scholarly journals A High-Throughput Method for the Comprehensive Analysis of Terpenes and Terpenoids in Medicinal Cannabis Biomass

Metabolites ◽  
2020 ◽  
Vol 10 (7) ◽  
pp. 276
Author(s):  
Christian Krill ◽  
Simone Rochfort ◽  
German Spangenberg

Cannabis and its secondary metabolite content have recently seen a surge in research interest. Cannabis terpenes and terpenoids in particular are increasingly the focus of research efforts due to the possibility of their contribution to the overall therapeutic effect of medicinal cannabis. Current methodology to quantify terpenes in cannabis biomass mostly relies on large quantities of biomass, long extraction protocols, and long GC gradient times, often exceeding 60 min. They are therefore not easily applicable in the high-throughput environment of a cannabis breeding program. The method presented here, however, is based on a simple hexane extract from 40 mg of biomass, with 50 μg/mL dodecane as internal standard, and a gradient of less than 30 min. The method can detect 48 individual terpenes and terpenoids and was validated for selectivity, linearity, LOD/LOQ, precision, intermediate precision, and accuracy (recovery) for 22 terpenes and terpenoids. The validation parameters are comparable to previously published studies that employ significantly longer runtimes and/or more complex extraction protocols. It is currently being applied to medicinal cannabis precision breeding programs.

2021 ◽  
Author(s):  
Kyle J. Walker ◽  
Christopher T. Williams ◽  
Folasade O. Oladepo ◽  
John Richard Lucas ◽  
David Malone ◽  
...  

Abstract Long-lasting insecticide-treated nets (LLINs) are essential to preventing malaria transmission. The LLINs should last for at least three years, even after repeated washings. Currently, tracking insecticides in LLINs is cumbersome, costly, and requires specialized equipment and hazardous solvents. We therefore developed a low-resource, high-throughput method for detecting insecticides in LLINs. In order to extract insecticides from polyethylene, LLIN samples were heated for 45 minutes at 85oC in 1-propanol-heptane containing dicyclohexylphthalate as an internal standard. Sample size was reduced to ~0.2 g for reduced extraction volume, which is 10% less than what was recommended. We optimized HPLC chromatographic conditions to assess pyrethroid and pyriproxyfen content in polyethylene-based LLINs. The method is capable of quantifying levels ≥ 0.0015% permethrin, 0.00045% alpha-cypermethrin and 0.00025% pyriproxyfen (w/w) in polyethylene, allowing tracking the insecticides before and after LLINs use. A variety of LLINs can be evaluated with this method, including those with 1% pyriproxyfen (pyriproxyfen-LLIN) or 2% permethrin (Olyset® Net), 1% pyriproxyfen and 2% permethrin (Olyset® Duo), or 0.55% pyriproxyfen combined with 0.55% alpha-cypermethrin (Royal Gaurd®). Analysis of 120 samples (40 nets) per run can be done with high precision and accuracy, reducing labour time and costs whilst reducing the environmental impact of organic solvents.


Planta Medica ◽  
2016 ◽  
Vol 82 (05) ◽  
Author(s):  
C Avonto ◽  
AG Chittiboyina ◽  
D Rua ◽  
IA Khan

2019 ◽  
Vol 15 (5) ◽  
pp. 591-598 ◽  
Author(s):  
Haitham Alrabiah ◽  
Ahmed Bakheit ◽  
Sabray Attia ◽  
Gamal A.E. Mostafa

Background: Conivaptan inhibits two of vasopressin receptor (vasopressin receptor V1a and V2). Conivaptan is used for the treatment of hyponatremia, and in some instances, for the treatment of the heart failure. Methods: The present study aimed to develop a simple, sensitive, and accurate HPLC with ultraviolet detection for the assay of conivaptan (CON) in mouse plasma using bisoprolol as internal standard (IS). A precipitation procedure was used to extract CON and the IS from the mouse plasma. CON was chromatographically separated using a C18 analytical column at 25°C. The separation was carried out using a mixture of phosphate buffer (50 mM): acetonitrile (60: 40, v/v, pH 4.5) with a flow rate of 1.0 mL/min and detection was performed at 240 nm. Results: The assay was validated according to the US Food and Drug (FDA) guidelines. The method demonstrated linearity over a concentration range of 150 - 2000 ng/mL (correlation coefficient: r 2 = 0.9985). The mean recovery of CON from the mouse plasma was 101.13%. All validation parameters for CON were within the acceptable range. Conclusion: The investigated method has been shown to be suitable for estimating the CON in plasma samples, and this method is sensitive and highly selective, allowing the estimation of its concentrations up to the nano-scale. The suggested method was successfully used in a pharmacokinetic study of CON in mouse plasma.


Molecules ◽  
2021 ◽  
Vol 26 (6) ◽  
pp. 1656
Author(s):  
Nataliya E. Kuz’mina ◽  
Sergey V. Moiseev ◽  
Mikhail D. Khorolskiy ◽  
Anna I. Lutceva

The authors developed a 1H qNMR test procedure for identification and quantification of impurity A present in gabapentin active pharmaceutical ingredient (API) and gabapentin products. The validation studies helped to determine the limit of quantitation and assess linearity, accuracy, repeatability, intermediate precision, specificity, and robustness of the procedure. Spike-and-recovery assays were used to calculate standard deviations, coefficients of variation, confidence intervals, bias, Fisher’s F test, and Student’s t-test for assay results. The obtained statistical values satisfy the acceptance criteria for the validation parameters. The authors compared the results of impurity A quantification in gabapentin APIs and capsules by using the 1H qNMR and HPLC test methods.


Polymers ◽  
2021 ◽  
Vol 13 (8) ◽  
pp. 1313
Author(s):  
Andreas Hoffmann ◽  
Alexander J. C. Kuehne

Carbon nanofiber nonwovens are promising materials for electrode or filtration applications; however, their utilization is obviated by a lack of high throughput production methods. In this study, we utilize a highly effective high-throughput method for the fabrication of polyacrylonitrile (PAN) nanofibers as a nonwoven on a dedicated substrate. The method employs rotational-, air pressure- and electrostatic forces to produce fibers from the inner edge of a rotating bell towards a flat collector. We investigate the impact of all above-mentioned forces on the fiber diameter, morphology, and bundling of the carbon-precursor PAN fibers. The interplay of radial forces with collector-facing forces has an influence on the uniformity of fiber deposition. Finally, the obtained PAN nanofibers are converted to carbon nonwovens by thermal treatment.


Soft Matter ◽  
2021 ◽  
Author(s):  
Tao Lin ◽  
Zhen Wang ◽  
Wen Wang ◽  
Yi Sui

We have developed a high-throughput method, by combining a hybrid neural network with a mechanistic capsule model, to predict membrane elasticity and viscosity of microcapsules from their dynamic deformation in a branched microchannel.


Nutrients ◽  
2021 ◽  
Vol 13 (5) ◽  
pp. 1466
Author(s):  
Lisard Iglesias-Carres ◽  
Lauren A. Essenmacher ◽  
Kathryn C. Racine ◽  
Andrew P. Neilson

Choline is metabolized by the gut microbiota into trimethylamine (TMA), the precursor of pro-atherosclerotic molecule trimethylamine N-oxide (TMAO). A reduction in TMA formation has shown cardioprotective effects, and some phytochemicals may reduce TMA formation. This study aimed to develop an optimized, high-throughput anaerobic fermentation methodology to study the inhibition of choline microbial metabolism into TMA by phenolic compounds with healthy human fecal starter. Optimal fermentation conditions were: 20% fecal slurry (1:10 in PBS), 100 µM choline, and 12 h fermentation. Additionally, 10 mM of 3,3-dimethyl-1-butanol (DMB) was defined as a positive TMA production inhibitor, achieving a ~50% reduction in TMA production. Gallic acid and chlorogenic acid reported higher TMA inhibitory potential (maximum of 80–90% TMA production inhibition), with IC50 around 5 mM. Neither DMB nor gallic acid or chlorogenic acid reduced TMA production through cytotoxic effects, indicating mechanisms such as altered TMA-lyase activity or expression.


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