyte instability and storage and transportation problems. Using an original, validated liquid chromatography–tandem mass spectrometry (LC-MS/MS) method, exogenous and endogenous unconjugated steroids were analysed. Despite the limitations of microsampling volume, good sensitivity was obtained (limit of quantitation ≤1.5 ng/mL for all analytes), with satisfactory precision (relative standard deviation <7.6%) and absolute recovery (>70.3%). Both microsampling platforms provide reliable results, in good agreement with those obtained from urine. Full article

(This article belongs to the Special Issue Bioanalysis and Biological Matrix Sampling)

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19 pages, 959 KiB

Open AccessReview

The Evolving Role of Microsampling in Therapeutic Drug Monitoring of Monoclonal Antibodies in Inflammatory Diseases

by Panagiotis-Dimitrios Mingas, Jurij Zdovc, Iztok Grabnar and Tomaž Vovk

Molecules 2021, 26(6), 1787; https://doi.org/10.3390/molecules26061787 - 22 Mar 2021

Cited by 8 | Viewed by 3776

Abstract

Monoclonal antibodies (mAbs) have been extensively developed over the past few years, for the treatment of various inflammatory diseases. They are large molecules characterized by complex pharmacokinetic and pharmacodynamic properties. Therapeutic drug monitoring (TDM) is routinely implemented in the therapy with mAbs, to monitor patients’ treatment response and to further guide dose adjustments. Serum has been the matrix of choice in the TDM of mAbs and its sampling requires the visit of the patients to laboratories that are not always easily accessible. Therefore, dried blood spots (DBS) and various microsampling techniques have been suggested as an alternative. DBS is a sampling technique in which capillary blood is deposited on a special filter paper. It is a relatively simple procedure, and the patients can perform the home-sampling. The convenience it offers has enabled its use in the quantification of small-molecule drugs, whilst in the recent years, studies aimed to develop microsampling methods that will facilitate the TDM of mAbs. Nevertheless, hematocrit still remains an obstacle that hinders a more widespread implementation of DBS in clinical practice. The introduction of novel analytical techniques and contemporary microsampling devices can be considered the steppingstone to the attempts made addressing this issue. Full article

(This article belongs to the Special Issue Bioanalysis and Biological Matrix Sampling)

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