Mccoycoates3493
A liquid chromatography (LC) stability-indicating method was developed and validated for the quantitative determination of bilastine in coated tablets.
The procedure was validated for specificity, linearity, robustness, precision, and accuracy. Plackett-Burmann experimental design was used to determine the robustness of the method.
Chromatographic separation was performed on a Shim-pack® RP-18 column with fluorescence detection. The degradation products formed under oxidative conditions were isolated and identified using high-resolution mass spectrometry (HRMS). In silico prediction of degradation products and in silico toxicity studies were also performed.
The LC method presented good recovery and precision (intraday and interday), the response was linear in a range of 0.20 to 0.70 μg mL-1, and the results demonstrated the robustness of the analytical method under the evaluated conditions.
The degradation products were identified as benzimidazole (DP1) and amine N-oxide of bilastine (DP2). The results for the toxicity studies demonstrated the high mutagenic potential of DP1 and hepatotoxicity and hERG I inhibitor effects of DP2.
Bilastine degradation products were identified as benzimidazole and amine N-oxide using HRMS.
Bilastine degradation products were identified as benzimidazole and amine N-oxide using HRMS.
As known to us, HPLC method was often used to determine the contents of Angelicae sinesis Radix. In view of the shortcomings of HPLC method, qNMR has prominent advantages in determining the contents of bioactive components in the quantitative and qualitative analysis of Angelicae sinesis Radix.
In this study, a quick, simple, and accurate method was established to determine the components of ferulic acid, coniferyl ferulate, and ligustilide in Angelicae sinesis Radix.
Using dimethyl sulfoxide-d6(DMSO-d6) as the test solvent and pyrazine as the internal standard substance, 1H-qNMR measurement was performed on a 600 MHz spectrometer. The quantitative resonance peaks of pyrazine, ferulic acid, ligustilide, and coniferyl ferulate were at δ8.66 ppm, δ6.35-6.37 ppm, δ5.53-5.55 ppm, and δ6.50-6.53 ppm, respectively.
The linear relationship, limit of detection, limit of quantification, precision, stability, and recovery were verified and the results were good. On the other hand, it was verified by HPLC, and the HPLC used for verification passed the methodological investigation of linearity, precision, repeatability, stability, and recovery, and the results were good. In addition, no significant difference in results was found between the 1H-qNMR and HPLC-UV methods in determining the content of three components in three batches of Angelicae sinesis Radix.
The method can be used for simultaneous determination of three active components, and providing a scientific basis for the overall quality evaluation and quality control of Angelicae sinesis Radix.
In this study, 1H-qNMR was used to determine ferulic acid, coniferyl ferulate and ligustilide in Angelicae Sinensis Radix for the first time.
In this study, 1H-qNMR was used to determine ferulic acid, coniferyl ferulate and ligustilide in Angelicae Sinensis Radix for the first time.
Tea is a popular traditional non-alcoholic beverage worldwide. Flonicamid is a selective systemic pyridine carboxamide insecticide that is widely used for controlling tea leafhopper in tea.
The leaching rates, dissipation dynamics, and residue levels of flonicamid and its metabolites in tea leaves during processing and transferring were investigated to validate the safe risk in tea and transfer behavior using high performance liquid chromatography-tandem mass spectrometry with a convenient pretreatment method.
The extracting method and immersion rate experiments were optimized by single factor analysis and orthogonal tests.The acetonitrile extracting solvent with 0.5% formic acid was used and optimal leaching conditions were obtained with a regime of 15 min immersion time, 100°C temperature, three immersions and a tea-to-water ratio of 150.
Average recoveries in processed green tea and infusions were 80.85-98.75% with relative standard deviations <5.87%. LODs and LOQs of flonicamid, 4-trifluoromethylnicotinic acid (TFNA), N-(4-trifluoromethylnicotinoyl) glycine (TFNG), and 4-trifluoromethylnicotinamide (TFNA-AM) were 0.0013-0.350 and 0.004-1 μg/g, respectively. The processing factor of flonicamid was 0.36-5.52 during green tea manufacture. The leaching rates were 22.9-97.4% from processed tea to infusion.
The risk of long-term and short-term dietary intake of flonicamid was safe in tea infusions with the risk quotient (RQ) values <1 for the Chinese consumer. This work may provide guidance for safe and reasonable consumption of flonicamid in tea in China.
The suitable leaching factors of flonicamid and its metabolites in tea infusions were optimized by orthogonal experimentation for the first time.
The suitable leaching factors of flonicamid and its metabolites in tea infusions were optimized by orthogonal experimentation for the first time.
Moringa pods are known for their nutritional and health benefits. The cultivation of this crop receives frequent pesticide applications. In the absence of risk assessment data, maximum residue limits of pesticides in this crop are considered at the default level (0.01 mg/kg). However, there exists scarcely any validated method for pesticide residue analysis in this matrix.
This study was undertaken to develop and validate a multiresidue method for the simultaneous analysis of multi-class pesticides in moringa pods by gas chromatography-tandem mass spectrometry (GC-MS/MS), and liquid chromatography-tandem mass spectrometry (LC-MS/MS).
The homogenized sample (10 g) was extracted with acetonitrile (10 mL). The extract was cleaned by dispersive solid-phase extraction using a combination of 50 mg primary secondary amine, 5 mg graphitized carbon black, and 25 mg C18 sorbents, and was directly analyzed by LC-MS/MS. Another portion of the extract was reconstituted in ethyl acetate before GC-MS/MS analysis. The curacy, and precision.
The study reports a validated method for large-scale multiresidue analysis of pesticides in moringa matrix for the first time. The method provided a high throughput analysis of multi-class pesticides with satisfactory selectivity, sensitivity, accuracy, and precision.
Synthetic musk compounds are widely used as fragrances in many consumer products; however, information on human exposure and health effects is limited. Also, analytical methods for their quantification in biological matrices are limited.
In this study, an integrated method was developed and validated for the analysis of selected synthetic musk compounds in human serum.
The method is based on liquid-liquid extraction (LLE), sample clean-up by solid-phase extraction (SPE), and separation and detection by gas chromatography coupled with tandem mass spectrometry (GC-MS/MS).
The method demonstrated good recoveries (86-105%) and high sensitivity, with low method detection limits (MDLs) ranging from 0.04 to 0.17 µg/L. The method was applied to the analysis of 10 synthetic musk compounds in 40 serum samples collected from Canadian women aged 20-44 years (20 individual samples collected in 2014 and 20 pooled samples collected in 2006). The most commonly detected compound was Galaxolide (HHCB), with median concentrations of 0.59 µg/L in samples collected in 2006, and 0.34 µg/L for samples collected in 2014. Musk ketone (MK) was not detected in any of the samples collected in 2006, but was detected in 60% of the samples collected in 2014 with a median concentration of 0.29 µg/L. Tonalide (AHTN) was detected in only one sample above its MDL (0.12 µg/L).
This is the first study in Canada to report levels of synthetic musks in human. The data generated from this study has been used in risk screening assessment by Environment and Climate Change Canada and Health Canada.
This is the first study in Canada to report levels of synthetic musks in human. The data generated from this study has been used in risk screening assessment by Environment and Climate Change Canada and Health Canada.Acetyl-CoA carboxylase (ACC) is an enzyme within the de novo lipogenesis (DNL) pathway and plays a role in regulating lipid metabolism. Pharmacologic ACC inhibition has been an area of interest for multiple potential indications including oncology, acne vulgaris, metabolic diseases such as type 2 diabetes mellitus, and non-alcoholic fatty liver disease/non-alcoholic steatohepatitis. A critical role for ACC in de novo synthesis of long-chain fatty acids during fetal development has been demonstrated in studies in mice lacking Acc1, where the absence of Acc1 results in early embryonic lethality. Following positive predictions of developmental toxicity in alternative in vitro assays (positive in murine embryonic stem cell [mESC] assay and rat whole embryo culture, but negative in zebrafish), developmental toxicity (growth retardation and dysmorphogenesis associated with disrupted midline fusion) was observed with the oral administration of the dual ACC1 and 2 inhibitor, PF-05175157, in Sprague Dawley rats and New Zealand White rabbits. The results of these studies are presented here to make comparisons across the assays, as well as mechanistic insights from the mESC assay demonstrating high ACC expression in the mESC and that ACC induced developmental toxicity can be rescued with palmitic acid providing supportive evidence for DNL pathway inhibition as the underlying mechanism. Ultimately, while the battery of alternative approaches and weight-of-evidence case were useful for hazard identification, the embryo-fetal development studies were necessary to inform the risk assessment on the adverse fetal response, as malformations and/or embryo fetal lethality were limited to doses that caused near complete inhibition of DNL.Observational evidence shows that the use of multiple arterial grafts (MAG) is associated with longer postoperative survival and improved clinical outcomes. The current European Society of Cardiology/European Association for Cardio-Thoracic Surgery Guidelines on myocardial revascularization recommend the use of MAG in appropriate patients. However, a significant volume-to-outcome relationship exists for MAG, and lack of sufficient experience is associated with increased operative risk. A stepwise approach to building experience with MAG allows successful implementation of this technique into routine coronary surgery practice.Glucose levels are tightly regulated at all times. Gluconeogenesis is the metabolic pathway dedicated to glucose synthesis from non-hexose precursors. Gluconeogenesis is critical for glucose homoeostasis, particularly during fasting or stress conditions. The renal contribution to systemic gluconeogenesis is increasingly recognized. During the post-absorptive phase, the kidney accounts for ∼40% of endogenous gluconeogenesis, occurring mainly in the kidney proximal tubule. The main substrate for renal gluconeogenesis is lactate and the process is regulated by insulin and cellular glucose levels, but also by acidosis and stress hormones. The kidney thus plays an important role in the maintenance of glucose and lactate homoeostasis during stress conditions. The impact of acute and chronic kidney disease and proximal tubular injury on gluconeogenesis is not well studied. Ispinesib Recent evidence shows that in both experimental and clinical acute kidney injury, impaired renal gluconeogenesis could significantly participate in systemic metabolic disturbance and thus alter the prognosis.
