Liquid Chromatography Quadrupole Time-of-flight Mass Spectrometry Research Articles

Alleviating Continuous Cropping Obstacles in Celery Using Engineered Biochar: Insights into Chemical and Microbiological Aspects

In the pursuit of environmental sustainability and food security, biochar has emerged as a promising soil conditioner to mitigate continuous cropping obstacles (CCOs). This study explored the use of engineered biochar (WP400) with high adsorption capacity for phenolic acids in celery cultivation. Using liquid chromatography quadrupole time-of-flight mass spectrometry (LC-QTOF/MS) for both target and suspect analyses, along with Biolog EcoPlate™ to track the functional diversity of soil bacteria, the study examined chemical and microbiological interactions at varying WP400 application rates. WP400 enhanced celery growth, reduced disease severity, and adsorbed p-coumaric acid (COU), a potential autotoxin. Additionally, other potential allelochemicals, predominantly fatty acid-related, were identified, suggesting a broader role for fatty acids in allelopathy. WP400 also influenced soil bacterial carbon utilization and altered microbial communities. However, higher WP400 doses (0.8% w/w) may not be beneficial for celery growth and reduced bacterial metabolic potential, indicating limitations to its effectiveness. Proper application of WP400 provides a sustainable solution for alleviating continuous cropping issues, promoting both environmental sustainability and agricultural development.

Activity of Bambara Groundnut Seed Coat Extract Against Shewanella Species: Efficacy and Mechanisms of Action.

The Bambara groundnut is the indigenous legume in the southern part of Thailand. It contains a seed coat rich in polyphenols, which can serve as natural antimicrobial agents. The extracts from red and white seed coats of Bambara groundnuts, namely RSC and WSC, respectively, were prepared using an ultrasound-assisted extraction process. The extraction yield, total phenolic content (TPC), and antimicrobial activity of both extracts were examined. The RSC extract demonstrated a significantly higher extraction yield (8.35%) than WSC extract (2.34%) (p < 0.05). Furthermore, the TPC of RSC extract (420.98 ± 0.27 mg of gallic acid/g dry extract) was higher than that of WSC extract (28.29 ± 0.91 mg of gallic acid/g dry extract). The RSC extract exhibited stronger inhibition against Shewanella putrefaciens and S. algae than its WSC counterpart. Liquid chromatography quadrupole time-of-flight mass spectrometry (LC-Q-TOF/MS) analysis indicated that the RSC extract was rich in flavonoids and polyphenols, while the WSC extract contained more triterpenoid saponins. Time-kill kinetics showed that the RSC extract reduced bacterial loads in a dose-dependent manner. Scanning electron microscopic images revealed that drastic bacterial cell membrane damage with a rough surface and the deformation of cells was caused by the extract. Furthermore, confocal laser scanning microscopic (CLSM) images confirmed the inhibition of S. algae biofilm formation by RSC extract. RSC extract also suppressed bacterial motility, induced protein leakage, and reduced extracellular protease activity, thus highlighting its potent bactericidal effects. These findings suggested that the RSC extract rich in phenolic compounds could serve as an antimicrobial agent and hold promise as a natural preservative for perishable foods, especially seafoods.

A modified QuEChERS method for the generic and rapid determination of pesticides and mycotoxins in raw coffee beans by liquid chromatography-quadrupole-time-of-flight mass spectrometry

In this work, a simple, high-throughput, and sensitive analytical method for simultaneously determining 270 pesticides and 13 mycotoxins from different chemical classes in raw coffee beans was developed. The modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) process mainly involved the effects of hydration volume, extraction solvent, extraction salt, and the type and amount of adsorbent used for sample extraction and purification. The samples were detected by liquid chromatography-quadrupole-time-of-flight mass spectrometry (LC-Q-TOF/MS) with a self-built database. The method effectively reduced matrix effects and the 283 compounds showed good linearity in their respective linear ranges (R2> 0.99). The screening detection limits (SDL) of the method were in the range of 0.1–20 μg/kg, and the limits of quantification (LOQ) were in the range of 0.2–20 μg/kg. The average recoveries of the 283 compounds at three spiked levels ranged from 72.1 % to 114.9 %, with intra-day and inter-day relative standard deviations less than 9.8 % and 17.1 %, respectively. The recoveries of all analytes ranged from 70.0 % to 120.0 % at three spiked levels (1×LOQ, 2×LOQ, and 10×LOQ), with relative standard deviations less than 20.0 %. The results were satisfactory according to the SANTE/11312/2021 guidelines. The method successfully analyzed 34 batches of actual samples, with concentrations ranging from 0.1 to 61.9 μg/kg for pesticides and 2.3–43.0 μg/kg for mycotoxins. This method provides a powerful tool for monitoring organic contaminants in raw coffee beans.

Multi-residue analytical method development and dietary exposure risk assessment of 345 pesticides in mango by LC-Q-TOF/MS

Mango is attracting increasing global attention for its superior flavor and nutritional benefits. However, the use of pesticides has resulted in a threat to its quality, safety, and human health due to their inevitable residue. There is an urgent need for advanced technologies that can efficiently and sensitively analyze a wide range of pesticides. In this study, a high-throughput screening and quantification method for 345 pesticides in mango was established by applying a modified QuEChERS method combined with liquid chromatography-quadrupole-time-of-flight mass spectrometry (LC-Q-TOF/MS). A response surface methodology (RSM) optimized the critical parameters for extracting various pesticides in 1% acetic acid-acetonitrile (v/v) using MgSO4, PSA, C18, and GCB as the adsorbents. The proposed method was successfully validated and applied to the quantitative detection of pesticide residues in 73 mango samples from Hainan. The study found pesticide residues in 95.9% of mango samples, of which 3 samples had residue concentrations in excess of the Chinese maximum residue limit. A total of 24 pesticides were detected, with detection percentages ranging from 1.4% (Thiabendazole) to 41.1% (Pyraclostrobin). Considering the possible health risks related to pesticide residues, risk assessment of human exposure to pesticides via intake of mango was evaluated. The acute and chronic dietary exposure risks related to pesticide residues in mango were accepted. In conclusion, this study provides a powerful platform for monitoring multiple pesticides in mango. First, it can promote the rational use of pesticides, and second, it can help consumers to assess the risk of dietary exposure to pesticide residues.

Comprehensive analysis of respiratory pharmaceuticals in dietary supplements using advanced chromatographic techniques

Recently, the number of people suffering from respiratory symptoms has continued to increase because of COVID-19 and particulate contamination. Accordingly, the demand for respiratory-related dietary supplements is increasing. Over the past few years, dietary supplements adulterated with pharmaceutical drugs have continued to appear, increasing the risk of side effects; thus, preventive measures are needed. In this study, we developed a simultaneous analysis method for 11 respiratory-related pharmaceutical compounds using ultra-performance liquid chromatography with a photodiode array (UPLC-PDA). The sample preparation method was optimized by comparing filtration and two clean-up methods (QuEChERS), for solid and liquid formulations, and the optimal analytical conditions were established by comparing various analysis parameters. Concerning method validation, all parameters meet International Council for Harmonisation guidelines. Subsequently, 54 types of dietary supplements promoting relief of respiratory-related symptoms were purchased online and analyzed using UPLC-PDA. As a result, theobromine, azelastine, and dexamethasone were detected in three products. In addition, the detected compounds were confirmed by comparing fragmentation patterns using liquid chromatography quadrupole time-of-flight mass spectrometry (LC-QTOF/MS). This study will contribute to preemptively blocking dietary supplements adulterated with respiratory-related drugs from entering the market and can be used as a reference for future research.

Identification of fentanyl analogs and potential biomarkers in urine using liquid chromatography-tandem mass spectrometry (LC-MS/MS) and liquid chromatography-quadrupole/time of flight mass spectrometry (LC-Q/TOF-MS)

Novel synthetic opioids are a class of drugs abused for their potent analgesic effect and are responsible for many fatal intoxications, particularly within the United States. A targeted assay was developed and validated using LC-MS/MS, capable of identifying nineteen fentalogs. Solid phase extraction was used to isolate analytes of interest from urine. Limits of detection ranged from 0.05 to 0.1 ng/mL and the limit of quantitation was 0.5 ng/mL. Extraction efficiencies using the optimized procedure were 77–88 % for all targeted species. Bias, precision, matrix effects and interferences were within acceptable thresholds for all analytes. The validated assay was used to identify analytes of interest from thirty-seven individuals that had used fentanyl and related substances. In addition to quantitative analyses, a non-targeted liquid chromatography quadrupole time-of-flight mass spectrometry (LC-Q/TOF-MS) assay was also used to identify additional substances and potential biomarkers. Additional N-oxide and N-dealkylated species were identified using this approach, and the potential for biomarker use is presented, given the stability of some analytes within this class.

Step-By-Step Procedure to Identify Previously Unknown Compounds by LC-QTOF-MS Exemplified by an Intoxication With the Methaqualone Analog SL-164.

In September 2019, a 22-year-old man with a history of drug abuse presented to the hospital with altered mental status. Due to a suspected drug overdose, a blood sample taken on admission and a urine sample collected 30 h thereafter were submitted to our laboratory to test for illegal drugs, pharmaceutical substances, and designer drugs. During the routine toxicological analysis of the serum sample, morphine and phenobarbital were identified by liquid chromatography-quadrupole-time-of-flight mass spectrometry (LC-QTOF-MS). Additionally, two compounds showing identical accurate masses and isotope ratios as the designer benzodiazepine diclazepam and the benzodiazepine lormetazepam were found. However, retention times differed significantly from the expected values, and the acquired MS/MS spectra did not match the library entries of the two compounds, indicating the presence of two previously unknown substances. After further investigation, SL-164 (5-chloro-3-(4-chloro-2-methylphenyl)-2-methyl-4(3H)-quinazolinone), a methaqualone analog, which has recently emerged on the research chemical market, and its hydroxy metabolite were tentatively identified by accurate mass, isotope matching, and plausible fragmentation. However, for unequivocal confirmation and quantification, a reference standard is required. As no reference material was available by the end of 2019, SL-164 was obtained from an online shop, and its identity and purity (97.8%) were confirmed by nuclear magnetic resonance spectroscopy. The subsequent quantitative analysis revealed a concentration of 390 ng/mL SL-164 in serum. In the urine sample, the parent compound was not detected, but three suspected monohydroxylated metabolites were found. This example shows that LC-QTOF-MS is a powerful approach for the (tentative) identification of unknown compounds in biological matrices.

Phenolic Constituents, Photoprotective Effect, and Antioxidant Capacities of Achillea ligustica All.

The present investigation was performed to figure out the chemical constituents and biological potential of polar extracts (AcOEt and BuOH) from Achillea ligustica, a medicinal species of the Asteraceae family. Liquid chromatography quadrupole time-of-flight mass spectrometry (LC-Q-TOF-MS) was utilized to conduct a preliminary analysis of the phytochemical profiles of the AcOEt and BuOH extracts. The analysis revealed the existence of twenty compounds in the AcOEt extract and twenty-two in the BuOH extract, classified into various types of secondary metabolites. Subsequently, the exudate from the plant yielded five flavonoids, including two 6-methoxyflavonols identified for the first time in this genus. The isolation of compounds from AcOEt and BuOH extracts was achieved through the combined use of column chromatography (silica gel and Sephadex LH-20) and preparative TLC chromatography. The structures have been elucidated using 1D and 2D NMR spectroscopy, alongside comparisons with research data. Our study measured the total phenolic and flavonoid contents and carried out a comprehensive range of antioxidant tests using DPPH, GOR, CUPRAC, reducing power, and O-phenanthroline assays. Both extracts exhibited considerable antioxidant potential and contained high levels of phenolic and flavonoid compounds. The photoprotective effect of the AcOEt and BuOH extracts was evaluated in vitro by measuring the sun protection factor. Both extracts exhibited a high capacity for UV radiation absorption. Consequently, this plant presents an intriguing prospect for future research focused on incorporating it into photoprotective cosmetic products and pharmaceutical formulations.

Enhancing chemotherapeutic efficacy: Niosome-encapsulated Dox-Cis with MUC-1 aptamer.

Cancer remains a formidable global health challenge, currently affecting nearly 20 million individuals worldwide. Due to the absence of universally effective treatments, ongoing research explores diverse strategies to combat this disease. Recent efforts have concentrated on developing combined drug regimens and targeted therapeutic approaches. This study aimed to investigate the anticancer efficacy of a conjugated drug system, consisting of doxorubicin and cisplatin (Dox-Cis), encapsulated within niosomes and modified with MUC-1 aptamers to enhance biocompatibility and target specific cancer cells. The chemical structure of the Dox-Cis conjugate was characterized using Fourier Transform Infrared Spectroscopy (FTIR) and Liquid Chromatography Quadrupole Time-of-Flight Mass Spectrometry (LC-Q-TOF/MS). The zeta potential and morphological parameters of the niosomal vesicles were determined through Dynamic Light Scattering (DLS) and Transmission Electron Microscopy (TEM). In vitro assessments of cell viability and apoptosis were conducted on MUC-1 positive HeLa cells and MUC-1 negative U87 cells. The findings confirmed the successful conjugation of Dox and Cis within the niosomes. The Nio/Dox-Cis/MUC-1 formulation demonstrated enhanced efficacy compared to the individual drugs and their unencapsulated combination in both cell lines. Notably, the Nio/Dox-Cis/MUC-1 formulation exhibited greater effectiveness on HeLa cells (38.503 ± 1.407) than on U87 cells (46.653 ± 1.297). The study underscores the potential of the Dox-Cis conjugate as a promising strategy for cancer treatment, particularly through platforms that facilitate targeted drug delivery to cancer cells. This targeted approach could lead to more effective and personalized cancer therapies.

In vitro metabolism study of ADB-P-5Br-INACA and ADB-4en-P-5Br-INACA using human hepatocytes, liver microsomes, and in-house synthesized references.

Synthetic cannabinoids (SCs) remain a major public health concern, as they continuously are linked to severe intoxications and drug-related deaths worldwide. As new SCs continue to emerge on the illicit drug market, an understanding of SC metabolism is needed to identify formed metabolites that may serve as biomarkers in forensic toxicology screening and for understanding the pharmacokinetics of the drugs. In this work, the metabolism of ADB-4en-P-5Br-INACA and ADB-P-5Br-INACA ((S)-N-(1-amino-3,3-dimethyl-1-oxobutan-2-yl)-5-bromo-1-(pent-4-en-1-yl)-1H-indazole-3-carboxamide, (S)-N-(1-amino-3,3-dimethyl-1-oxobutan-2-yl)-5-bromo-1-pentyl-1H-indazole-3-carboxamide respectively) were investigated using human hepatocytes in vitro and in-house synthesized references. Both SCs were incubated with pooled human hepatocytes over 3h, with the aim to identify unique and abundant metabolites using liquid chromatography-quadrupole time-of-flight mass spectrometry (LC-QTOF-MS). In total nine metabolites were identified for ADB-4en-P-5Br-INACA and 10 metabolites for ADB-P-5Br-INACA. The observed biotransformations included dihydrodiol formation, terminal amide hydrolysis, hydroxylation, dehydrogenation, carbonyl formation, glucuronidation, and combinations thereof. The major metabolites were confirmed by in-house synthesized references. Recommended biomarkers for ADB-P-5Br-INACA and ADB-4en-P-5Br-INACA are the terminal hydroxy and dihydrodiol metabolite respectively.

Serum lipidomic profiling of dairy calves fed milk replacers containing animal or vegetable fats

Vegetable fat blends are commonly used as fat sources in milk replacers (MR) for calves, but their composition differs considerably from that of bovine milk fat. The aim of this study was to investigate the serum lipid profile of preweaning calves fed twice-daily MR containing 30% fat (% DM). Upon arrival, 30 male Holstein-Friesian calves (BW = 45.6 ± 4.0 kg, age = 2.29 ± 0.8 d) were randomly assigned to 2 experimental diets (n = 15 per treatment): one MR was derived from either vegetable fats (VG; 65% rapeseed and 35% coconut fats) or animal fats (AN; 65% packers lard and 35% dairy cream). The 2 MR formulas contained 30% fat, 24% CP, and 36% lactose. Calves were housed indoors in individual pens with ad libitum access to chopped straw and water. Daily milk allowances were 6.0 L from d 1 to 5, 7.0 L from d 6 to 9, and 8.0 L from d 10 to 35, divided into 2 equal meals and prepared at 13.5% solids. An untargeted liquid chromatography-quadrupole time-of-flight mass spectrometry (LC-QTOF-MS) method was employed to analyze the lipid profiles in the serum of calves sampled from the jugular vein at 35 d of age. In total, 594 lipids were characterized, comprising 25 different lipid classes. Principal component analysis (PCA) showed significant separation between VG and AN, indicating different lipid profiles in the serum. An orthogonal partial least squares discriminant analysis (OPLS-DA) classification model was used to further validate the distinction between the 2 treatment groups. The model exhibited a robust class separation and high predictive accuracy. Using a volcano plot (fold change threshold ≥1.5 and false discovery rate ≤0.05), it was observed that calves fed AN had higher levels of 39 lipid species in serum than calves fed VG, whereas 171 lipid species were lower in the AN group. Lipid classes, such as phosphatidylcholine (PC), phosphatidylethanolamine (PE), sphingomyelin (SM), triglycerides (TG), lysophosphatidylcholine (LPC), and lysophosphatidylethanolamine (LPE), were different. In particular, PC and PE were observed at lower levels in calves fed AN, possibly indicating shifts in cell membrane characteristics, intracellular signaling, and liver functions. In addition, a decrease in certain triglyceride (TG) species was observed in calves fed AN, including a decrease in TG species such as TG 36:0 and TG 38:0, possibly related to variations in the content of certain fatty acids within the AN MR, such as C10:0, C12:0, C14:0, and C18:0, compared with the VG MR. Calves fed AN had lower levels of LPC and LPE, and lysophosphatidylinositol, SM, and phosphatidylinositol species than calves fed VG, suggesting shifts in lipoprotein and lipid metabolic pathways. In conclusion, these results deepen the understanding of how lipid sources in MR can modulate the serum lipidome profiles of dairy calves.

Temperature and pH-dependent stability of fentanyl analogs: Degradation pathways and potential biomarkers.

The collection, storage, and transport of samples prior to and during analysis is of utmost importance, especially for highly potent analogs that may not be present in high concentrations and are susceptible to pH or thermally mediated degradation. An accelerated stability study was performed on 17 fentanyl analogs (fentalogs) over a wide range of pH (2-10) and temperature (20-60°C) conditions over 24 h. Dilute aqueous systems were used to investigate temperature and pH-dependent kinetics using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Liquid chromatography-quadrupole/time-of-flight-mass spectrometry (LC-Q/TOF-MS) was used for structural elucidation of degradants. With the exception of remifentanil, all fentalogs evaluated were stable at pH 6 or lower. Fentalogs were generally unstable in strongly alkaline environments and at elevated temperatures. Remifentanil was the least stable drug and N-dealkylated fentalogs were the most stable. Fentanyl degraded to acetylfentanyl, norfentanyl, fentanyl N-oxide, and 1-phenethylpyridinium salt (1-PEP). A total of 26 unique breakdown products were observed for 15 of the fentanyl derivatives studied. Common degradation pathways involved N-dealkylation, oxidation of the piperidine nitrogen, and β-elimination of N-phenylpropanamide followed by oxidation/dehydration of the piperidine ring. Ester and amide hydrolysis, demethylation at the propanamide, and O-demethylation were observed for selected fentalogs only. The potential for analyte loss should be considered during the pre-analytical phase (i.e., shipping and transport) where environmental conditions may not be controlled, as well as during the analysis itself.

Urine as a Biobased Fertilizer: The Netherlands as Case Study

AbstractHumankind has grown increasingly dependent on mineral fertilizer to feed a growing world population. However, nutrients are rarely recovered and recycled after consumption, leading to environmental waste issues now and potential supply issues in the future. Urine is rich in these nutrients and is therefore a prime candidate as a precursor for biobased fertilizers. This work presents a case study to remove potentially present contaminants from human urine using activated carbon adsorbents to adhere to Dutch fertilizer legislation. In the urine, three pharmaceuticals were identified by target analysis and 11 other contaminants by suspect screening using liquid chromatography quadrupole time-of-flight mass spectrometry (LC-QTOF/MS). These were successfully removed by treatments with both granulated and powdered activated carbon, albeit with a loss of 16–17% and 2–4% of dissolved nutrients, respectively. Further screening of inorganic contaminants and persistent organic pollutants by inductively coupled plasma mass spectrometry (ICP-MS) and gas chromatography quadrupole-Orbitrap mass spectrometry (GC-Q-Orbitrap/MS) showed that all prerequisites for fertilizer status are met, paving the way for its future legal use as a biobased fertilizer in the Netherlands.

LC-MS and GC–MS based metabolomics analysis revealed the impact of tea trichomes on the chemical and flavor characteristics of white tea

To explore the influence of tea trichomes on the quality of white tea, liquid chromatography quadrupole time-of-flight mass spectrometry (LC-Q-TOF-MS), and headspace solid phase microextraction gas chromatography-mass spectrometry (HS-SPME-GC–MS) were used to identify non-volatile and volatile compounds white tea without trichomes (WTwt) and pure trichomes (PT). It was found that the bitter and astringent compounds, caffeine (CAF), epigallocatechin gallate (EGCG), epicatechin gallate (ECG) and flavonol glycosides, were mainly enriched in the WTwt, with 16.3-fold, 47.1-fold and 28.7-fold decrease in CAF and EGCG and ECG, respectively, and the content of these compounds in PT were lower than the taste thresholds. In PT, kaempferol-3-O-(p-coumaroyl)-glucoside and kaempferol-3-O-(di-p-coumaroyl)-glucoside were non-volatile marker compounds, and decanal was significant aroma contributor with rOAV = 250.86. Moreover, the compounds in trichomes mainly contributed to the fruity and floral aroma of white tea, among which benzyl alcohol, (E)-geranylacetone, decanal, dodecanal and 6-methyl-5-hepten-2-one were the crucial aroma components, which were 2.1, 1.7, 1.8, 1.4 and 2.2 times as much as the WTwt in the PT, respectively. In conclusion, trichomes can improve the quality of white tea by reducing the bitterness and astringency, increasing the umami, as well as enhancing the fruity and floral aromas.

Identification of Anastatica hierochuntica L. Methanolic-Leaf-Extract-Derived Metabolites Exhibiting Xanthine Oxidase Inhibitory Activities: In Vitro and In Silico Approaches.

There is a growing interest in the discovery of novel xanthine oxidase inhibitors for gout prevention and treatment with fewer side effects. This study aimed to identify the xanthine oxidase (XO) inhibitory potential and drug-likeness of the metabolites present in the methanolic leaf extract of Anastatica (A.) hierochuntica L. using in vitro and in silico models. The extract-derived metabolites were identified by liquid-chromatography-quadrupole-time-of-flight-mass-spectrometry (LC-QTOF-MS). Molecular docking predicted the XO inhibitory activity of the identified metabolites and validated the best scored in vitro XO inhibitory activities for experimental verification, as well as predictions of their anticancer, pharmacokinetic, and toxic properties; oral bioavailability; and endocrine disruption using SwissADMET, PASS, ProTox-II, and Endocrine Disruptome web servers. A total of 12 metabolites, with a majority of flavonoids, were identified. Rutin, quercetin, and luteolin flavonoids demonstrated the highest ranked docking scores of -12.39, -11.15, and -10.43, respectively, while the half-maximal inhibitory concentration (IC50) values of these metabolites against XO activity were 11.35 µM, 11.1 µM, and 21.58 µM, respectively. In addition, SwissADMET generated data related to the physicochemical properties and drug-likeness of the metabolites. Similarly, the PASS, ProTox-II, and Endocrine Disruptome prediction models stated the safe and potential use of these natural compounds. However, in vivo studies are necessary to support the development of the prominent and promising therapeutic use of A. hierochuntica methanolic-leaf-extract-derived metabolites as XO inhibitors for the prevention and treatment of hyperuricemic and gout patients. Furthermore, the predicted findings of the present study open a new paradigm for these extract-derived metabolites by revealing novel oncogenic targets for the potential treatment of human malignancies.

Comprehensive Quality Assessment of Brassica napus L. Seeds via HPTLC, LC-QToF, and Anatomical Investigation.

The Brassicaceae family, commonly referred to as cruciferous plants, is globally cultivated and consumed, with the Brassica genus being particularly renowned for its functional components. These vegetables are rich sources of nutrients and health-promoting phytochemicals, garnering increased attention in recent years. This study presents a comprehensive microscopic, chromatographic, and spectroscopic characterization of Brassica napus L. seeds from Kazakhstan aimed at elucidating their morphological features and chemical composition. Microscopic analysis revealed distinct localization of flavonoids, total lipids, and alkaloids. High-performance thin-layer chromatography (HPTLC) analysis of seed extracts demonstrated a complex chemical profile with significant quantities of non-polar compounds in the hexane extracts. Additionally, methanolic extracts revealed the presence of diverse chemical compounds, including alkaloids, flavonoids, and glucosinolates. The chemical composition exhibited varietal differences across different Brassica species, with B. napus L. seeds showing higher concentrations of bioactive compounds. Furthermore, liquid chromatography-quadrupole time-of-flight mass spectrometry (LC-QToF-MS) analysis provided insights into the chemical composition, with sinapine isomers, feruloyl, and sinapoyl choline derivatives as major compounds in the seeds. This study contributes to a better understanding of the chemical diversity and quality control methods' approximations of B. napus L. seeds, highlighting their importance in functional food and nutraceutical applications.

Profiling of saponins in four different species of Chlorophytum by liquid chromatography quadrupole time of flight mass spectrometry

The genus Chlorophytum, rich in saponins is used in Ayurveda, an Indian alternative system of medicine. This study illustrates a comprehensive picture of saponins in four different species of Chlorophytum viz., Chlorophytum borivilianum Santapau and Fernandes, Chlorophytum glaucoides Blatt, Chlorophytum glaucum Dalz, Chlorophytum bharuchae Ansari, Sundargarh, Hemadri, from the western ghats of India. Metabolite profiling of leaves and tubers using Liquid Chromatography Quadrupole Time Of Flight Mass Spectrometry (LC-Q-TOF-MS) indicated presence of 13 saponins. C. glaucum was found to be abundant in saponins followed by C. glaucoides. Tokorogenin, diosgenin and sarsasapogenin are most abundant saponins confirmed from the leaves of C. glaucum and tubers of C. glaucoides.

Xylazine awareness, desire, use and exposure: Preliminary findings from the Rhode Island community-based drug checking cohort study

BackgroundXylazine is an ⍺2 adrenergic receptor agonist and a veterinary sedative that can cause severe health complications yet interventions to detect and treat human exposure remain underdeveloped. Community-based drug checking services (DCS) involve the testing of small amounts of drugs to increase community knowledge of unregulated supplies and decrease harms. This study characterized xylazine awareness, desire, use and exposure among people who use drugs (PWUD) in Rhode Island, US. MethodsWe analyzed data from an ongoing PWUD cohort study. In 2023, 125 PWUD were enrolled and surveyed. Using point-of-care Fourier Transform infrared spectroscopy (FTIR-S), we tested a drug sample from each participant onsite and confirmed the results offsite at a laboratory. Results were conveyed in real-time, along with harm reduction education, referrals to resources and care. ResultsVirtually all participants (99.2 %) wanted to avoid xylazine exposure. Half (51.2 %) knew what xylazine was, and a quarter (26.1 %) suspected previous exposure. Xylazine exposure was primarily surmised through sedating (45.2 %) and ulcerative (29.0 %) effects. Only 8.8 % of participants submitted a sample that they expected to contain xylazine. Xylazine was detected in 14.5 % of samples using FTIR-S and in 21.4 % of samples using a dual laboratory approach of gas chromatography mass spectrometry (GC-MS) and liquid chromatography quadrupole-time-of-flight mass spectrometry (LC-QTOF-MS). Participants thought that these xylazine-positive samples were fentanyl (78.3 %), heroin (13.0 %), or Percocet® (8.7 %). ConclusionImplementing point-of-care DCS at harm reduction organizations could be useful in rapidly increasing xylazine awareness and engaging at-risk individuals in prevention, harm reduction, treatment, and rapid care for xylazine-related wounds.

Pilot findings on the real-world performance of xylazine test strips for drug residue testing and the importance of secondary testing methods

BackgroundXylazine is a sedative found increasingly in the illicit fentanyl supply that can cause hypotension, bradycardia, necrosis and death. This pilot examined the real-world performance of BTNX xylazine test strips (XTS) in drug residue samples. MethodsThis study was nested within a drug checking service in Rhode Island. We tested unmeasured drug residue dissolved in 5mL of distilled water using XTS and Liquid Chromatography Quadrupole Time-of-Flight Mass Spectrometry (LC-QTOF-MS). Analyses compared XTS and LC-QTOF-MS results to calculate XTS detection of xylazine in residue. ResultsAmong 41 residue samples, xylazine was detected in 11% by the XTS and 44 % by the laboratory. The LC-QTOF-MS detected xylazine in 18 samples: 4 major, 9 minor, 5 trace by volume relative to the whole sample. The XTS disagreed with the LC-QTOF-MS by indicating a negative result in 77.8 % (N=14) of the samples but never indicated a positive when the LC-QTOF-MS reported xylazine’s absence. The XTS correctly detected xylazine 22 % of the time, however, this increased to 100 % of the time if xylazine was a major active component. ConclusionsIn this study, the BTNX XTS often disagreed with LC-QTOF-MS by indicating a negative result, likely due to the dilution levels used and sample composition. The XTS may not be accurate in detecting residual amounts of xylazine, especially if xylazine is not a dominant component of the tested sample. Given the novelty of BTNX’s XTS products, we recommend XTS only be used in conjunction with other advanced drug checking modalities for residue testing.

Unraveling a Historical Mystery: Identification of a Lichen Dye Source in a Fifteenth Century Medieval Tapestry

As part of a long-term campaign to document, study, and conserve the Heroes tapestries from The Cloisters collection at The Metropolitan Museum of Art, organic colorant analysis of Julius Caesar (accession number 47.101.3) was performed. Analysis with liquid chromatography–quadrupole time-of-flight mass spectrometry (LC-qToF-MS) revealed the presence of several multiply chlorinated xanthones produced only by certain species of lichen. Various lichen dye sources have been documented in the literature for centuries and are classified as either ammonia fermentation method (AFM) or boiling water method (BWM) dyes based on their method of production. However, none of these known sources produce the distinctive metabolites present in the tapestry. LC-qToF-MS was also used to compare the chemical composition of the dyes in the tapestry with that of several species of crustose lichen. Lichen metabolites, including thiophanic acid and arthothelin, were definitively identified in the tapestry based on comparison with lichen xanthone standards and a reference of Lecanora sulphurata, confirming the presence of a lichen source. This finding marks the first time that lichen xanthones have been identified in a historic object and the first evidence that BWM lichen dyes may have been used prior to the eighteenth century.