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Breast cancer (BC) is the leading cause of cancer death among women worldwide, making the discovery and quantification of new biomarkers essential for improving diagnostic and preventive strategies to limit dissemination and improve prognosis. Essential trace metals such as Fe, Cu, and Zn may play critical roles in the pathophysiology of both benign and malignant breast tumors. However, due to the high metabolic activity and reduced element selectivity of cancer cells, also non-essential elements may be taken up and may even be implicated with disease progression. This study investigates the spatial distribution and concentrations of both essential and non-essential elements in breast tissues, assessing their potential for diagnostic applications. Laser ablation (LA)–inductively coupled plasma–mass spectrometry (ICP-MS) with a time-of-flight (ToF) mass analyzer (LA-ICP-ToF–MS) was used to inquire the distribution of almost all elements across the periodic table and their abundance in metastatic (n = 11), non-metastatic (n = 7), and healthy (n = 4) breast tissues. Quantification was achieved using gelatine-based standards for external calibration to quantitatively map various elements. Overall, the Fe, Cu, Zn, Sr, and Ba levels were significantly increased in tumor samples with Sr and Ba showing strong correlation, likely due to their similar chemistry. Comparison of calibrated LA-ICP-ToF–MS data with a histologic staining demonstrated the possibility to clearly differentiate between various tissue types and structures in breast tissues such as tumor niche and stroma. The levels of the studied elements were significantly higher in the tumor niche areas compared to the stroma, and for Fe, a significant accumulation was observed in the tumor niche areas from the metastatic patient group relative to the levels found in the same areas of the non-metastatic group. LA-ICP-ToF–MS was used to quantitatively map the biodistribution of essential and non-essential elements in metastatic and non-metastatic breast cancer tissues. [ABSTRACT FROM AUTHOR]

The study focuses on validating reference methods such as ICP-OES and ICP-MS for detecting ultra-trace levels of chromium in groundwater, where concentrations are typically very low. Additionally, it verifies a hyphenated technique, IC-ICP-MS, for determining naturally occurring Cr(VI) in tested waters. The validation process involved various chromium analysis variants, including isotopes 52Cr and 53Cr in ICP-MS and IC-ICP-MS techniques, along with specific emission lines in the ICP-OES technique. Statistical data processing revealed that the achieved limits of quantification for Cr in different techniques ranged from 0.053 µg/L to 1.3 µg/L, with the associated measurement uncertainty estimated between 14% and 19% (at a coverage factor k = 2, 95%). For speciation analysis, it was possible to quantitatively determine Cr(VI) at concentrations as low as 0.12 µg/L, with the measurement uncertainty ranging between 10% and 14%. The Kruskal-Wallis test indicated that for the 14 water samples analysed, there was no statistically significant difference in the results obtained using different analytical techniques (p > 0.05). The geochemical modelling approach applied enhances the understanding of chromium speciation in water samples, verifying the accuracy of speciation analysis and identifying specific ion forms in which Cr(III) and Cr(VI) occur. In the analysed water samples, the concentration of Cr(VI) ranges between 0.13 and 35 µg/L, with the primary form identified as the oxoanion CrO42−. Importantly, statistical tests demonstrated no statistically significant differences between the total chromium concentration in water and the concentration of Cr(VI), indicating that the entire concentration of total chromium corresponds to Cr(VI) speciation. [ABSTRACT FROM AUTHOR]

Until the end of the 70s of the last century, the major tool for fractionating complex polymers regarding molecular size is gel permeation chromatography (GPC) (more accurately size exclusion chromatography, SEC). A milestone in fractionating polymers with regard to chemical composition is achieved when it is shown that random copolymers can be separated according to copolymer composition using solvent gradient HPLC. Another important step toward selective fractionation is taken when liquid chromatography at the critical point of adsorption is introduced as an efficient way to separate functional polymers with regard to their functionality type distribution. Another milestone is the discovery that temperature gradients can also be used for the selective separation of complex polymers with regard to composition. The combination of different LC methods in comprehensive 2D HPLC setups is another milestone. As of today, a toolbox of HPLC methods is in place that enables the fractionation of complex polymers according to all molecular parameters including tacticity and branching. Here, an overview on the different techniques and some major applications is presented. The most important developments in the field are discussed, and different techniques, experimental protocols, and applications are highlighted. In conclusion, challenges for future developments are outlined. [ABSTRACT FROM AUTHOR]

Bio-based and biodegradable materials play a vital role in a sustainable and green economy. These materials must exhibit properties that are similar to or better than the properties of oil- or coal-based materials and require sophisticated synthesis technologies and detailed knowledge of structure–property correlations. For comprehensive molecular structure elucidation, advanced analytical methods, including coupled and hyphenated techniques that combine advanced fractionation and information-rich spectroscopic detectors, are an indispensable tool. One important tool for fractionating complex polymers regarding molecular size is size exclusion chromatography. For fractionating polymers with regard to chemical composition, solvent (or temperature) gradient HPLC has been developed. The combination of different liquid chromatography methods in comprehensive two-dimensional HPLC setups is another important tool. Today, a toolbox of HPLC methods is in place that enables the fractionation of complex bio-based and biodegradable polymers according to the most important molecular parameters including molecular size, composition, functionality, and branching. Here, an overview of the different techniques and some major applications is presented. Some representative developments in the field are discussed, and different techniques, experimental protocols, and applications are highlighted. [ABSTRACT FROM AUTHOR]

The extensive application of metallic nanoparticles (NPs) in several fields has significantly impacted our daily lives. Nonetheless, uncertainties persist regarding the toxicity and potential risks associated with the vast number of NPs entering the environment and human bodies, so the performance of toxicological studies are highly demanded. While traditional assays focus primarily on the effects, the comprehension of the underlying processes requires innovative analytical approaches that can detect, characterize, and quantify NPs in complex biological matrices. Among the available alternatives to achieve this information, mass spectrometry, and more concretely, inductively coupled plasma mass spectrometry (ICP-MS), has emerged as an appealing option. This work critically reviews the valuable contribution of ICP-MS-based techniques to investigate NP toxicity and their transformations during in vitro and in vivo toxicological assays. Various ICP-MS modalities, such as total elemental analysis, single particle or single-cell modes, and coupling with separation techniques, as well as the potential of laser ablation as a spatially resolved sample introduction approach, are explored and discussed. Moreover, this review addresses limitations, novel trends, and perspectives in the field of nanotoxicology, particularly concerning NP internalization and pathways. These processes encompass cellular uptake and quantification, localization, translocation to other cell compartments, and biological transformations. By leveraging the capabilities of ICP-MS, researchers can gain deeper insights into the behaviour and effects of NPs, which can pave the way for safer and more responsible use of these materials. [ABSTRACT FROM AUTHOR]

Innate immune systems alter the concentrations of trace elements in host niches in response to invading pathogens during infection. This work reports the interplay between d-block metal ions and their associated biomolecules using hyphenated elemental techniques to spatially quantify both elemental distributions and the abundance of specific transport proteins. Here, lung tissues were collected for analyses from naïve and Streptococcus pneumoniae-infected mice fed on a zinc-restricted or zinc-supplemented diet. Spatiotemporal distributions of manganese (55Mn), iron (56Fe), copper (63Cu), and zinc (66Zn) were determined by quantitative laser ablation–inductively coupled plasma–mass spectrometry. The murine transport proteins ZIP8 and ZIP14, which are associated with zinc transport, were also imaged by incorporation of immunohistochemistry techniques into the analytical workflow. Collectively, this work demonstrates the potential of a single instrumental platform suitable for multiplex analyses of tissues and labelled antibodies to investigate complex elemental interactions at the host-pathogen interface. Further, these methods have the potential for broad application to investigations of biological pathways where concomitant measurement of elements and biomolecules is crucial to understand the basis of disease and aid in development of new therapeutic approaches. [ABSTRACT FROM AUTHOR]

A simple, reliable, and stability‐indicating RP‐HPLC‐UV method was developed and validated for the estimation of related substances (p‐chlorophenol and unknown impurities) of chlorzoxazone (skeletal muscle relaxant). Along with this as the compound contains a potential genotoxic impurity (2‐amino‐4‐chlorophenol), which needs to have more sensitivity in quantification, we have also developed and validated a separate RP‐HPLC‐mass spectrometry (MS)/MS method for the estimation of 2‐amino‐4‐chlorophenol impurity. Both methods (RP‐HPLC‐UV & RP‐HPLC–MS/MS) were validated in accordance with International Council for Harmonization Q2(R1) and were found to be precise, accurate, robust, linear, and specific with limit of quantification values established with respect to 100% of test concentration, 0.018% w/w of p‐chlorophenol by RP‐HPLC‐UV, and 2 ppm of 2‐amino‐4‐chlorophenol by RP‐HPLC–MS. [ABSTRACT FROM AUTHOR]

Impurities found in active pharmaceutical ingredients (APIs) and pharmaceutical products are of ever‐increasing interest. According to several regulatory agencies, purity and impurity profiles are essential. An impurity is defined as any additional inorganic or organic material, residual solvents other than the medicinal components, or undesired compounds that remain with APIs. Impurities and degradation products in bulk drug materials and pharmaceutical formulations are identified, their structures are clarified, and their quantitative determination is part of impurity profiling. Unrecognized, poisonous impurities are dangerous to health and should be identified by selective procedures to increase the safety of drug therapy, and impurity profiling has become more significant in pharmaceutical analysis. This review briefly introduces process and product‐related impurities and emphasizes the creation of cutting‐edge analytical techniques for identifying them. It discusses the use of analytical methods, particularly high‐performance thin‐layer chromatography, liquid chromatography with mass spectrometry (MS), ultrahigh‐performance liquid chromatography, gas chromatography–MS, and nuclear magnetic resonance spectroscopy for the identification of contaminants and degradation products. It has discussed the importance of the quality, efficacy, and safety of drug substances and products, including the origin, types, and quality control of impurities, the need for the development of impurity profiling methods, impurity identification, and regulatory aspects. [ABSTRACT FROM AUTHOR]

Cannabis and its related products have increasingly been consumed in India as they produce the desired euphoric effects in human body. Cannabis blends many of the properties of alcohol, opium, tranquilizers, and hallucinogens and develops severe effects when synthesized using other chemicals. In India, cannabis is listed as a narcotic drug, and the consumption of cannabis is increasing steadily across the nation. Long-term and regular use of cannabis can lead to addiction and drug-facilitated crimes in our society. In such predicaments, conducting a chemical analysis for these drugs is necessary to detect the type and the amount of drug consumed by an abuser. For this purpose, chromatography coupled with mass spectrometry setups has been highly employed by researchers. This study is a review conducted on articles that have been developed and validated chromatography and mass spectrometry techniques between years 2015 and 2022 for the detection of cannabinoids. The sample preparation and extraction procedures employed in each research paper have been discussed in detail. The analytical parameters of the instrument used in each article have been tabulated, and the range of the same has been calculated. The review is a cumulative report of chromatography and mass spectrometric techniques used for the detection of natural and synthetic cannabinoids. The study offers a wide range of novel and modified extraction and analytical techniques implemented on different sample matrices. The report will help the experts to review and select suitable analytical method and parameters according to the matrix available for analysis. The study shows that the researchers prefer liquid chromatography-mass spectrometry setups for the detection of cannabinoids. [ABSTRACT FROM AUTHOR]

A hyphenated electrochemical technique consists of the combination of the coupling of an electrochemical technique with a non-electrochemical technique, such as spectroscopical and optical techniques, electrogravimetric techniques, and electromechanical techniques, among others. This review highlights the development of the use of this kind of technique to appreciate the useful information which can be extracted for the characterization of electroactive materials. The use of time derivatives and the acquisition of simultaneous signals from different techniques allow extra information from the crossed derivative functions in the dc-regime to be obtained. This strategy has also been effectively used in the ac-regime, reaching valuable information about the kinetics of the electrochemical processes taking place. Among others, molar masses of exchanged species or apparent molar absorptivities at different wavelengths have been estimated, increasing the knowledge of the mechanisms for different electrode processes. [ABSTRACT FROM AUTHOR]

Ferrate(VI) is a green and efficient water treatment agent for drinking and wastewater. It is widely used in water treatment because it has multi-functional uses such as oxidation, algae removal, disinfection, and adsorption flocculation. It does not cause secondary pollution to the environment. This paper compares ferrate(VI) with other water treatment agents and discusses three methods of preparing ferrate(VI). The removal, adsorption, and control of organic matter, algae, disinfection by-products, and heavy metal ions in water when ferrate(VI) was used as an oxidant, disinfectant, and coagulant were summarized. Ferrate(VI) has some advantages in removing toxic, harmful, and difficult-to-degrade substances from water. Due to the disadvantages of ferrate(VI) such as oxidation selectivity and instability, it is necessary to develop the hyphenated techniques of ferrate(VI). In this review, three hyphenated techniques of ferrate(VI) are summarized: ferrate(VI)–photocatalytic synergistic coupling, ferrate(VI)–PAA synergistic coupling, and ferrate(VI)–PMS synergistic coupling. [ABSTRACT FROM AUTHOR]

Colorimetric sensors are preferred for visually detecting target analytes, but achieving ultra-low detection capabilities for food analysis, environmental samples, and molecular diagnostics is challenging. In this study, we interfaced a purpald-based formaldehyde color sensor (as a model probe reaction) with a surface plasmon gold microarray imaging chip. Such hyphenated surface-sensitive signal-amplifying techniques enabled ultra-low detection in biofluids with a linear range of 10−5 – 0.5 ppm compared to the spectrophotometric narrower linear range of 0.01–1 ppm. The detection limit of 86×10−6 ppm from the hyphenated sensing is 140-fold lower than the detection limit from the spectrophotometric method alone (12×10−3 ppm). The absorbance maximum of the purpald-formaldehyde adduct was 553 nm, with no notable tail overlap between the adduct absorbance band beyond 700 nm and the fixed angle source incident wavelength of 800 nm from the surface plasmon instrument. Hence, the possible adduct thiol-surface plasmon gold surface interaction, affinity, and the higher mass and refractive index changes of the adduct are likely causes of the observed signal amplification. We achieved a formaldehyde sample recovery of 92 % from a diluted serum (a minimally invasive assay method), which was comparable to the results in a buffer solution. Further, we extended to demonstrate in diluted urine sample matrices to be noninvasive bioanalysis and determined the interference from urea that could also form a purpald adduct like formaldehyde. In conclusion, coupling a surface-sensitive transducer with less sensitive colorimetric reactions is promising for molecular diagnostics in real samples and can be broadly extended to any other desired molecular targets and sample matrices. [Display omitted] • Colorimetric sensor is directly integrated with a surface plasmon transducer. • Several orders of shift in lower detection limits are achieved from the integration. • Formaldehyde-purpald color adduct is used as the probe reaction. • Diluted serum and salivary sample matrices are demonstrated with a sensor adduct mechanism. • Broader applicability of small molecule detection methodology is significant. [ABSTRACT FROM AUTHOR]

In recent period of time, mankind has been giving more and more effort towards dietary supplements because now people are more concerned about their health. So, the availability and uses are also increased. For enhancing the frequency and effect of the dietary supplements, synthetic products like Phosphodiesterase Type 5 (PDE-5) Inhibitor, Cocaine, Fluoxetine, or some unwanted steroids are added to the supplements to enhance their market value. The consumption of these adulterated supplements has been linked to health problems and has had a negative impact on the quality and safety of dietary supplements as well as public health. To stop such dishonest practises, analytical techniques that enable quick and accurate testing of dietary supplements for the presence of synthetic drugs are required. For the determination of adulterated products in dietary supplements there are so many hyphenated techniques are available among all Gas Chromatography and Mass Spectrometry (GC-MS) is more specific and delicate because of its unique combination of Mass Spectrometry and Gas chromatography which helps in the field of Separation and structural identification of the adulterant. The role of GC-MS in the detection, quantification, conformation analysis of adulterants in dietary supplements is evaluated critically in the current review.

Proton-transfer reaction mass spectrometry (PTR-MS) is a versatile tool for the mass spectrometric analysis of organic molecules in gaseous samples. Due to its operation principle, PTR-MS is a soft ionization technique generating spectral data typically rich in protonated molecule information. Most of the currently reported PTR-MS applications are designed to determine volatile compounds. Herein, we present a redesigned instrumental setup termed "high-temperature (HT)-PTR-MS" with improved capabilities for the analysis of low-volatile compounds. The developed HT-PTR-MS prototype was successfully hyphenated with gas chromatography (GC) to enable qualitative and quantitative analysis of licit and illicit drugs in human blood/plasma samples. Different kinds of spiked and authentic samples were used to evaluate the performance of the GC-HT-PTR-MS in forensic drug testing. Benchmarking against GC-MS with electron ionization demonstrated the improved detection capabilities of GC-HT-PTR-MS in screening applications. On average, one order of magnitude lower limits of detection/identification were reached. Clearly, GC-HT-PTR-MS has the vast potential to complement or even replace established mass spectrometric techniques in forensic drug analysis. [ABSTRACT FROM AUTHOR]

Nanotechnology has prompted new aspirations for managing modern human challenges. Furthermore, it has been utilized for aid in the prevention, diagnosis, and treatment of ovulatory disorders. Women with ovulatory issues may benefit from formulations using nanotechnology as an alternative possible treatment. Clomiphene citrate is a nonsteroidal, ovulatory stimulant that acts as a selective estrogen receptor modulator (SERM). It is a triphenyl ethylene stilbene derivative that is primarily used to trigger ovulation in female infertility cases where there is anovulation. Anovulatory infertility is most frequently caused by polycystic ovarian syndrome (PCOS), which is a gynecological endocrine disorder. Elevated serum concentrations of androgens, LH, and insulin are the main features of its endocrine profile. The primary goal of treating PCOS-related infertility is to increase the amount of FSH that is exposed to the ovary, either by antagonizing the estrogenic effects of clomiphene citrate in the hypothalamus or by directly affecting the ovary using recombinant follicle-stimulating hormone (FSH). In about 80% of treated individuals, ovulation is recovered by clomiphene citrate. In this review, we discuss the chemistry and pharmacology of clomiphene citrate, as well as the delivery of clomiphene citrate via nanosystems for improving solubility and limiting side-effects. The hyphenated techniques for analyzing and quantifying clomiphene citrate in solvents and biological samples are also overviewed.

Narcotic drugs have analgesic properties due to which they are commonly consumed to relieve pain from the body. The mode of action of these drugs is to depress the central nervous system. Long-term consumption of narcotic drugs can lead to physical dependency and drug abuse complications. In India, abuse of prohibited narcotic drugs such as cocaine, opium and cannabis by the young generation is to the great extent and the drug-facilitated crimes are also increasing day by day. In such scenarios, detection and identification of these drugs become an integral part of forensic investigation. Among the various analytical techniques, chromatography and mass spectrometry techniques have been predominantly used for the detection of narcotic drugs. In this review, research articles on chromatography and mass spectrometry techniques used for the detection of cocaine, published between 2015 and 2021, have been collected. The methods of sample collection, preparation, and extraction, and the data such as the analytical parameters, sample matrix, mode of analysis, and the manufacturing company employed in each research have been accumulated. The range of LOD, LOQ, retention time, and mass-to-charge ratio has been analyzed. This review will serve as a collective report of chromatography and mass spectrometric techniques used in the past six years for the detection of cocaine. It will also help the scientific officers to analyze and choose a finer analytical technique with respect to the matrix and sample volume available for the analysis. The results of the review indicate that hyphenated techniques of chromatography and mass spectrometry serve as an ideal technique for cocaine detection. [ABSTRACT FROM AUTHOR]

Medicinal plant metabolomics has emerged as a goldmine for the natural product chemists. It provides a pool of bioactive phytoconstituents leading to accelerated novel discoveries and the elucidation of a variety of biosynthetic pathways. Further, it also acts as an innovative tool for herbal medicine's scientific validation and quality assurance. This review highlights different strategies and analytical techniques employed in the practice of metabolomics. Further, it also discusses several other applications and advantages of metabolomics in the area of natural product chemistry. Additional examples of integrating metabolomics with multivariate data analysis techniques for some Indian medicinal plants are also reviewed. Recent technical advances in mass spectrometry‐based hyphenated techniques, nuclear magnetic resonance‐based techniques, and comprehensive hyphenated technologies for phytometabolite profiling studies have also been reviewed. Mass Spectral Imaging (MSI) has been presented as a highly promising method for high precision in situ spatiotemporal monitoring of phytometabolites. We conclude by introducing GNPS (Global Natural Products Social Molecular Networking) as an emerging platform to make social networks of related molecules, to explore data and to annotate more metabolites, and expand the networks to novel "predictive" metabolites that can be validated. [ABSTRACT FROM AUTHOR]

Introduction: The chemical diversity of plants plays an essential role in the development of new drugs. However, new bioactive compound identification and isolation are challenging due to the complexity and time‐consuming nature of the traditional process. Recently, alternative strategies have become popular, such as the statistical approach to correlate compounds with biological activities, overcoming bottlenecks in bioactive natural product research. Objective: We aimed to determine bioactive compounds against resistant human melanoma cells from leaves of Aspidosperma subincanum, Copaifera langsdorffii, Coussarea hydrangeifolia, Guarea guidonea and Tapirira guianensis, using a metabolomics approach. Material and Methods: The extracts and fractions were obtained by accelerated solvent extraction (ASE) and tested against resistant melanoma cells SK‐MEL‐28 and SK‐MEL‐103. Chemical analysis was performed by high‐performance diode array detector tandem mass spectrometry (HPLC‐DAD‐MS/MS). Chemical and biological data were analysed through univariate and multivariate analysis. Results: The species present high chemical diversity, including indole alkaloids, glycosylated flavonoids, galloylquinic acid derivatives, cinnamic acid derivatives, and terpenes. The ASE fractionation separated the compounds according to the physicochemical properties; only C. langsdorffii and T. guianensis extracts were active. Both results from the chemical profile and the biological assay were treated using a metabolomics approach to identify the contribution of different classes of secondary metabolites in the viability of human melanoma cells. The analyses showed the metabolites from C. langsdorffii and T. guianensis, such as polyphenols and terpenes, were the main compounds correlated with the biological response. Conclusion: These findings afford alternative pathways that are trustworthy and less time‐consuming to identify new bioactive compounds against multidrug‐resistant human melanoma cells. We determined bioactive compounds against resistant human melanoma SK‐MEL‐28 and SK‐MEL‐103 cells from Aspidosperma subincanum, Copaifera langsdorffii, Coussarea hydrangeifolia, Guarea guidonea, and Tapirira guianensis, using ASE, HPLC‐DAD‐MS/MS, and metabolomics. The species have alkaloids, glycosylated flavonoids, galloylquinic acid derivatives, cinnamic acid derivatives, and terpenes. C. langsdorffii and T. guianensis were active; metabolomics identifies polyphenols and terpenes as the main compounds correlated with the biological response. These findings afford alternative pathways that are trustworthy and less time‐consuming to identify new bioactive compounds. [ABSTRACT FROM AUTHOR]

Introduction: Human blood and saliva are increasingly under investigation for the detection of biomarkers for early diagnosis of non-communicable (e.g.cancers) and communicable diseases like COVID-19. Exploring the potential application of human tears, an easily accessible body fluid, for the diagnosis of various diseases is the need of the hour. Areas covered: This review deals with a comprehensive account of applications of tear analysis using different techniques, their comparison and overall progress achieved till now. The techniques used for tear fluid analysis are HPLC/UPLC/SDS-PAGE, CE, etc., together with ELISA, Mass Spectrometry, etc. But, with advances in instrumentation and data processing methods, it has become easy to couple the various separation methods with highly sensitive optical techniques for the analysis of body fluids. Expert opinion: Tear analysis can provide valuable information about the health condition of the eyes since it contains several molecular constituents, and their relative concentrations may alter under abnormal conditions. Tear analysis has the advantage that it is totally non-invasive. This study recommends tear fluid as a reliable clinical sample to be probed by highly sensitive optical techniques to diagnose different health conditions, with special emphasis on eye diseases. [ABSTRACT FROM AUTHOR]

[Display omitted] • Identifying and managing PGIs in synthetic processes is arduous. • There is a growing preference for sophisticated hyphenated techniques for the detection of PGIs. • Precise and accurate quantification is achieved by using hyphenated techniques. • Quantifying PGIs help in development of robust regulatory framework for new drugs. Genotoxin is a chemical that has the potential to cause DNA damage, which can result in germline and somatic mutations leading to malignant transformation and cause cancer. The assessment and control of GTIs in pharmaceuticals at trace levels are raising concerns to both the pharmaceutical and regulatory agencies due to this possibility for human carcinogens. Identifying these GTIs at trace levels requires a sophisticated approach, which poses significant challenges for analysts in pharmaceutical research and development. Therefore, it is crucial to understand the various issues related to GTIs and find the potential ways to address them. This article provides a brief overview of the various sources of potential impurities in drug components, such as active pharmaceutical ingredients (APIs), GTIs in food and cosmetics, identification of GTIs using advanced techniques like high-performance liquid chromatography-mass spectroscopy (LC-MS) and gas chromatography-mass spectroscopy (GC–MS). In addition to the sources and identification of GTIs in drug components, the article covers APIs that contain GTIs and their determination using analytical techniques and explores the optimized results obtained from this determination. [ABSTRACT FROM AUTHOR]

[Display omitted] Current challenges in oncology are largely associated with the need to improve the effectiveness of cancer treatment and to reduce drug's side effects. An effective strategy to cope with these challenges is behind designing and developing drug delivery systems based on smart nanomaterials and approved anticancer drugs. The present study offers a novel and straightforward approach to efficiently load the cisplatin drug into the newly constructed liposome-based nanosystems as well a reliable technique for monitoring this process based on capillary electrophoresis hyphenated with inductively coupled plasma tandem mass spectrometry. The proposed drug-loading methodology comprises liposome formation via a simple ethanol-injection method and propels increased drug encapsulation using tailor-made freeze-thawing or lyophilization-hydration procedures. To optimize liposome generation and drug encapsulation, the effects of dilution medium and liposome composition (types of phospholipids and their percentage ratio) have been investigated in detail. It was shown that modest alterations of the composition of three-component phospholipid liposomes and parameters of the freeze-thawing procedure have a strong impact on the formation of cisplatin–liposome systems. The obtained cisplatin–liposome formulation features a remarkable degree of drug encapsulation, over 100 mg L–1, and holds promise for further preclinical development as a potent drug-delivery platform. [ABSTRACT FROM AUTHOR]

Co‐crystallisation is widely explored as a route to improve the physical properties of pharmaceutical active ingredients, but little is known about the fundamental mechanisms of the process. Herein, we apply a hyphenated differential scanning calorimetry—X‐ray diffraction technique to mimic the commercial hot melt extrusion process, and explore the heat‐induced synthesis of a series of new co‐crystals containing isonicotinamide. These comprise a 1:1 co‐crystal with 4‐hydroxybenzoic acid, 2:1 and 1:2 systems with 4‐hydroxyphenylacetic acid and a 1:1 crystal with 3,4‐dihydroxyphenylactic acid. The formation of co‐crystals during heating is complex mechanistically. In addition to co‐crystallisation, conversions between polymorphs of the co‐former starting materials and co‐crystal products are also observed. A subsequent study exploring the use of inkjet printing and milling to generate co‐crystals revealed that the synthetic approach has a major effect on the co‐crystal species and polymorphs produced. [ABSTRACT FROM AUTHOR]

Expectations for continuous miniaturization in mass spectrometry are not declining for years. Portable instruments are highly welcome by the industry, science, space agencies, forensic laboratories, and many other units. All are striving for the small, cheap, and as good as possible instruments. This review describes the recent developments of miniature mass spectrometers and also provides selected applications where these devices are used. Upcoming perspectives of further development are also discussed. @ 2019 John Wiley & Sons Ltd. Mass Spec Rev [ABSTRACT FROM AUTHOR]

Hyphenation of electrochemistry and mass spectrometry is an attractive method to investigate oxidation and reduction processes. By using mass spectrometry, electrochemically generated products can be identified. In this Review, different approaches to electrochemistry–mass spectrometry will be summarized, including hyphenation of electrochemical flow cells to mass spectrometry as well as integration of separation steps between electrochemical reactions and detection of products. Fields of application range from bioanalytical studies to studies regarding corrosion, electrosynthesis and energy carriers. Important historical developments will be highlighted, followed by an overview of terminology and instrumental setups and discussion of developments within recent years (2017–2020). [ABSTRACT FROM AUTHOR]

Nonadherence to prescribed pharmacotherapy is an understated public health problem globally and is costing many patients their chance to return to good health and healthcare systems billions. Clinicians need an accurate assessment of adherence to medications to aid the clinical decision-making process in the event of poor patient progress and to maximise the patient health outcomes from the drug therapies prescribed. An overview of indirect and direct methods used to measure medication adherence is presented, highlighting the potential for accurate measuring of drugs in biological samples using hyphenated mass spectrometry (MS) techniques to provide healthcare professionals with a reliable evidence base for clinical decision making. In this review we summarise published applications of hyphenated MS techniques for a diverse range of clinical areas demonstrating the rise in the use of such direct methods for assessing medication adherence. Although liquid chromatography-tandem mass spectrometry (LC-MS/MS) methods using plasma, serum and urine samples are the most popular, in recent years increased attention has been given to liquid chromatography high-resolution mass spectrometry (LC-HRMS) methods and alternative biosample matrices including hair, saliva and blood microsamples. The advantages and challenges of using hyphenated MS techniques to address this healthcare problem are also discussed alongside future perspectives. [ABSTRACT FROM AUTHOR]

The increased availability and use of botanical dietary supplements (BDS) has been accompanied by an increased frequency of adulteration of these products with pharmaceutical chemicals. These adulterated products are a worldwide problem, and their consumption poses health risks to consumers. The main focus of this paper is to highlight novel screening approaches utilized in the detection of adulterants in BDS marketed for different therapeutic purposes. We summarize spectroscopic methods involving near-infrared, infrared, Raman, and nuclear magnetic resonance spectroscopy as feasible and interesting in-field screening tools for the analysis of suspected products (adulterated or not) before being sent to a laboratory for deeper inspection. In addition, the new approaches based on chromatographic methods such as liquid chromatography-circular dichroism, liquid chromatography-mass spectrometry, thin layer chromatography-surface enhanced Raman spectroscopy, and thin layer chromatography-mass spectrometry are discussed and reviewed. Novel analysis strategies from targeted analysis to post-targeted and non-targeted analysis allowing simultaneous determination of the number of multiclass pharmaceuticals are discussed.

In this study, the polymorphic transitions of mefenamic acid (MA) were studied by synchrotron X‐ray powder diffraction combined with differential scanning calorimetry (XRD‐DSC). The initial material was found to be phase‐pure form I which, when heated, produces two endotherms that can be observed by DSC at 162.72 and 219.55°C. The former was found to correspond to a solid–solid enantiotropic transition from form I to a mixture of forms II and III. The latter is the melting point of form II. As form I is heated, significantly greater unit‐cell expansion is seen in the a direction than in b and c, which can be explained by the stronger intermolecular interactions in the bc plane. Refinements of the reported MA structures against the patterns collected during heating revealed that at 175°C there exists a mixture of forms I, II and III, whereas only forms II and III remain at 205°C. However, reflections are observed at both temperatures which cannot be fitted with the known forms of MA. It is hypothesized that a new form of MA is produced upon heating. The stability of MA after the enantiotropic transition temperature is II > III > I, which differs from the previously reported II > I > III. [ABSTRACT FROM AUTHOR]

Sensitive and robust in situ chemical analysis of organic biomarkers is essential in the endeavor of finding chemical signatures of life either extinct or extant on our solar system bodies such as Europa, Enceladus, or Titan. Development of new analytical instruments and accompanying methodologies are needed, especially those that are compatible with unknown and diverse samples potentially found on solar system targets and that avoid complexities involved with other wet chemistry techniques (desalting, derivatization and contamination issues, etc.). In this study, we demonstrate that online supercritical fluid extraction and supercritical fluid chromatography with water-saturated CO2 can extract and separate nonpolar analytes of astrobiological interest, such as free fatty acids, polycyclic aromatic hydrocarbons, and polycyclic aromatic compounds containing nitrogen or sulfur. Silica was used as a support material to immobilize aqueous samples during extraction. A C18 stationary phase with an embedded polar functional group and efficient end-capping in combination with water in the mobile phase allowed efficient separation of both free fatty acids and basic compounds. The total analysis time was 30 min, including extraction, equilibration, and separation. Detection was performed with a UV detector and a quadrupole mass spectrometer equipped with electrospray ionization. The method was validated in terms of lower detection limits (0.02–40 μg/L), precision (repeatability 3–13%), relative standard deviation (RSD), intermediate precision 4–26% (RSD), trueness (bias ranging from − 48 to 9%), and retention time shifts (< 2% RSD) for 16 analytes in sample matrices with sodium chloride and magnesium sulfate that may be present in ocean worlds such as Europa or Enceladus. [ABSTRACT FROM AUTHOR]

Abstract Recently, the high analytical power provided by the new HRMS instruments (working in the MS or MS/MS mode, stand alone or hyphenated with separation techniques) is making more feasible the characterization of plant secondary metabolites. In this regard, HRMS-based techniques are becoming the technique of choice, since they are capable of answering many questions regarding the analytical characterization of secondary metabolites, usually found in very complex matrices, including their structural elucidation and quantification in a very fast and sensitive way. In this manuscript we will provide a critical and updated revision of this topic covering the works published in the last 4 years (2015–2018), including the different configurations in which HRMS may be used (stand alone or hyphenated), the data treatment, the strategies for the identification of unknown metabolites, the current software for structure elucidation, as well as the last trends and future outlooks in this hot area of research. Highlights • Recent HRMS-based applications for plant secondary metabolites are reviewed. • Stand alone or hyphenated HRMS configurations are discussed and compared. • A broad variety of databases and HRMS-data mining strategies are presented. • Future challenges in dereplication and metabolite profiling are emphasized. [ABSTRACT FROM AUTHOR]

Deep eutectic solvents (DESs) as new and green solvents, are formed by two or three components combined by hydrogen bond interactions to create a eutectic mixture with a melting point lower than the original components. The core focus of this review is on DES-based sample preparation methods considering microextraction methods performed prior to chromatographic techniques consisting of gas chromatography (GC) and liquid chromatography (LC) equipped with mass spectrometry (MS). Depending on the nature of DES, there are various ways to utilization of them in extraction procedures, including liquid- and solid-based extraction approaches. For the writing of the current paper, the main terms "DES", "extraction" and related terms were searched in Google Scholar, and all related articles were selected until 2023. An attempt has been made to present the field employing DESs in the extraction as having a backward-looking compilation. Fundamental recommendations were compiled to inform the future development of DES-based extraction approaches. • DES preparation, composition, and type were reviewed. • DES-based sample preparation methods performed prior to gas and liquid chromatography techniques were reviewed. • The review was focused on the use of hyphenated chromatographic methods with mass spectrometry and tandem mass spectrometry. • Advantages and disadvantages of all developed methods were discussed. [ABSTRACT FROM AUTHOR]

Liquid chromatography (LC)–nuclear magnetic resonance (NMR) combines the advantage of the outstanding separation power of liquid chromatography (LC) and the superior structural elucidating capability of nuclear magnetic resonance (NMR). NMR has proved that it is a standout detector for LC by providing maximum structural information about plant originated extracts, particularly on the isolating ability of isomeric (same molecular formula) and/or isobaric (same molecular weight) compounds as compared to other detectors. The present review provides an overview of the developmental trends and application of LC–NMR in natural product analysis. The different LC–NMR operational modes are described, and how technical improvements assist in establishing this powerful technique as an important analytical tool in the analysis of complex plant-derived compounds is also highlighted. On-flow, stop-flow and loop-storage modes, as well as the new offline mode LC–solid phase extraction (SPE)–NMR and capillary LC (capLC)–NMR configurations which avoid the ingestion of expensive deuterated solvents throughout the experiment, are mentioned. Utilization of cryogenic probe and microprobe technologies, which are the other important promising approaches for guaranteeing sensitivity, are also described. Concluding remarks and future outlooks are also discussed.

Recently, high demand of high-throughput analyses with high sensitivity and selectivity to molecules and drugs in different classes with different physical-chemical properties—and a reduction in analysis time—is a principal milestone for novel methodologies that researchers are trying to achieve—especially when analytical procedures are applied to clinical purposes. In addition, to avoid high doses of a single drug that could cause serious side effects, multi-drug therapies are often used to treat numerous diseases. For these reasons, the demand for methods that allow the rapid analysis of mixed compounds has increased in recent years. In order to respond to these needs, new methods and instruments have been developed. However, often the complexity of a matrix can require a long time for the preparation and processing of the samples. Different problems in terms of components, types of matrices, compounds and physical-chemical complexity are encountered when considering drugs association profiles for quantitative analyses. This review addresses not only recently optimized procedures such as chromatographic separation, but also methods that have allowed us to obtain accuracy (precision and trueness), sensitivity and selectivity in quantitative analyses for cases of drug associations.