Plant-Derived and Synthetic Nicotine in E-Cigarettes: Is Differentiation with NMR Spectroscopy Possible?

To circumvent regulatory frameworks, many producers start to substitute plant-derived nicotine (tobacco-derived nicotine, TDN) by synthetic nicotine (tobacco-free nicotine, TFN) in e-cigarette products. Due to the higher costs of enantiomeric synthesis and purification of TFN, there is a need to develop an analytical method that clearly distinguishes between the two sources. To trace nicotine's origin, its enantiomeric purity can be postulated by H NMR spectroscopy using ()-(-)-1,1'-binaphthyl-2,2'-diyl hydrogen phosphate (BNPPA) as a chiral complexing agent.

Multicomponent analysis of dietary supplements containing glucosamine and chondroitin: comparative low- and high-field NMR spectroscopic study.

With the prevalence of glucosamine- and chondroitin-containing dietary supplements for people with osteoarthritis in the marketplace, it is important to have an accurate and reproducible analytical method for the quantitation of these compounds in finished products. NMR spectroscopic method based both on low- (80 MHz) and high- (500-600 MHz) field NMR instrumentation was established, compared and validated for the determination of chondroitin sulfate and glucosamine in dietary supplements. The proposed method was applied for analysis of 20 different dietary supplements.

Development of potato (Solanum tuberosum L.) plants with StLEAFY knockout.

StLFY-knockout potato plants were developed using CRISPR/Cas9 system. Inflorescences of edited plants transited to flowering, but inflorescence structures lacked flowers and were indeterminate, producing multiple shoot meristems. The tetraploid potato (Solanum tuberosum L.

Nuclear magnetic resonance spectroscopy as an elegant tool for a complete quality control of crude heparin material.

Nuclear magnetic resonance (NMR) spectrometric methods for the quantitative analysis of pure heparin in crude heparin is proposed. For quantification, a two-step routine was developed using a USP heparin reference sample for calibration and benzoic acid as an internal standard. The method was successfully validated for its accuracy, reproducibility, and precision.

Is the Calibration Transfer of Multivariate Calibration Models between High- and Low-Field NMR Instruments Possible? A Case Study of Lignin Molecular Weight.

Although several successful applications of benchtop nuclear magnetic resonance (NMR) spectroscopy in quantitative mixture analysis exist, the possibility of calibration transfer remains mostly unexplored, especially between high- and low-field NMR. This study investigates for the first time the calibration transfer of partial least squares regressions [weight average molecular weight () of lignin] between high-field (600 MHz) NMR and benchtop NMR devices (43 and 60 MHz). For the transfer, piecewise direct standardization, calibration transfer based on canonical correlation analysis, and transfer via the extreme learning machine auto-encoder method are employed.

Benchtop versus high field NMR: Comparable performance found for the molecular weight determination of lignin.

Lignin is a promising renewable biopolymer being investigated worldwide as an environmentally benign substitute of fossil-based aromatic compounds, e.g. for the use as an excipient with antioxidant and antimicrobial properties in drug delivery or even as active compound.

Multinuclear NMR screening of pharmaceuticals using standardization by H integral of a deuterated solvent.

NMR standardization approach that uses the H integral of deuterated solvent for quantitative multinuclear analysis of pharmaceuticals is described. As a proof of principle, the existing NMR procedure for the analysis of heparin products according to US Pharmacopeia monograph is extended to the determination of Na and Cl content in this matrix. Quantification is performed based on the ratio of a Na (Cl) NMR integral and H NMR signal of deuterated solvent, DO, acquired using the specific spectrometer hardware.

Is NMR Combined with Multivariate Regression Applicable for the Molecular Weight Determination of Randomly Cross-Linked Polymers Such as Lignin?

The molecular weight properties of lignins are one of the key elements that need to be analyzed for a successful industrial application of these promising biopolymers. In this study, the use of H NMR as well as diffusion-ordered spectroscopy (DOSY NMR), combined with multivariate regression methods, was investigated for the determination of the molecular weight ( and ) and the polydispersity of organosolv lignins ( = 53, , , and ). The suitability of the models was demonstrated by cross validation (CV) as well as by an independent validation set of samples from different biomass origins (beech wood and wheat straw).

Tracing the origin of paracetamol tablets by near-infrared, mid-infrared, and nuclear magnetic resonance spectroscopy using principal component analysis and linear discriminant analysis.

Most drugs are no longer produced in their own countries by the pharmaceutical companies, but by contract manufacturers or at manufacturing sites in countries that can produce more cheaply. This not only makes it difficult to trace them back but also leaves room for criminal organizations to fake them unnoticed. For these reasons, it is becoming increasingly difficult to determine the exact origin of drugs.

An ERF121 transcription factor from Brassica oleracea is a target for the conserved TAL-effectors from different Xanthomonas campestris pv. campestris strains.

Transcription activator-like effectors (TALEs), which induce the expression of specific plant genes to promote infection, are the main pathogenic determinants of various Xanthomonas bacteria. However, investigation of TALEs from Xanthomonas campestris pv. campestris, which causes black rot disease of crucifers, received little attention.

Lignins Isolated via Catalyst-Free Organosolv Pulping from , , and : A Comparative Study.

As a low-input crop, offers numerous advantages that, in addition to agricultural applications, permits its exploitation for energy, fuel, and material production. Depending on the genotype, season, and harvest time as well as plant component (leaf versus stem), correlations between structure and properties of the corresponding isolated lignins differ. Here, a comparative study is presented between lignins isolated from , , and using a catalyst-free organosolv pulping process.

Is infrared spectroscopy combined with multivariate analysis a promising tool for heparin authentication?

The investigation of the possibility to determine various characteristics of powder heparin (n = 115) was carried out with infrared spectroscopy. The evaluation of heparin samples included several parameters such as purity grade, distributing company, animal source as well as heparin species (i.e.

Novel approach of qNMR workflow by standardization using 2H integral: Application to any intrinsic calibration standard.

Quantitative nuclear magnetic resonance (qNMR) is routinely performed by the internal or external standardization. The manuscript describes a simple alternative to these common workflows by using NMR signal of another active nuclei of calibration compound. For example, for any arbitrary compound quantification by NMR can be based on the use of an indirect concentration referencing that relies on a solvent having both 1H and 2H signals.

Quality Control of Heparin Injections: Comparison of Four Established Methods.

Heparin is an anticoagulant medication that is usually injected subcutaneously. The quality of a set of commercial heparin injections from different producers was examined by NMR, IR, UV-Vis spectroscopies and potentiometric multisensor system. The type of raw material regarding heparin animal origin and producer, heparin molecular weight and activity values were derived based on the non-targeted analysis of H NMR fingerprints.

Distinguishing paracetamol formulations: Comparison of potentiometric "Electronic Tongue" with established analytical techniques.

Fast and inexpensive analytical tools for identification of the origin of pharmaceutical formulations are important to ensure consumers safety. This study explores the potential of potentiometric multisensor systems ("electronic tongues") in this type of application. 72 paracetamol samples purchased in different countries and produced by various companies were studied via infrared spectroscopy (IR), near infrared spectroscopy (NIR), nuclear magnetic resonance spectroscopy (NMR) and multisensor system (ET).

Extraction of High-Purity Lignins via Catalyst-free Organosolv Pulping from Low-Input Crops.

A catalyst-free organosolv pulping process was applied to cup plant (, S), Miscanthus grass (, M), and the Paulownia tree (, P), resulting in high-purity lignins with no signals for cellulose, hemicellulose, or other impurities in two-dimensional heteronuclear single quantum coherence (HSQC) nuclear magnetic resonance (NMR) spectra. Different biomass particle sizes used for the organosolv pulping (1.6-2.

Comparing chemical composition and lignin structure of and harvested in autumn and spring and separated into stems and leaves.

crops possess very attractive properties such as high photosynthesis yield and carbon fixation rate. Because of these properties, it is currently considered for use in second-generation biorefineries. Here we analyze the differences in chemical composition between , a commonly studied genotype, and , which is relatively understudied but has useful properties such as increased frost resistance and higher stem stability.

Independent components analysis (ICA) at the "cocktail-party" in analytical chemistry.

Independent components analysis (ICA) is a probabilistic method, whose goal is to extract underlying component signals, that are maximally independent and non-Gaussian, from mixed observed signals. Since the data acquired in many applications in analytical chemistry are mixtures of component signals, such a method is of great interest. In this article recent ICA applications for quantitative and qualitative analysis in analytical chemistry are reviewed.

Quo Vadis qNMR?

The quantification of a drug, its impurities, and e.g. components of a mixture has become routine in NMR laboratories and many applications have been described in the literature.

Anticoagulant activity of porcine heparin: Structural-property relationship and semi-quantitative estimation by nuclear magnetic resonance (NMR) spectrometry.

Heparin is a carbohydrate polymer, which is clinically used as an anticoagulant for the treatment of thrombotic disorders. The anticoagulant process is mainly mediated by the interaction of heparin with antithrombin followed by inhibition of clotting factors IIa (FIIa) and Xa (FXa). The influence of polymer disaccharide structure, average molecular weight and impurity profiling (e.

Retrospective multivariate analysis of pharmaceutical preparations using H nuclear magnetic resonance (NMR) spectroscopy: Example of 990 heparin samples.

NMR spectroscopy has become an essential diagnostic tool for pharmaceutical preparations worldwide, with many runs performed annually on a routine basis. In this study multivariate analysis was performed on a big dataset of 990 NMR heparin spectra recorded over six years (2012-2017) in our laboratory. Several steps of statistical analysis of accumulated data were used to differentiate samples according to animal origin (bovine, porcine and ovine heparin), purity grade (crude and purified heparin), distributing company as well as to estimate their closeness to the heparin reference sample (SST) provided by US Pharmacopeia.

Fragmentation Through Polymerization (FTP): A new method to fragment DNA for next-generation sequencing.

Fragmentation of DNA is the very important first step in preparing nucleic acids for next-generation sequencing. Here we report a novel Fragmentation Through Polymerization (FTP) technique, which is a simple, robust, and low-cost enzymatic method of fragmentation. This method generates double-stranded DNA fragments that are suitable for direct use in NGS library construction and allows the elimination of the additional step of reparation of DNA ends.

x Stem Versus Leaf-Derived Lignins Differing in Monolignol Ratio and Linkage.

As a renewable, offers numerous advantages such as high photosynthesis activity (as a C₄ plant) and an exceptional CO₂ fixation rate. These properties make very attractive for industrial exploitation, such as lignin generation. In this paper, we present a systematic study analyzing the correlation of the lignin structure with the genotype and plant portion (stem versus leaf).

Automated multicomponent phospholipid analysis using P NMR spectroscopy: example of vegetable lecithin and krill oil.

Nuclear magnetic resonance (NMR) spectroscopy is widely applied in the field of metabolomics due to its quantitative nature and the reproducibility of data generated. However, one of the main challenges in routine NMR analysis is to obtain valuable information from large datasets of raw data in a high-throughput, automatic, and reproducible manner. In this study, a method to automatically annotate and quantify 12 phospholipids (PLs) in vegetable lecithin (soy, sunflower, rape) and krill oil is introduced.