Combining surface-enhanced Raman spectroscopy (SERS) and paper spray mass spectrometry (PS-MS) for illicit drug detection.

There is an ongoing effort in the US illicit drug market to make new psychoactive compounds more potent and addictive. Due to continuous chemical modifications, many fentanyl analogs are developed and mixed with more traditional illicit drugs, such as cocaine and heroin. Detecting fentanyl and fentanyl analogs in these illicit drug mixtures has become more crucial because of the increased potency and associated health risks. Most confirmatory procedures require time-consuming and expensive, highly sophisticated laboratory equipment and experimental procedures, which can delay critical information that might save a victim or find a suspect. In this study, we propose miniaturizing and accelerating this process by combining surface-enhanced Raman spectroscopy (SERS) analysis and paper spray mass spectrometry (PS-MS). For this aim, dual-purposed paper substrates were developed through soaking in Au/Ag nanostars suspensions. These novel, in-house prepared paper SERS substrates showed stability for up to four weeks with and without the presence of drug compounds. Fentanyl analogs with similar SERS spectra were differentiated by coupling with PS-MS. The limit of detection (LOD) for fentanyl on the paper substrates is 34 µg/mL and 0.32 µg/mL for SERS and PS-MS, respectively. Fentanyl and fentanyl analogs show selective SERS enhancement that helped to detect trace amounts of these opioids in heroin and cocaine street samples. In short, we propose the combination of SERS/PS-MS by using modified paper substrates to develop cost-effective, sensitive, rapid, portable, reliable, and reproducible methods to detect illicit drugs, especially trace amounts of fentanyl and fentanyl analogs in illicit drug mixtures. The combination of these two category A techniques allows for the identification of illicit drugs according to the SWGDRUG guidelines.

Development and validation of a quantitative method for the analysis of delta-9-tetrahydrocannabinol (delta-9-THC), delta-8-tetrahydrocannabinol (delta-8-THC), delta-9-tetrahydrocannabinolic acid (THCA), and cannabidiol (CBD) in botanicals, edibles, liquids, oils, waxes, and bath products by gas chromatography mass spectrometry (GC/MS).

A quantitative gas chromatography mass spectrometry (GC/MS) method was developed for delta-9-tetrahydrocannabinol (delta-9-THC), delta-8-tetrahydrocannabinol (delta-8-THC), tetrahydrocannabinolic acid (THCA), and cannabidiol (CBD) in matrices including plant material, liquids and oils, waxes, edibles, and bath and body products. Samples were prepared by homogenization, extraction of the cannabinoids into solvent, liquid/liquid extraction, and derivatization. The GC/MS method was validated from 0.15% to 5.00% (weight basis) to encompass the 0.3% legal distinction between hemp and marijuana. Validation was performed assessing imprecision/bias, calibration model, recovery, interferences, limit of detection, matrix matching, carryover, accuracy, and an assessment of CBD conversion to delta-9-THC. The calibration curves were quadratic weighted 1/x with r2 > 0.990. The method had a detection limit of 0.075% in plant material for each analyte. Analyte recovery was greater than 70% in plant material. Carryover was not observed up to concentrations equivalent to 100% analyte, and no forensically significant conversion of CBD to delta-9-THC was observed. One cannabinoid isomer, 9(R)-delta-7-tetrahydrocannabinol (9(R)-delta-7-THC), was determined to interfere with the quantitation of delta-9-THC, but could be differentiated based on mass spectrum. The method was determined to be suitable for quantitation of delta-9-THC, delta-8-THC, delta-9-THCA, and CBD and was able to differentiate hemp samples from marijuana samples.

Rapid Separation and Detection of Drugs in Complex Biological Matrix Using TD-CDI Mass Spectrometer.

The drug detection technology plays a pivotal role in the domains of pharmaceutical regulation and law enforcement. In this study, we introduce a method that combines thermal desorption corona discharge ionization (TD-CDI) with mass spectrometry for efficient drug detection. The TD-CDI module, characterized by its compact and simple design, enables the separation of analytes within seconds and real-time presentation of one or two analyte peaks on the mass spectrum most of the time, which reduces matrix interference and improves detection performance. Through experimental investigation, we studied the characteristics of TD-CDI for analyte separation and detection, even with the same mass number, and optimized the TD-CDI approach. TD-CDI-MS was employed for the rapid detection of drugs in various traditional medicine, food products, and human samples. Additionally, by utilizing TD-CDI for segmented hair direct analysis, it becomes possible to trace the drug usage cycle of individuals. This underscores the feasibility of the proposed analytical method within the realm of drug detection.

Efficient magnetic solid-phase extraction, UPLC-MS/MS detection, and consumption assessment of five trace psychoactive substances.

Wastewater-based epidemiology (WBE) has become an objective and updated surveillance strategy for monitoring and estimating consumption trends of psychoactive substances (PSs) in the population. Firstly, magnetic shrimp shell biochar-based adsorbent (DZMBC) was synthesized and employed for extraction trace PSs from municipal wastewater. Proper pyrolysis temperature and increased KOH activator content favored the pore structure and surface area, thus facilitating extraction. DZMBC delivered exceptional extraction performance such as pH stability, anti-interference property, fast magnetic separation ability, reusability, and reproducibility. Then, a method based on magnetic solid-phase extraction (MSPE) followed by ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed, validated, and utilized for the quantitative determination of five PSs in real wastewater samples. Methodological validation results indicated a favorable linearity, low method limits of detection (1.00-4.75 ng/L), and good precisions (intra-day and inter-day relative standard deviations < 4.8%). Finally, an objective snapshot of Chongqing drug use and consumption pattern was obtained. Methamphetamine (MAMP) and 3,4-methylenedioxymethamphetamine (MDMA) were the prevalent illegal drugs in local. Both concentrations and per capita consumption of MDMA displayed a change (P < 0.05) between July and September, while no statistical differences were observed for each week.

Long term online desalting analysis of MS/LC-MS using thermal assisted recrystallization ionization.

Mass spectrometric analysis of non-volatile salts containing samples remains challenging due to salt-induced ion suppression and contamination. This challenge is even more pronounced for a liquid chromatography-mass spectrometry analysis, where the accumulation of salts in the transmission system poses an ongoing problem. In this study, a novel thermal assisted recrystallization ionization mass spectrometry (TARI-MS) device was developed to achieve efficient on-line desalting and prolonged analysis of saline samples. The core component of this device was a heated plate positioned between the electrospray unit and the MS inlet. The desalting mechanism was demonstrated as the spontaneous separation of target molecules from salts during the "crystallization" process. After optimization, the angle between the nebulizer and the heated plate was 45°; the distance between the front end of the heated plate and the MS inlet was 2 mm; the distance between the front edge of the heated plate and the center of the sample spray projected onto the heating plate was 3 mm; the distance between the emitter of nebulizer and the heated plate was 3 mm. TARI-MS realized direct analysis of eight drugs dissolved in eight commonly used non-volatile salts solutions (up to 0.5 mol/L). The high sensitivity, repeatability, linearity, accuracy, and intra- and inter-day precision of TARI-MS confirm its reliability as a robust tool for the analysis of saline samples. Furthermore, TARI-MS allowed continuous analysis of salty eluates of LC for up to nearly 1 h without maintenance and verified the feasibility of LC-MS analysis through detecting a five-drug mixture and a crude aripiprazole product. Finally, six impurities in the crude aripiprazole product were successfully detected by LC-TARI-MS. The established method holds promise for applications across academic and pharmaceutical domains.

Nanomaterials as catalysts for the sensitive and selective determination of diclofenac.

Background and purpose: Diclofenac (DCF) is a non-steroidal anti-inflammatory drug possessing analgesic and antipyretic properties. It is used for the treatment of rheumatoid arthritis pain, osteoarthritis, and acute muscle pain conditions and can be administrated orally, topically or intravenously. Because of its widespread use, hydrophilicity, stability and poor degradation (bioaccumulation in the food chain), DCF is an emerging chemical contaminant that can cause adverse effects in the ecosystems. Taking into account the consumption of DCF in pharmaceutical formulations and its negative impact on the environment, the development of new sensitive, selective, cheap, fast, and online capable analytical devices is needed for on-site applications. Experimental approach: This brief review attempts to cover the recent developments related to the use of nanomaterials as catalysts for electrochemical determination of DCF in pharmaceutical formulations, biological fluids and environmental samples. Key results: The article aims to prove how electrochemical sensors represent reliable alternatives to conventional methods for DCF analysis. Conclusion: The manuscript highlights the progress in the development of electrochemical sensors for DCF detection. We have analyzed numerous recent papers (mainly since 2019) on sensors developed for the quantitative determination of DCF, indicating the limit of detection, linear range, stability, reproducibility, and analytical applications. Current challenges related to the sensor design and future perspectives are outlined.

Machine learning-enhanced drug testing for simultaneous morphine and methadone detection in urinary biofluids.

The simultaneous identification of drugs has considerable difficulties due to the intricate interplay of analytes and the interference present in biological matrices. In this study, we introduce an innovative electrochemical sensor that overcomes these hurdles, enabling the precise and simultaneous determination of morphine (MOR), methadone (MET), and uric acid (UA) in urine samples. The sensor harnesses the strategically adapted carbon nanotubes (CNT) modified with graphitic carbon nitride (g-C3N4) nanosheets to ensure exceptional precision and sensitivity for the targeted analytes. Through systematic optimization of pivotal parameters, we attained accurate and quantitative measurements of the analytes within intricate matrices employing the fast Fourier transform (FFT) voltammetry technique. The sensor's performance was validated using 17 training and 12 test solutions, employing the widely acclaimed machine learning method, partial least squares (PLS), for predictive modeling. The root mean square error of cross-validation (RMSECV) values for morphine, methadone, and uric acid were significantly low, measuring 0.1827 µM, 0.1951 µM, and 0.1584 µM, respectively, with corresponding root mean square error of prediction (RMSEP) values of 0.1925 µM, 0.2035 µM, and 0.1659 µM. These results showcased the robust resiliency and reliability of our predictive model. Our sensor's efficacy in real urine samples was demonstrated by the narrow range of relative standard deviation (RSD) values, ranging from 3.71 to 5.26%, and recovery percentages from 96 to 106%. This performance underscores the potential of the sensor for practical and clinical applications, offering precise measurements even in complex and variable biological matrices. The successful integration of g-C3N4-CNT nanocomposites and the robust PLS method has driven the evolution of sophisticated electrochemical sensors, initiating a transformative era in drug analysis.

Current Analytical Methods for the Sensitive Assay of New-Generation Ovarian Cancer Drugs in Pharmaceutical and Biological Samples.

Ovarian cancer, which affects the female reproductive organs, is one of the most common types of cancer. Since this type of cancer has a high mortality rate from gynaecological cancers, the scientific community shows great interest in studies on its treatment. Chemotherapy, radiotherapy, and surgical treatment methods are used in its treatment. In the absence of targeted treatments in these treatment methods, side effects occur in patients, and patients show resistance to the drug. In addition, the underlying causes of ovarian cancer are still not fully known. The scientific world thinks that genetic factors, environmental conditions, and consumed foods may cause this cancer. The most important factor in the treatment of ovarian cancer is early diagnosis. Therefore, the drugs used in the treatment of ovarian cancer are platinum-based anticancer drugs. In addition to these drugs, the most preferred treatment method recently is targeted treatment approaches using poly(adenosine diphosphate ribose) polymerase (PARP) inhibitors. In this review, studies on the sensitive analysis of the treatment methods of these new-generation drugs used in the treatment of ovarian cancer have been comprehensively examined. In addition, the basic features, structural aspects, and biological data of analytical methods used in treatments with new-generation drugs are explained. Analytical studies carried out in the literature in recent years aim to show future developments in how these new-generation drugs are used today and to guide future studies by comprehensively examining and explaining the structure-activity relationship, mechanism of action, toxicity, and pharmacokinetic studies. Finally, in this study, the methods used in the analysis of drugs used in the treatment of ovarian cancer and the studies conducted between 2015 and 2023 were discussed in detail.

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.

Analysis of drugs seized from amnesty bins at two major United Kingdom summer music festivals using two portable gas chromatography-mass spectrometry (GC-MS) instruments.

Globally, the number of drug users and the proportion of the drug using population has increased from 210 million in 2009 to 269 million in 2019. Several studies suggest that music festival attendees are more likely to abuse illicit substances and have a high-risk profile. Consequently, it is crucial to develop robust field drug analysis methods that facilitate harm reduction and drug monitoring. The work presented in this report aimed at developing and validating qualitative analytical methods for 3,4-methylenedioxymethamphetamine, 4-bromo-2,5-dimethoxyphenethylamine (2C-B), ketamine and N-ethylpentylone on two portable gas chromatography-mass spectrometry (GC-MS) systems: Griffin G510 (Teledyne FLIR, West Lafayette, IN) and Torion T-9 (PerkinElmer, Shelton, CT). The diagnostic ability of the mobile GC-MS units was assessed on 200 samples in total, seized at two large summer music festivals in the United Kingdom. The method validation process included selectivity/specificity, limit of identification, carry-over, ruggedness/robustness, and inter- and intra-day precision (repeatability and reproducibility). The Griffin G510 demonstrated a limit of identification from 1 mg/mL for 2C-B to 0.063 mg/mL for ketamine and good ruggedness and precision results. The precision for 2C-B using the Torion T-9 was poorer than for the Griffin G510, but equivalent for the other compounds tested. Correct identifications (versus benchtop GC-MS) for the two festivals were 85%-86% and 74%-83% for the Griffin G510 and the Torion T-9, respectively. The two portable instruments were able to adequately cover current on-site drug-testing analytical gaps and proved to be a powerful addition to the on-site drug analysis techniques.

Ionic Liquids in Pharmaceutical and Biomedical Applications: A Review.

The unique properties of ionic liquids (ILs), such as structural tunability, good solubility, chemical/thermal stability, favorable biocompatibility, and simplicity of preparation, have led to a wide range of applications in the pharmaceutical and biomedical fields. ILs can not only speed up the chemical reaction process, improve the yield, and reduce environmental pollution but also improve many problems in the field of medicine, such as the poor drug solubility, product crystal instability, poor biological activity, and low drug delivery efficiency. This paper presents a systematic and concise analysis of the recent advancements and further applications of ILs in the pharmaceutical field from the aspects of drug synthesis, drug analysis, drug solubilization, and drug crystal engineering. Additionally, it explores the biomedical field, covering aspects such as drug carriers, stabilization of proteins, antimicrobials, and bioactive ionic liquids.

Headspace solid-phase microextraction - gas chromatography - mass spectrometry qualitative screening method for active compounds, adulterants and impurities in ecstasy tablets seized in Northern Santa Catarina State, Brazil.

The present work describes the development of a headspace solid-phase microextraction (HS-SPME) followed by gas chromatography - mass spectrometry (GC-MS) method for the qualitative analysis of compounds in seized ecstasy tablets that can be easily implemented in regular laboratories. HS-SPME with a DVB/CAR/PDMS 50/30 µm fiber was used to extract the ecstasy pills' components, including major and minor ones, in a single extraction/chromatographic run. For HS-SPME, the incubation time (0 min to 30 min), the extraction time (10 min to 40 min) and temperature (40 °C to 80 ºC), the buffer volume (3 mL to 8 mL), the buffer pH (6 to 9) and the NaCl concentration (0 mol/L to 6 mol/L) were evaluated using fractional factorial design. Different split ratios and detector voltages were also evaluated. The optimal compromise between sensitivity and peak resolution was found to be incubation and extraction at 65 ºC for 10 min and 25 min, respectively, 3 mL of pH 9 buffer containing 3 mol/L NaCl, using 40.0 mg of the powdered samples in a 15-mL amber glass vial, and an injection with a split ratio of 1:10 at 260 ºC for 10 min. Under optimal conditions, 44 samples from different seizures were analyzed. Seventy-five compounds were tentatively identified by the proposed method, including active substances, medicines, caffeine, safrole derivatives, synthesis intermediates and solvent residues. The number of tentatively identified compounds per sample varied from 8 to 24, with a mean of 15. Important findings in ecstasy samples, such as norcinamolaurin, α-methyl-1,3-benzodioxole-5-propanamide, α-methyl-3,4-methylenedioxyphenylpropionitrile, acetylsalicylic acid, piperonylonitrile, methyl isobutyl ketone, mesitylene, and 4-[3-(dimethylamino)propyl]- 2,6-dimethylphenol, identified with a frequency higher than 10%, are not found in the literature so far. The method precision, based on relative standard deviation of peak areas, ranged from 5% to 15%, depending on the compound. The method was shown to be simple, relatively fast, precise and a powerful tool for the identification of major and minor components in ecstasy tablets in a single analytical cycle, being useful for screening or quantitative purposes, if authentic standards are available.

Fabrication of a novel tantalum boride/vanadium carbide modified screen-printed carbon electrode for voltammetric determination of pimonidazole in bio-fluids.

For the first time, a tumour hypoxia marker detection has been developed using two-dimensional layered composite modified electrodes in biological and environmental samples. The concept of TaB2 and V4C3-based MXene composite materials is not reported hitherto using ball-milling and thermal methods and it remains the potentiality of the present work. The successful formation is confirmed through various characterisation techniques like X-ray crystallography, scanning electron microscopy photoelectron, and impedance spectroscopy. A reliable and repeatable electrochemical sensor based on TaB2@V4C3/SPCE was developed for quick and extremely sensitive detection of pimonidazole by various electroanalytical methods. It has been shown that the modified electrode intensifies the reduction peak current and causes a decrease in the potential for reduction, in comparison with the bare electrode. The proposed sensor for pimonidazole reduction has strong electrocatalytic activity and high sensitivity, as demonstrated by the cyclic voltammetry approach. Under the optimal experimental circumstances, differential pulse voltammetry techniques were utilised for generating the wide linear range (0.02 to 928.51 µM) with a detection limit of 0.0072 µM. The resultant data demonstrates that TaB2@V4C3/SPCE nano-sensor exhibits excellent stability, reliability, and repeatability in the determination of pimonidazole. Additionally, the suggested sensor was successfully used to determine the presence of pimonidazole in several real samples, such as human blood serum, urine, water, and drugs.

Results of the first international quality control programme for oral targeted oncolytics.

AIMS: With the rising number of oral targeted oncolytics and growing awareness of the benefits of therapeutic drug monitoring (TDM) within the field of oncology, it is expected that the requests for quantifying concentrations of these drugs will increase. It is important to (cross-)validate available assays and ensure its quality, as results may lead to altered dosing recommendations. Therefore, we aimed to evaluate the performance of laboratories measuring concentrations of targeted oral oncolytics in a one-time international quality control (QC) programme. METHODS: Participating laboratories received a set of plasma samples containing low, medium and high concentrations of imatinib, sunitinib, desethylsunitinib, pazopanib, cabozantinib, olaparib, enzalutamide, desmethylenzalutamide and abiraterone, with the request to report their results back within five weeks after shipment. Accuracy was defined acceptable if measurements where within 85%-115% from the weighed-in reference concentrations. Besides descriptive statistics, an exploratory ANOVA was performed. RESULTS: Seventeen laboratories from six countries reported 243 results. Overall, 80.7% of all measurements were within the predefined range of acceptable accuracy. Laboratories performed best in quantifying imatinib and poorest in quantifying desethylsunitinib (median absolute inaccuracy respectively 4.0% (interquartile range (IQR) 1.8%-6.5%) and 15.5% (IQR 8.8%-34.9%)). The poorest performance of desethylsunitinib might be caused by using the stable-isotope-labelled sunitinib instead of desethylsunitinib as an internal standard, or due to the light-induced cis(Z)/trans(E) isomerization of (desethyl)sunitinib. Overall, drug substance and performing laboratory seemed to influence the absolute inaccuracy (F = 16.4; p < 0.001 and F = 35.5; p < 0.001, respectively). CONCLUSION: Considering this is the first evaluation of an international QC programme for oral targeted oncolytics, an impressive high percentage of measurements were within the predefined range of accuracy. Cross-validation of assays that are used for dose optimization of oncolytics will secure the performance and will protect patients from incorrect advices.

Application of a Modified 3D-PCSI-MS Ion Source to On-Site, Trace Evidence Processing via Integrated Vacuum Collection.

Trace evidence, including hair, fibers, soil/dust, and gunshot residue (GSR), can be recovered from a crime scene to help identify or associate a suspect with illegal activities via physical, chemical, and biological testing. Vacuum collection is one technique that is employed in recovering such trace evidence but is often done so in a targeted manner, leaving other complementary, chemical-specific information unexamined. Here, we describe a modified 3D-printed cone spray ionization (3D-PCSI) source with integrated vacuum collection for on-site, forensic evidence screening, allowing the processing of targeted physical traces and nontargeted chemical species alike. The reported form factor allows sample collection, onboard extraction, filtration, and spray-based ionization in a singular vessel with minimal handling of evidence by the operator. Utilizing authentic forensic evidence types and portable MS instrumentation, this new method was characterized through systematic studies that replicate CSI applications. Reliability in the form of false positive/negative response rates was determined from a modest, user-blinded data set, and other attributes, such as collection efficacy and detection limit, were examined.

Preparation of chiral monoliths with new modulation of the monolith surface chemistry for the enantioseparation of chiral drugs by nano-liquid chromatography.

Here, we report the preparation and application of two new chiral monoliths for the enantioseparation of chiral drugs in nano-LC. Using 3­chloro-2-hydroxypropylmethacrylate (HPMA-Cl, 2) as a precursor monomer, two different chiral monomers namely, Nα-Boc-Lys-HPMA (3A) and Nα-Fmoc-Lys-HPMA (3B) were synthesized and used for the preparation of chiral polymer monoliths. The first monolithic column (referred to as monolith I) was prepared by an in-situ polymerization of Nα-Boc-Lys-HPMA as the chiral monomer and ethylene dimethacrylate while the second monolithic column (referred to as monolith II) was prepared by an in-situ polymerization of Nα-Fmoc-Lys-HPMA as the chiral monomer and ethylene dimethacrylate as the crosslinker. Methanol and 1-propanol were used as the porogenic solvents. The prepared chiral monoliths were investigated for the enantioseparation of chiral drugs, including ß-blockers (e.g., atenolol, propranolol, metoprolol) and anti-inflammatory drugs (e.g., ketoprofen, ibuprofen, flurbiprofen, naproxen, etodolac). The enantioseparation could be achieved via the formation of π-π interactions on the aromate-rich and aromate-poor chiral molecules while enantioseparation mechanism of chiral drugs included mostly π-π interactions and hydrogen bonding. Monolith II showed better enantioselectivity than Monolith I and the resolution values up to 2.12 were successfully achieved.

Application progress on in vivo drug analysis technique in clinical pharmacy / 药学实践杂志

Objective To explore the progress on the application of in vivo drug analysis techniques in clinical pharmacy work. Methods Relevant literature was reviewed to provide an overview of the characteristics of clinical samples, common in vivo drug analysis methods used in the clinic, the application and existing problems of in vivo drug analysis in clinical pharmacy. Results and Conclusion In recent years, with the increasing demand for individualized and precise treatment in clinical practice and the continuous development of analytical techniques, in vivo drug analysis techniques have been widely used in clinical pharmacy work, which have become one of the important auxiliary techniques to promote rational clinical drug use, improve individualized treatment and reduce the occurrence of adverse reactions. However, in the actual application, there were still problems such as the invasive blood sampling that hinders sampling, the weak ability to interpret drug monitoring results and clinical testing methods that still need to be improved. These problems should be taken seriously and continuously improved and solved in the subsequent research and application.

Quality control of psychoactive substances in human breastmilk samples from a human milk bank by disposable pipette extraction-gas chromatography-mass spectrometry.

The lack of data regarding infant exposure to drugs of abuse consumed by lactating mothers has become a major health concern. Investigating psychoactive substances and their metabolites in breastmilk is an analytical approach to estimate the rate at which drugs of abuse are excreted and how much infants are exposed to them. In this study, we have developed and validated a GC-MS method using disposable pipette tips for simultaneously extracting ten analytes from breastmilk samples obtained from a milk bank in the city of Ribeirão Preto, Brazil. All the 67 analyzed samples tested negative for all the analytes. This is the first study that has applied disposable pipette extraction to analyze drugs of abuse in breastmilk samples.

Breastfeeding, the most effective single strategy to reduce child mortality, provides numerous benefits for both the mother and the infant. The mother's consumption habits during breastfeeding strongly influence breastmilk quality and the newborn's nutrition. Given that drugs of abuse negatively affect both the mother's and the infant's health, analyzing breastmilk samples helps to estimate infant exposure to these drugs and to evaluate how severe this public health issue is. We have developed a new method to monitor ten substances in breastmilk, to improve our understanding of this issue in Brazil. None of the substances were detected in the few samples obtained from a milk bank, which showed that this organization successfully analyzes the donor's profile and conducts effective anamnesis. Future analysis of a larger number of samples and hence more data could help to describe the current scenario in more detail.

Application of gas chromatography in the analysis of phytocannabinoids: An update (2020-2023).

INTRODUCTION: Cannabinoids are a group of compounds that bind to cannabinoid receptors. They possess pharmacological properties like that of the plant Cannabis sativa. Gas chromatography (GC) is one of the popular chromatographic techniques that has been routinely used in the analysis of cannabinoids in different matrices. OBJECTIVE: The article aims to review the literature on the application of GC-based analytical methods for the analysis of phytocannabinoids published during the period from January 2020 to August 2023. METHODOLOGY: A thorough literature search was conducted using different databases, like Web of Knowledge, PubMed, Google Scholar, and other relevant published materials including published books. The keywords used, in various combinations, with cannabinoids being present in all combinations, in the search were cannabinoids, Cannabis sativa, marijuana, analysis, GC, quantitative, qualitative, and quality control. From the search results, only the publications that incorporate the GC analysis of phytocannabinoids were reviewed, and papers on synthetic cannabinoids were excluded. RESULTS: Since the publication of the review article on GC analysis of phytocannabinoids in early 2020, several GC-based methods for the analysis of phytocannabinoids have appeared in the literature. While simple 1D GC-mass spectrometry (MS) and GC-flame ionisation detector (FID) methods are still quite common in phytocannabinoids analysis, 2D GC-MS and GC-MS/MS are increasingly becoming popular, as these techniques offer more useful data for identification and quantification of phytocannabinoids in various matrices. The use of automation in sample preparation and the utilisation of mathematical and computational models for optimisation of different protocols have become a norm in phytocannabinoids analysis. Pre-analyses have been found to incorporate different derivatisation techniques and environmentally friendly extraction protocols. CONCLUSIONS: GC-based analysis of phytocannabinoids, especially using GC-MS, remains one of the most preferred methods for the analysis of these compounds. New derivatisation methods, ionisation techniques, mathematical models, and computational approaches for method optimisation have been introduced.

Biomass-Derived Core-Shell Carbon Dots with Embedded Tripodal Receptors for the Selective Recognition of Mefenamic Acid in Pharmaceutical Formulations and Urine.

A tripodal amine (TPA) with -OH, N, and S donors is synthesized to functionalize a core-shell carbon dot composite (FCDs@SiO2-TPA) for sensing application. The TPA is characterized by spectroscopic and spectrometric techniques, and the composite is characterized by Fourier transform infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), Brunauer-Emmett-Teller (BET), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy-dispersive X-ray spectra (EDS) techniques. The composite has the ability to recognize mefenamic acid (MFA) selectively even in the presence of other drugs like ibuprofen sodium, acetylsalicylic acid, naproxen sodium, diclofenac sodium, and ketoprofen. It can also be used for the quantification of MFA by recording the emission quenching response of the sample at λexc. = 350 nm and λems. = 460 nm (linear range = 1-8 µM and LOD = 197 nM). The density functional theory calculations and 1H NMR titration suggest quenching of the emission signal due to photoinduced electron transfer via hydrogen bonding between the probe and MFA. The composite FCDs@SiO2-TPA has been demonstrated as a reliable and cost-effective sensing probe for the detection of MFA in pharmaceutical formulations, water samples, and cow urine samples.