Gas Chromatography-mass Spectrometry Method Research Articles

Urinary benzyl alcohol and hippuric acid in workers exposed to benzyl alcohol during paint stripping work.

This research aimed to develop a reliable gas chromatography-mass spectrometry (GC-MS) method for detecting urinary benzyl alcohol (BeOH) concentrations and assess its suitability as a biomarker for occupational BeOH exposure. Thirteen male participants exposed to BeOH during paint stripping work provided preshift and postshift urine samples, and their personal exposure concentrations were measured. Meanwhile, a control group of 10 nonexposed workers contributed urine samples. The newly developed GC-MS method met regulatory guidelines. The personal exposure concentrations of BeOH ranged from 8.4 to 45.2mg/m3. Postshift urine samples from exposed participants showed significant BeOH and hippuric acid (HA) concentration increases compared to preshift samples (BeOH, post-/pre-shift geometric mean (GM) ratio = 7.5-7.8, p < 0.001; HA, post-/pre-shift GM ratio = 4.3-4.5, p < 0.001). These levels were considerably higher than those in postshift samples from the nonexposed control group (BeOH, exposed-/nonexposed-workers GM ratio = 14.8-19.0, p < 0.001; HA, exposed-/nonexposed-workers GM ratio = 12.1-15.3, p < 0.001), even after urine density correction. Urinary BeOH and HA can serve as potential biomarkers of occupational exposure to BeOH. More specifically, BeOH might serve as a superior biomarker than HA because it is apparently less influenced by confounding factors such as dietary intake and genetic polymorphism of low-Km aldehyde dehydrogenase (ALDH2). The findings will improve workplace safety measures and protocols, assisting healthcare professionals in diagnosing and managing exposure-related health issues, thereby potentially reducing the risk of occupational exposure to BeOH.

B-168 Development and Validation of a Quantitative Ultra-Performance Liquid Chromatography Quadrupole Time-of-Flight (UPLC-QToF) Method for Urine Organic Acid Analysis

Abstract Background Urine organic acid (UOA) analysis is essential for the diagnosis of inborn errors of metabolism (IEMs). Traditionally, UOA analysis is performed with gas chromatography-mass spectrometry (GC-MS) and requires time-consuming sample preparation steps including liquid-liquid extraction and derivatization. The rapid development of Ultra-Performance Liquid Chromatography Tandem Mass Spectrometry (UPLC-MS/MS) in the past few years provides the opportunity to perform UOA analysis with a dilute-and-shoot methodology. We describe the development and validation of a quantitative Ultra-Performance Liquid Chromatography Quadrupole Time-of-Flight (UPLC-QToF) method for UOA analysis. Methods Urine specimens were diluted to normalize creatinine concentrations to 1 mmol/L. 20 µL of urine specimen (diluted), calibrator, or quality control (QC) material was mixed with 400 µL of mobile phase A (0.05% formic acid in water) and a mixture of isotope-labeled internal standards. After centrifugation, 10 µL of the supernatant was analyzed using a Xevo G3 QTOF mass spectrometer (Waters) with a ACQUITYTM Premier HSS T3 1.8 µm VanGuardTM FIT 2.1 x 150 mm column (Waters). Data collection was performed with negative electrospray ionization (ESI) mode using the MSE method to produce fragment ions when applicable. Repeatability, reproducibility, and carryover were assessed using the QC materials. The analytical measuring range (AMR) was assessed using synthetic urine spiked with increasing concentrations of each organic acid. Accuracy was assessed by method comparison with the UOA test performed at Mayo Clinic Laboratory and by spike-recovery study using a pooled urine specimen. Matrix effect was also evaluated with matrix dilution study. Results An optimized LC method was used to enable high-resolution separation of selected UOAs (N = 29) and isomers. Total analytical time was 20 min per injection. Both linear and quadratic regressions were used to build the calibration curves. AMR and correlation coefficients of a few representative UOAs were: orotic acid (3.4 to 214.2 mmol/mol creatinine, R^2 = 0.99, linear regression); 2-methylcitric acid (4 to 189 mmol/mol creatinine, R^2 = 0.99, linear regression); 3-methylcrotonylglycine (0.3 to 18.0 mmol/mol creatinine, R^2 = 0.99, linear regression). Repeatability and reproducibility were mostly &amp;lt;=10% CV and no carryover was observed. Spike-recovery study demonstrated recoveries between 80% and 120%, and method comparison study demonstrated no discrepancies with results from Mayo Clinic Laboratory. Conclusions We have developed and validated a novel UPLC-QTOF method for UOA analysis to support the diagnosis of IEMs with acceptable analytical and clinical performances. Compared with the traditional GC-MS method, the UPLC-QTOF method requires a very small specimen volume and does not require laborious and time-consuming sample preparation steps. Continued optimization of the method will be pursued to measure more UOAs to support the diagnosis of more IEMs.

A GC-MS Method for Determination of β-Propiolactone Residues in Inactivated Covid-19 Vaccines.

β-propiolactone is a common inactivator agent used in vaccines. Due to β-propiolactone carcinogenicity, complete hydrolysis of it is necessary to prevent cytotoxicity in mammalian cells. As a result, more attention should be paid to it at the clinic, and it is important to measure its trace amounts. β-propiolactone analysis is challenging due to its instability. A simple and fast gas chromatography-mass spectrometry method was developed for quantitation of residual β-propiolactone in inactivated coronavirus disease 2019 (Covid-19) vaccines. Caprolactone was used as an internal standard in sample solutions; the analysis was performed after extraction of analyte from vaccine media by ethyl acetate. The validity of the method was studied with a linearity of r2> 0.99 over the concentration range of 0.2-20μg/mL with the limit of detection and the limit of quantification of 0.07 and 0.20μg/mL, respectively. The target analyte β-propiolactone was not detected in the samples, demonstrating the test samples were qualified. The established method can be used for quality control of inactivated Covid-19 vaccines.

The optimization and validation of a gas chromatography-mass spectrometry method to analyze the concentration of acetate, propionate and butyrate in human plasma or serum

Fermentation-derived short-chain fatty acids (SCFA)44SCFA: short-chain fatty acids. are potential mediators of the health benefits associated with dietary fiber intake. SCFA affect physiological processes locally in the gut and on distant organs via the systemic circulation. Since SCFA are used as energy source for colonocytes and substrate for the liver metabolism, their concentrations in the systemic circulation are low. Therefore, quantification of systemic SCFA requires sensitive analytical techniques. This article covers the optimization and validation of a gas chromatography-mass spectrometry method to measure systemic SCFA concentrations following derivatization with 2,4-difluoroaniline (DFA)55DFA: 2,4-difluoroaniline. and extraction in ethyl acetate. Sample preparation was optimized by varying the amount of DFA, coupling agent 1,3-dicyclohexylcarbodiimide, ethyl acetate and sodium bicarbonate, which is used to quench derivatization. In addition, evaporation of the samples using a vacuum concentrator resulted in less contamination, notably of acetate, compared to drying with N2 gas. The method showed excellent linearity with coefficient of variation (R2) > 0.99 and a good precision (relative standard deviation < 20 %) and accuracy. Finally, systemic concentrations of SCFA in human plasma samples could successfully be determined.

GC-MS validation and analysis of targeted plasma metabolites related to carbonyl stress in type 2 diabetes mellitus patients with and without acute coronary syndrome.

Methylglyoxal (MG) is responsible for advanced glycation end-product formation, the mechanisms leading to diabetes pathogenesis and complications like acute coronary syndrome (ACS). Sugar metabolites, amino acids and fatty acids are possible substrates for MG. The study aimed to measure plasma MG substrate levels using a validated gas chromatography-mass spectrometry (GC-MS) method and explore their association with ACS risk in type 2 diabetes mellitus (T2DM). The study included 150 T2DM patients with ACS as cases and 150 T2DM without ACS as controls for the analysis of glucose, fructose, ribulose, sorbitol, glycerol, pyruvate, lactate, glycine, serine, threonine, C16:0, C16:1, C18:0, C18:1, C18:2, C18:3, C20:0 and C22:6 by GC-MS. Validated GC-MS methods were accurate, precise and sensitive. Cases significantly differed in plasma MG and metabolite levels except for lactate, C16:0, C18:0, C18:2, and C18:3 levels compared with controls. On multivariable logistic regression, plasma C20:0, C18:1, glycine and glycerol levels had increased odds of ACS risk. On multivariate receiver operating characteristic analysis, a model containing plasma C20:0, C16:1, C18:1, C18:2, serine, glycerol, lactate and threonine levels had the highest area under the curve value (0.932) for ACS diagnosis. In conclusion, plasma C20:0, C16:1, C18:1, glycine, glycerol and sorbitol levels were associated with ACS risk in T2DM.

Contamination of Phthalic Acid Esters (PAEs) in Surface Sediment Samples Collected from Rao Cai River in Ha Tinh, Vietnam

In this report, the solid phase extraction technique combined with the gas chromatography-mass spectrometry method (GC-MS) was optimized to determine the contamination of nine phthalic acid esters (PAEs) in the surface sediment samples collected from Rao Cai River in Ha Tinh, Vietnam. The method detection limits (MDLs) were from 2.0 to 6.0 ng/g-dry weight (ng/g-dw). The recoveries of surrogate standards (PAE-d4) in both blank and real samples ranged from 79.6 to 94.3% (RSD &lt; 8.7%). The total concentration of PAEs in the surface sediment samples was in the range of 72.4-1390 ng/g-dw (mean/median: 561/552 ng/g-dw). Among PAEs, di-(2-ethyl)hexyl phthalate (DEHP) was detected at the highest level in all samples. In contrast, dimethyl phthalate (DMP), diethyl phthalate (DEP), and dipropyl phthalate (DPP) were found at low frequency and concentration. Moreover, the risk quotient of PAEs in sediments was estimated based on the measured concentrations. Diisobutyl phthalate (DiBP) posed a medium risk for fish.

Microbial Community Dynamics and Metabolite Changes during Wheat Starch Slurry Fermentation.

Wheat starch fermentation slurry is the main substrate for producing Ganmianpi, a traditional Chinese fermented wheat starch-based noodle. In the present work, the microbial population dynamics and metabolite changes in wheat starch fermentation slurry at different fermentation times (0, 1, 2, 3, and 4 days) were measured by using high-throughput sequencing analysis and headspace solid-phase microextraction gas chromatography-mass spectrometry (HS-SPME/GC-MS) methods. The texture and sensory properties of Ganmianpi made from fermented starch slurry are also evaluated. The results showed that Latilactobacillus curvatus and Leuconostoc citreum were the dominant bacteria in wheat starch fermentation slurry, while Saccharomyces cerevisiae and Kazachstania wufongensis were identified as the main species of fungi. With the extension of fermentation time, the reducing sugar content first increased and then decreased, when the titratable acidity content showed an increasing trend, and the nonvolatile acid was significantly higher than the volatile acid. A total of 62 volatile flavor compounds were identified, and the highest content is alcohols, followed by acids. Fermentation significantly reduced the hardness and chewiness of Ganmianpi, and increased its resilience and cohesiveness. Ganmianpi made from fermented starch slurry for two and three days showed a higher sensory score than other samples. The present study is expected to provide a theoretical basis for exploiting the strains with potential for commercial application as starter cultures and quality improvement of Ganmianpi.

The influence of cancer on the reprogramming of lipid metabolism in healthy thyroid tissues of patients with papillary thyroid carcinoma.

Over the years we observed changes in the metabolism of glucose, amino acids, fatty acids (FA) and nucleotides in cancer cells in order to maintain their viability and proliferate. Moreover, as the latest data show, cancer also forces a complete change in the behavior of other tissues. For instance, fat-filled adipocytes are often found in the vicinity of invasive solid human tumors. We investigated the effects of papillary thyroid carcinoma (PTC) on the lipid metabolism of healthy tissue distant from the tumor. Thyroid tissue was collected from female patients immediately after surgical removal of the entire thyroid gland. Blood samples were collected from PTC patients and healthy volunteers. Real-time PCR assays were performed to analyze the expression of lipogenic genes and a broad panel of FA was determined using the gas chromatography-mass spectrometry method. The concentration of lipids was higher in paratumor tissue than in healthy thyroid tissue (p = 0.005). The lipogenic genes tested were significantly increased in paratumor tissue compared to healthy tissue, especially enzymes related to the synthesis of very long-chain saturated and polyunsaturated FAs (VLCSFAs and PUFAs, respectively) (p < 0.001). The FA profile also showed increased levels of C22-C26, VLCSFAs and almost all PUFAs in paratumor tissue (p < 0.05). Our study suggests that a restructuring of lipid metabolism occurs in the adjacent healthy thyroid gland and that the metabolism of VLCSFAs and PUFAs is higher in the paratumor tissue than in the distant tissue of the healthy thyroid gland.

Identification and health risk assessment of volatile and semi-volatile migrants along with chemical elements in food contact water-borne coating paper

Water-borne coating paper, with its food contact potential, raises concerns due to unknown contaminants. Herein, the presence and migration of volatile and semi-volatile compounds, along with chemical elements from two water-borne coating paperboards were investigated using 4 % acetic acid, 50 % ethanol, and 95 % ethanol, while also evaluating associated health risks. The results showed that the overall migration to 95 % ethanol from both papers indicated the non-compliance with the reference limit of 10 mg/dm2. Utilizing an optimized direct immersion-solid-phase microextraction coupled to gas chromatography-mass spectrometry method, a total of 66 migrants were identified, among which 16 and 7 were classified as Cramer Ⅲ and Cramer Ⅱ, respectively, linked to coating and paper raw materials. Additionally, 28 chemical elements released from papers were analysed using inductively coupled plasma mass spectrometry, where higher levels of elements (i.e., Na, K) were observed in the migration of 4 % acetic acid, potentially from additives or raw materials used in papermaking processes. More importantly, health risk assessment based on the Threshold of Toxicological Concern approach or worst-case dietary intake assumption indicated that, the estimated daily intake of most migrants and chemical elements through human exposure fell below toxicological reference values. However, certain migrants (e.g., 2-ethylhexyl acrylate, methyl benzoate, phenanthrene, and longifolene) exhibited concerning migration levels in 50 % ethanol and 95 % ethanol that exceed their safety thresholds and may pose health risks. Overall, understanding the migration and potential risk of migrants are imperative for ensuring the safety of using commercially available water-borne coating paper in food contact applications.

Evaluation of thermal maturity of source rock based on geochemical method, a case study of Late Oligocene source rock in Hoa Tra field, Cuu Long basin, Vietnam

The &amp;nbsp;Hoa Tra field is located in the southeast of the Cuu Long basin which has great potential for oil and gas. The source rocks in this area are mainly fine-grained sediments from the late Oligocene and early Miocene, which are located in a continuous deposition zone and under anaerobic conditions. This paper focuses on studying the maturity level of late Oligocene source rock through geochemical analysis methods. Specifically, the paper uses indicators such as T­,&amp;nbsp;R&lt;sub&gt;o&lt;/sub&gt;, MPI-1, T&lt;sub&gt;s&lt;/sub&gt;/(T&lt;sub&gt;s&lt;/sub&gt;+T&lt;sub&gt;m&lt;/sub&gt;) and C&lt;sub&gt;29&amp;nbsp;&lt;/sub&gt;steran 20S/(20S+20R) from Rock-Eval Pyrolysis, Vitrinite reflectance and Gas chromatography-Mass spectrometry methods, respectively, to evaluate the level of thermal maturity of the source rock. The source rocks in the Hoa Tra field mainly contain types I and II, which are poor in vitrinite particles, leading to low&amp;nbsp;R&lt;sub&gt;o&lt;/sub&gt; measurement results. However, when&amp;nbsp;R&lt;sub&gt;o&lt;/sub&gt; is calculated from T&lt;sub&gt;max&amp;nbsp;&lt;/sub&gt;and (MPI-1), it indicates that the thermal maturity of source rock from the upper part of the late Oligocene is in the early mature stage (R&lt;sub&gt;o avg&lt;/sub&gt;= 0.56%), while those from the lower part of late Oligocene are mature and in the phase of oil generation (R&lt;sub&gt;o avg&lt;/sub&gt;= 0.65%). These results are similar to those obtained from assessing thermal maturity using T&lt;sub&gt;s&lt;/sub&gt;/(T&lt;sub&gt;s&lt;/sub&gt;+T&lt;sub&gt;m&lt;/sub&gt; and&amp;nbsp;C&lt;sub&gt;29&amp;nbsp;&lt;/sub&gt;20S/(20S+20R) indicator (the average values for the respective parameters are 0.32 and 0.31 for the upper part, while those are 0.39 and 0.42 for the lower part of late Oligocene). The article also shows that the contribution to the &amp;nbsp;Hoa Tra field is not only from in-situ generated oil but also from migratory oil coming from nearby troughs.

Exploring the Bioactivity of Siddhalepa Asamodagam Spirit from Seeds of Trachyspermum roxburghianum (DC.) H. Wolff

Objectives The water distillate derived from Trachyspermum roxburghianum seeds has been traditionally employed in medicine for treating stomach infections and gastric ulcers. However, no systematic study has been conducted to evaluate its efficacy. Therefore, the present study focused on evaluating the potential health benefits, including the chemical constituents of the distillate. This distillate was prepared and identified as Siddhalepa Asamodagam Spirit (Sid.AS). Methods The chemical constituents of Sid.AS were identified and quantified using Gas Chromatography-Mass Spectrometry (GC-MS) method. The antioxidant potential of Sid.AS samples was assessed in vitro using DPPH and ABTS assays. Various concentrations of Sid.AS were subjected to antimicrobial, anti-obesity, anti-diabetic, anti-inflammatory, and urease inhibition assays according to the standard methods specified by the Ayurvedic Department in Sri Lanka. Results Thymol was identified as the major compound in Sid.AS through GC-MS analysis. Sid.AS demonstrated significant anti-urease, anti-inflammatory, anti-lipase, and antioxidant activities, as evidenced by low IC50 values compared to the positive controls. This suggests its potential in controlling gastric-related disorders, scavenging free radicals, and managing obesity by inhibiting the breakdown and absorption of fats. Additionally, Sid.AS exhibited inhibitory effects against alpha-amylase and alpha-glucosidase enzymes, indicating potential anti-diabetic activity by regulating blood sugar levels. Sid.AS displayed strong antimicrobial activity against tested microorganisms, with higher zones of inhibition and lower MIC and MLC values, indicating its effectiveness in combating microbial infections. Findings from the anti-lipase assay demonstrated activity comparable to that of the positive control, Orlistat. Conclusion The findings of Sid.AS suggest its potential as a multi-functional bioactive herbal distillate with various pharmacological activities. Our results highlight that Sid.AS is a promising natural herbal extract with diverse pharmacological properties, including anti-urease, antioxidant, anti-inflammatory, anti-diabetic, anti-obesity, and antimicrobial activities. Further research and development could explore its potential applications in various therapeutic areas.

Quantitative analysis of pA66/PA6 blend by pyrolysis gas chromatography-mass spectrometry

Abstract A pyrolysis gas chromatography-mass spectrometry method using correction factor area normalization was applied for quantitative analysis of the PA66/PA6 blend ratio. The PA66/PA6 blend sample with known proportions was prepared. The pyro grams of the sample were obtained at the pyrolysis temperature of 600°C. The characteristic peaks-cyclopentanone and caprolactam of thermally decomposed polyester were selected as the peak to quantitatively determine the blending ratio. A correction factor of the characteristic ion peak area and corresponding mass was obtained and applied to quantitative analysis of the proportion of PA66/PA6 blends in the actual sample. The known content PA66/PA6 blend samples with different PA66/PA6 bending ratios were measured, the rate of recovery was from 96.5% to 106.4%, and the relative standard deviation (RSD) was from 0.8% to 7.6% (n = 3). The result showed that the Pyrolysis Gas Chromatography-Mass Spectrometry method is simple and convenient, accurate, which is suitable for the analysis of the PA66/PA6 blending ratio in the full range.

A Reverse Thinking Based on Partially Methylated Aldononitrile Acetates to Analyze Glycoside Linkages of Polysaccharides Using Liquid Chromatography-Multiple Reaction Monitoring Mass Spectrometry.

Glycoside linkage analyses of medicine and food homologous plant polysaccharides have always been a key point and a difficulty of structural characterization. The gas chromatography-mass spectrometry (GC-MS) method is one of the commonly used traditional techniques to determine glycoside linkages via partially methylated alditol acetates and aldononitrile acetates (PMAAs and PMANs). Due to the simplicity of derivatization and the highly structural asymmetry of PMANs, reverse thinking is proposed using liquid chromatography-electrospray ionization-multiple reaction monitoring mass spectrometry (LC-ESI-MRM-MS) for the first time to directly determine the neutral and acidic glycosyl linkages of polysaccharides. The complete characterization of glycoside linkages deduced from PMANs was achieved using a combination of tR values, characteristic MRM ion pairs, diagnostic ESI+-MS/MS fragmentation ions (DFIs), and optimal collision energy (OCE). The DFI and OCE parameters were confirmed to be effective for the auxiliary discrimination of some isomers of the PMANs. The practicality of LC-ESI+-MRM-MS was further verified by analyzing the glycoside linkages of polysaccharides in five medicine and food homologous plants. This method can serve as an alternative to GC-MS for the simultaneous determination of neutral and acidic glycosyl linkages in polysaccharides.

Comparative Analysis of a Secondary Metabolite Profile from Leaves, Peel and Bulbs of Allium sativum L. by GC-MS

Garlic is a herbal plant that is widely used as a medicinal ingredient, because it contains secondary metabolite compounds such as alkaloids, flavonoids, tannins, phenols, terpenoids and saponins. The secondary metabolite content of plants is influenced by genetic, ontogenic, morphogenetic and environmental factors that can influence the biosynthesis and accumulation of secondary metabolites. Garlic is generally only used for the bulbs, while other parts such as the leaves and skin are still not widely used. This study aims to identify the secondary metabolite profile of ethanol extract of garlic leaves, bulbs and peels using the gas chromatography mass spectrometry (GC-MS) method. Identification of secondary metabolite compounds contained in each 70% ethanol extract was analyzed using the tube test, thin layer chromatography (TLC) and GC-MS methods. The results of analysis of secondary metabolite content using the tube test and TLC method showed that the ethanol extract of garlic leaves, skin and bulbs positively contained flavonoids, tannins, phenols and saponins. The results of secondary metabolite profile analysis using the GC-MS method from the ethanol extract of garlic skin and bulbs showed that 5 compounds were obtained with the main compound being 3,4-Dihydroxyphenylacetic acid and 23 compounds with the main compound being 1,2-Benzenedicaboxylic acid and palmitic acid, while the leek extract white only detected 1 compound. The conclusion is that the ethanol extract of garlic leaves, skin and bulbs has secondary metabolites in the form of flavonoids, tannins, phenols and saponins. There are differences in the profile of secondary metabolite compounds in the ethanol extract of garlic leaves, skin and bulbs in terms of the results of GC-MS analysis.

Headspace Gas Chromatography Mass Spectrometry Method for Determination of class-I Residual Solvents in Several Drug Substances: Method Evaluation by Quality by Design Statistical Tool.

Class-I residual solvents such as 1,1-dichloroethene, 1,1,1-trichloroethane, carbon tetrachloride, benzene, 1,2-dichloroethane are toxic, environmental hazard and carcinogenic to human. Headspace gas chromatography mass spectrometer is the sophisticated instrument for quantification of residual solvents at lower limits. An exact, sensitive, reliable and fast method was developed to determine the 1,1-dichloroethene, 1,1,1-trichloroethane, carbon tetrachloride, benzene and 1,2-dichloroethane present in different drug substances by using a headspace gas chromatography mass spectrometer. Helium is used as a carrier gas in this method. N-Methyl-2-pyrrolidone is used as a diluent and the stationary phase is a DB-624 (60 m x 0.25 mm x 1.4 μm film thickness) column with a flow rate of 1.5 mL/min. The concentration of limit of detection for 1,1-dichloroethene, 1,1,1-trichloroethane, carbon tetrachloride, benzene and 1,2-dichloroethane were achieved with 0.24 ppm, 5 ppm, 0.12 ppm, 0.06 ppm, 0.15 ppm. Subsequently, the concentrations of limit of quantification for aforementioned impurities were achieved with 0.8 ppm, 15 ppm, 0.4 ppm, 0.2 ppm, 0.5 ppm. The linearity was covered in the range of LOQ to 120% with respect to the specification level. The current method's system suitability, precision, linearity, accuracy parameters were performed in accordance to the USP < 1225> and ICH Q2(R2) and results were lies within the acceptance criteria. No research studies are reported for the determination of class-I residual solvents in lincomycin hydrochloride, dapagliflozin, vonoprazan fumarate, telmisartan drug substances. The proposed study is to develop the common method for quantification of class-I residual solvents for drug substances. QbD concept is utilized in the method performance verification.

Drugs in blood and urine samples from victims of suspected exposure to drink spiking: A prospective observational study from Oslo, Norway.

People regularly contact emergency medicine services concerned that they have been exposed to drink spiking, i.e., exposure to drugs without their knowledge or permission. We identified drugs in blood and urine samples from patients suspecting exposure to drink spiking, with special consideration for drugs not reported taken by the patient (unreported drugs). From September 2018 to May 2019, we collected blood and urine samples from patients 16 years or older presenting at an emergency clinic in Oslo, Norway, within 48 hours of suspected exposure to drink spiking. We also collected information on ethanol ingestion and drugs taken. Blood samples were analyzed for 20 classical recreational drugs using ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) and an automated enzymatic method for ethanol. Urine samples were analyzed using immunoassay methods and a specific gas chromatography mass spectrometry (GCMS) method for gammahydroxybutyrate (GHB). From 100 included patients (median age 24 years, 62 females), we collected 100 blood samples and 72 urine samples. Median time since exposure was 5 hours. Unreported drugs were found in 15 patients. Unreported drugs in the blood samples were clonazepam in 3, methylenedioxymethamphetamine (MDMA) in 3, amphetamine in 2, tetrahydrocannabinol (THC) in 2, tramadol in 1, cocaine in 1, and methamphetamine in 1. Unreported drugs in the urine samples were cocaine in 5, amphetamine in 4, ecstasy in 3, and cannabis in 2. Ethanol was found in 69 patients, all reporting ethanol ingestion. Median blood ethanol concentration was higher in patients with no unreported drugs detected, 1.00‰ (interquartile range (IQR) 0-1.52) vs. 0‰ (IQR 0-0.46) (p<0.001). GHB was not detected. Unreported drugs, possibly used for drink spiking, were found in 15% of patients. Blood ethanol concentration was higher when no unreported drugs were found. GHB was not detected in any patient.

Assessment of β-lactamase inhibition and antioxidant potential of ethanolic and aqueous leaf extracts of Irvingia gabonensis using GC-MS method

Objectives: This study aimed to investigate the antibiotic and antioxidant potential of aqueous and ethanol extracts from Irvingia gabonensis leaves, with a specific focus on their ability to inhibit β-lactamase enzyme activity. Both in vitro and in vivo approaches were employed to comprehensively assess the characteristics of the leaf extracts. Irvingia gabonensis, known for its medicinal properties, has been of interest due to its reported pharmacological activities. In the face of rising antimicrobial resistance, exploring natural sources for antimicrobial and antioxidant agents is crucial. This study builds upon existing knowledge by evaluating the phytochemical composition and potential therapeutic applications of Irvingia gabonensis leaf extracts. Materials and Methods: Gas chromatography-mass spectrometry (GC-MS) analysis was employed to identify the chemical components present in ethanolic leaf extracts. Antioxidant activities were assessed through various assays, including DPPH, FRAP, nitric oxide radical scavenging, and MDA scavenging assays. In vivo experiments involved the administration of different concentrations of leaf extracts to albino rats over a 28-day period. Blood samples collected were utilized for serum separation, enabling the analysis of antioxidant assays in vivo, including β-lactamase inhibition, lipid peroxidation (MDA), superoxide dismutase (SOD), and catalase (CAT) activity. Results: The ethanolic extracts exhibited a significant 65.96% inhibition rate against β-lactamase enzyme activity. Additionally, there was an increase in the concentrations of glutathione (GSH) and glutathione peroxidase (GPx), as well as heightened catalase (CAT) activity. Simultaneously, a decrease in malondialdehyde (MDA) concentration indicated the extracts’ potential to mitigate lipid peroxidation. These results highlight the robust antimicrobial and antioxidant properties of Irvingia gabonensis leaf extracts. Conclusion: Irvingia gabonensis leaf extracts demonstrate substantial potential as antimicrobial and antioxidant agents, emphasizing their role in combating antimicrobial resistance. The significant inhibition of β-lactamase enzyme activity and the modulation of key antioxidant markers suggest the extracts’ therapeutic relevance. This study contributes to the understanding of Irvingia gabonensis phytochemical composition and supports its potential application as an antioxidant supplement and β-lactamase inhibitor.

Comparative pharmacognostic study of the roots of the most common species of plants of the genus arctium

The aim is to carry out a comparative pharmacognostic study of the roots of A. tomentosum and A. minus with the root of A. lappa to confirm or deny their interchangeability. Materials and methods. A Delta optic BioLight 300 microscope (Poland) was used to study the macro- and microscopic features of plant raw materials. The method of gas chromatography-mass spectrometry was used to identify and quantify organic, including fatty, acids. Quantitative content of amount of organic acids, ascorbic acid, total polyphenols and amount of hydroxycinnamic acids was determined by using spectrophotometry. The content of polysaccharides was determined by the gravimetric method. The results. For the first time, a comparative morphological and anatomical study of the roots of A. tomentosum and A. minus in comparison with the root of A. lappa was carried out. As a result, a distinctive diagnostic microscopic feature of the roots was established: the shape of the receptacles of the schizogen type. For the first time, the component composition of organic, including fatty acids, for the roots of A. tomentosum and A. minus was determined in comparison with the root of A. lappa, which is the same. The content of 11 organics and 12 fatty acids in plant raw materials of 3 Arctium species was identified and determined. The quantitative content of the amount of organic acids, ascorbic acid, polysaccharides, total polyphenols, and amount of hydroxycinnamic acids in the roots of A. tomentosum and A. minus in comparison with the root of A. Lappa was established, and these indicators are comparable. Conclusions. For the first time, a comparative pharmacognostical study of the roots of A. tomentosum and A. minus in comparison with the root of A. lappa was carried out which showed minor differences between the roots of these Arctium species and confirms their interchangeability at this stage, especially when harvesting wild plant raw materials, when identification of the species at the botanical level is impossible

Potential of dragon’s blood fruit (Calamus draco) as a class I preservative agent and additive ingredient to improve the quality of whole coconut VCO (Virgin coconut oil)

The method developed uses whole coconut as the raw material for making VCO through an easy-to-apply fermentation process, adding dragon’s blood fruit extract in concentrations of 0%, 20%, 40%, 60%, and 80%. Peroxide and iodine numbers were tested as parameters of VCO quality. The gas chromatography mass spectrometry (GCMS) method was used to analyze the fatty acid profile of VCO after transesterification. The results showed that the highest total saturated fatty acid content of 97.28% was found in the VCO sample with a 40% concentration of dragon’s blood fruit, and the unsaturated fatty acid profiles detected in the VCO included palmitoleic acid, methyl linoleic, and methyl oleic. The addition of dragon’s blood fruit can also reduce the peroxide number and increase the iodine number in accordance with SNI 7381-2008, which is below the maximum limit of the VCO peroxide number of 2.0 mEq/kg of oil while the iodine number of the VCO is in the range of 4.1–11 g iodine/100g. It can be concluded that a 40% dragon’s blood fruit concentration can improve the quality of VCO preservation.

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.