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Food authenticity is becoming increasingly important to consumers, producers, and retailers. Furthermore, more and more food properties considered to be value-relevant are advertised. Food fraud, which is the intentional misrepresentation of a food's true qualities, not only harms buyers but also undermines confidence in entire market segments. Worldwide coffee production has had a rising trend despite some setbacks in recent years. Global consumption is also increasing and has only been slightly attenuated by phases of economic weakness. For example, the appetite for coffee in Germany has been growing over the years, with an average consumption of 450 cups per person in 2022, which is equivalent to 5.4 kg of coffee. The top coffee-loving countries consume around 10 kg of coffee per person per year. The rising demand for higher quality coffee with declared origin, botanical variety, and/or processing methods, combined with the significantly higher market prices for such specialty coffee, are opportunities for food fraudsters. In addition to compliance visits to production and processing sites and to auditing a company's accounting, well-established standardised and efficient laboratory analyses are an important part in fighting food fraud. As a metrological primary method of measurement, nuclear magnetic resonance spectrometry (NMR) has been increasingly used for routine chemical quantitative analysis. The NMR spectra typically show very good signal resolution, excellent reproducibility, and linearity of response independent of the substance. NMR can record signals from most metabolites in a biological sample with a single experiment in just a few minutes. Thus, NMR has a high potential to provide reliable data for the analysis of complex mixtures, such as food extracts. NMR spectra can be used as fingerprints to compare individual samples against databases of authentic references using multivariate analysis. This talk will present recent research on the potential of using NMR with targeted, quantitative analysis and also with non-targeted multivariate analysis to verify several product claims on roasted coffee, i.e. the geographical origin, botanical variety, and farming method (organic/conventional). By using targeted analysis, over a dozen characteristic substances can be quantified with good precision. The chemometrical evaluation of NMR spectra can raise reasonable suspicion about the geographical origin. [ABSTRACT FROM AUTHOR]

Inositol phosphates (IPs) are a major pool of identifiable organic phosphorus (P) in soil. However, insight into their distribution and cycling in soil remains limited, particularly of lower-order IP (IP 5 and IP 4). This is because the quantification of lower-order IP typically requires a series of chemical extractions, including hypobromite oxidation to isolate IP, followed by chromatographic separation. Here, for the first time, we identify the chemical nature of organic P in four soil extracts following hypobromite oxidation using solution 31 P NMR spectroscopy and transverse relaxation (T2) experiments. Soil samples analysed include A horizons from a Ferralsol (Colombia), a Cambisol and a Gleysol from Switzerland, and a Cambisol from Germany. Solution 31 P nuclear magnetic resonance (NMR) spectra of the phosphomonoester region in soil extracts following hypobromite oxidation revealed an increase in the number of sharp signals (up to 70) and an on average 2-fold decrease in the concentration of the broad signal compared to the untreated soil extracts. We identified the presence of four stereoisomers of IP 6 , four stereoisomers of IP 5 , and scyllo -IP 4. We also identified for the first time two isomers of myo -IP 5 in soil extracts: myo -(1,2,4,5,6)-IP 5 and myo -(1,3,4,5,6)-IP 5. Concentrations of total IP ranged from 1.4 to 159.3 mg P per kg soil across all soils, of which between 9 % and 50 % were comprised of lower-order IP. Furthermore, we found that the T2 times, which are considered to be inversely related to the tumbling of a molecule in solution and hence its molecular size, were significantly shorter for the underlying broad signal compared to for the sharp signals (IP 6) in soil extracts following hypobromite oxidation. In summary, we demonstrate the presence of a plethora of organic P compounds in soil extracts, largely attributed to IPs of various orders, and provide new insight into the chemical stability of complex forms of organic P associated with soil organic matter. [ABSTRACT FROM AUTHOR]

Stable carbon (C) and nitrogen (N) isotope ratios of sedimentary organic matter (OM) can reflect the biogeochemical history of aquatic ecosystems. However, diagenetic processes in sediments may alter isotope records of OM via microbial activity and preferential degradation of isotopically distinct organic components. This study investigated the isotope alteration caused by preferential degradation in surface sediments sampled from a eutrophic reservoir in Germany. Sediments were treated sequentially with hot water extraction, hydrochloric acid hydrolysis, hydrogen peroxide oxidation and di-sodium peroxodisulfate oxidation to chemically simulate preferential degradation pathways of sedimentary OM. Residue and extracts from each extraction step were analyzed using elemental analyzer-isotope ratio mass spectrometry and solid-state 13C nuclear magnetic resonance spectroscopy. Our results show that stable C and N isotope ratios reacted differently to changes in the biochemical composition of sedimentary OM. Preferential degradation of proteins and carbohydrates resulted in a 1.2‰ depletion of 13C, while the isotope composition of 15N remained nearly the same. Sedimentary δ15N values were notably altered when lignins and lipids were oxidized from residual sediments. Throughout the sequential fractionation procedure, δ13C was linearly correlated with the C:N of residual sediments. This finding demonstrates that changes in biochemical composition caused by preferential degradation altered δ13C values of sedimentary OM, while this trend was not observed for δ15N values. Our study identifies the influence of preferential degradation on stable C isotope ratios and provide additional insight into the isotope alteration caused by post-depositional processes. [ABSTRACT FROM AUTHOR]

In June 2018, 15 'Spice-like' herbal products from German language internet shops were analyzed. In total, three different synthetic cannabinoids (SCs) were identified by gas chromatography-mass spectrometry (GC-MS). Two of the active ingredients were identified as the recently described 5F-ADB and Cumyl-PeGaClone. The third compound was identified as the so far unknown SC 5F-Cumyl-PeGaClone. 5F-Cumyl-PeGaClone was subject to an in-depth characterization by nuclear magnetic resonance spectroscopy (NMR), electron ionization mass spectrometry (EI-MS), electrospray ionization tandem mass spectrometry (ESI-MS/MS), infrared and uItraviolet-visible spectroscopy (IR and UV/Vis). In addition, all SCs in all products were quantified by a GC-MS method using JWH-018 as internal standard and corresponding response factors. While Cumyl-PeGaClone and 5F-ADB were detected in one, respectively two products, the newly identified 5F-Cumyl-PeGaClone was detected as the only active ingredient in the remaining twelve products. The SC content ranged from 14.7 to 76.2mg/g (average: 32.1mg/g). [ABSTRACT FROM AUTHOR]

Wildfires change the chemical composition of soil organic matter (SOM). Since the effects of fires on organic matter (OM) in soil solution are largely unknown, we sought to compare the quality of dissolved organic matter (DOM) and total organic matter (TOM = DOM + particulate OM) between burned and control sites. The sites were subjected to a low-intensity surface fire in a coniferous forest in Germany dominated by spodic Cambisols derived from Triassic sandstone. Soil solutions from three different soil horizons (O, Ah, Bw), and throughfall (TF) were analyzed using solid-state 13 C NMR spectroscopy, allowing us to track the initial fire impact on OM vertically through the soil profile and 70 days after the fire. In addition, organic layer samples were analyzed by 13 C NMR spectroscopy to compare the OM quality. Under control conditions, properties of SOM influence the chemical composition of DOM and TOM in soil solutions. However, with fire, there is an initial increase in aromatic C in SOM, but not in DOM and TOM. Seventy days after the fire treatment, the aromatic C fraction in soil solutions of O and Ah layers increased, possibly due to accelerated oxidation processes, which would make the aromatic C more water-soluble. Our findings highlight the importance of short-term low-intensity fire-induced changes on forest soils that are useful to those seeking to better understand and model the temporal variability in the response of soil chemistry to fire to improve our knowledge of TOM and DOM dynamics in soils. [ABSTRACT FROM AUTHOR]

In February 2016, nine "spice-like" products from German language internet shops were analyzed. In total, eight different synthetic cannabinoids were identified by gas chromatography-mass spectrometry (GC-MS), namely THJ-018, THJ-2201, MAB-CHMINACA, 5F-ADB, 5Cl-AKB48 (syn.: 5C-AKB48), 4-pentenyl-AKB48, MDMB-CHMICA and 5F-AB-PINACA. For the majority of products only one synthetic cannabinoid was identified as the active ingredient, while two products contained 2 and 5 compounds, respectively. For some of the identified cannabinoids (MAB-CHMINACA, 5Cl-AKB48 and 4-pentenyl-AKB48) no or only insufficient physico-chemical data were available in literature. To our knowledge 5Cl-AKB48 and 4-pentenyl-AKB48 were found for the first time in commercially available products, hence an in-depth characterization of these compounds by NMR, EI-MS, ESI-MS/MS, IR- and UV spectroscopy was conducted. In addition, all synthetic cannabinoids were quantified by a GC-MS method using JWH-018 as internal standard and the corresponding response factors to calculate the total amount of all synthetic cannabinoids in the commercial smoking mixtures. The content of synthetic cannabinoids in the investigated products ranged from 23 to 120mg/g (average: 57mg/g), while individual compounds ranged from 1 to 120mg/g. [ABSTRACT FROM AUTHOR]

Background: Numerous observational studies have observed associations between vitamin D deficiency and cardiometabolic diseases, but these findings might be confounded by obesity. A characterization of the metabolic profile associated with serum 25-hydroxyvitamin D [25(OH)D] levels, in general and stratified by abdominal obesity, may help to untangle the relationship between vitamin D, obesity and cardiometabolic health.Methods: Serum metabolomics measurements were obtained from a nuclear magnetic resonance spectroscopy (NMR)- and a mass spectrometry (MS)-based platform. The discovery was conducted in 1726 participants of the population-based KORA-F4 study, in which the associations of the concentrations of 415 metabolites with 25(OH)D levels were assessed in linear models. The results were replicated in 6759 participants (NMR) and 609 (MS) participants, respectively, of the population-based FINRISK 1997 study.Results: Mean [standard deviation (SD)] 25(OH)D levels were 15.2 (7.5) ng/ml in KORA F4 and 13.8 (5.9) ng/ml in FINRISK 1997; 37 metabolites were associated with 25(OH)D in KORA F4 at P < 0.05/415. Of these, 30 associations were replicated in FINRISK 1997 at P < 0.05/37. Among these were constituents of (very) large very-low-density lipoprotein and small low-density lipoprotein subclasses and related measures like serum triglycerides as well as fatty acids and measures reflecting the degree of fatty acid saturation. The observed associations were independent of waist circumference and generally similar in abdominally obese and non-obese participants.Conclusions: Independently of abdominal obesity, higher 25(OH)D levels were associated with a metabolite profile characterized by lower concentrations of atherogenic lipids and a higher degree of fatty acid polyunsaturation. These results indicate that the relationship between vitamin D deficiency and cardiometabolic diseases is unlikely to merely reflect obesity-related pathomechanisms. [ABSTRACT FROM AUTHOR]

Background: Impaired energy metabolism is a possible mechanism that contributes to insulin resistance and ectopic fat storage. Objective: We examined whether meal ingestion differently affects hepatic phosphorus metabolites in insulin-sensitive and insulin-resistant humans. Design: Young, lean, insulin-sensitive humans (CONs) [mean ± SD body mass index (BMI; in kg/m²): 23.2 ± 1.5]; insulin-resistant, glucose-tolerant, obese humans (OBEs) (BMI: 34.3 ± 1.7); and type 2 diabetes patients (T2Ds) (BMI: 32.0 ± 2.4) were studied (n = 10/group). T2Ds (61 ± 7 y old) were older (P < 0.001) than were OBEs (31 ± 7 y old) and CONs (28 ± 3 y old). We quantified hepatic γATP, inorganic phosphate (Pi), and the fat content [hepa-tocellular lipids (HCLs)] with the use of 31P/¹H magnetic resonance spectroscopy before and at 160 and 240 min after a high-caloric mixed meal. In a subset of volunteers, we measured the skeletal muscle oxidative capacity with the use of high-resolution respirom-etry. Whole-body insulin sensitivity (M value) was assessed with the use of hyperinsulinemic-euglycemic clamps. Results: OBEs and T2Ds were similarly insulin resistant (M value: 3.5 ± 1.4 and 1.9 ± 2.5 mg ⋅ kg-1 ⋅ min-1, respectively; P = 0.9) and had 12-fold (P = 0.01) and 17-fold (P = 0.002) higher HCLs, respectively, than those of lean persons. Despite comparable fasting hepatic γATP concentrations, the maximum postprandial increase of γATP was 6-fold higher in OBEs (0.7 ± 0.2 mmol/L; P = 0.03) but only tended to be higher in T2Ds (0.6 ± 0.2 mmol/L; P = 0.09) than in CONs (0.1 ± 0.1 mmol/L). However, in the fasted state, muscle complex I activity was 53% lower (P = 0.01) in T2Ds but not in OBEs (P = 0.15) than in CONs. Conclusions: Young, obese, nondiabetic humans exhibit augmented postprandial hepatic energy metabolism, whereas elderly T2Ds have impaired fasting muscle energy metabolism. These findings support the concept of a differential and tissue-specific regulation of energy metabolism, which can occur independently of insulin resistance. This trial was registered at clinicaltrials.gov as NCT01229059. [ABSTRACT FROM AUTHOR]

Abstract: In absence of commercial fertilizers prehistoric agriculture relied heavily on nutrient supply from soil. This study was designed to reconstruct the phosphorus (P) status of prehistoric arable soils in order to highlight the possible importance of soil P limitation in Neolithic (after the Early Neolithic, i.e. around 4400 until 2200BC) and Bronze Age (2200 until 700BC) agriculture. For this purpose, we sampled buried archaeological topsoil relicts that have been preserved in prehistoric pit fillings outside ancient settlements in the loess areas in Central and Western Germany. Adjacent subsoils and recent topsoils served as references. Samples were characterized using sequential P extraction and selected samples were characterized using 31P NMR spectroscopy. Prehistoric topsoil relicts in the investigated regions showed larger contents of organic matter and extractable P (sum of all sequentially extracted inorganic and organic P fractions) than the adjacent subsoils. Sampling the soils at higher depth resolution did not provide any evidence of P-leaching. The P content in the topsoil relicts amounted to approximately 86% of the P content of the modern, fertilized topsoils. Most of the extractable P (>80%) comprised inorganic P. Organic P fractions were dominated by monoester-P. Intriguingly, plant available P contents (sum of resin-Pi, NaHCO3-Pi and NaOH-Pi) in the prehistoric topsoils and the recent topsoils were similar (23% and 20% of extractable P, respectively), suggesting that even plant available P was maintained in the prehistoric topsoil relicts. Also the contents of Ca-associated P were large, but reflected differences in pedogenesis among the sampling sites (Chernozem, Phaeozem and Luvisol). Hence, we have to conclude that there was no significant P limitation in the prehistoric farmland of the two loess areas, either because the soils had been fertilized or because the inherent P stocks were sufficient to sustain ancient farm yields. In any case our data do not support the hypothesis that prehistoric P limitations may have reduced crop yields. [Copyright &y& Elsevier]

It was demonstrated previously that polar and non-polar surface extracts of the brown alga Fucus vesiculosus collected during winter from the Kiel Bight (Germany) inhibited bacterial attachment at natural concentrations. The present study describes the bioassay-guided identification of the active metabolites from the polar fraction. Chromatographic separation on a size-exclusion liquid chromatography column and bioassays identified an active fraction that was further investigated using nuclear magnetic resonance spectroscopy and mass spectrometry. This fraction contained the metabolites dimethylsulphopropionate (DMSP), proline and alanine. DMSP and proline caused the anti-attachment activity. The metabolites were further quantified on the algal surface together with its associated boundary layer. DMSP and proline were detected in the range 0.12–1.08 ng cm−2 and 0.09–0.59 ng cm−2, respectively. These metabolites were tested in the concentration range from 0.1 to 1000 ng cm−2 against the attachment of five bacterial strains isolated from algae and sediment co-occurring with F. vesiculosus. The surface concentrations for 50% inhibition of attachment of these strains were always <0.38 ng cm−2 for DMSP and in four cases <0.1 ng cm−2 for proline, while one strain required 1.66 ng cm−2 of proline for 50% inhibition. Two further bacterial strains that had been directly isolated from F. vesiculosus were also tested, but proved to be the least sensitive. This study shows that DMSP and proline have an ecologically relevant role as surface inhibitors against bacterial attachment on F. vesiculosus. [ABSTRACT FROM AUTHOR]

Abstract: Four new pyrenocines, named pyrenocines J–M (1–4), were isolated from an endophytic fungus, Phomopsis sp, by a bioassay-guided method. The structures of the new compound have been assigned from 1H and 13C NMR spectra, DEPT, and by 2D COSY, HMQC, and HMBC experiments. Preliminary studied showed that compounds 1, 2 and 4 showed good antifungal, antibacterial, and algicidal properties, while compound 3 had good antibacterial and algicidal properties. [Copyright &y& Elsevier]

Background: Red yeast rice (i.e., rice fermented with Monascus spp.), as a food supplement, is claimed to be blood cholesterol-lowering. The red yeast rice constituent monacolin K, also known as lovastatin, is an inhibitor of the hydroxymethylglutaryl-CoA (HMG-CoA) reductase. This article aims to develop a sensitive nuclear magnetic resonance (NMR) method to determine the total statin content of red yeast rice products. Methods: The total statin content was determined by a 400 MHz 1H NMR spectroscopic method, based on the integration of the multiplet at &#948 5.37-5.32 ppm of a hydrogen at the hexahydronaphthalene moiety in comparison to an external calibration with lovastatin. The activity of HMG-CoA reductase was measured by a commercial spectrophotometric assay kit. Results: The NMR detection limit for total statins was 6 mg/L (equivalent to 0.3 mg/capsule, if two capsules are dissolved in 50 mL ethanol). The relative standard deviations were consistently lower than 11%. The total statin concentrations of five red yeast rice supplements were between 1.5 and 25.2 mg per specified daily dose. A dosedependent inhibition of the HMG-CoA reductase enzyme activity by the red yeast rice products was demonstrated. Conclusion: A simple and direct NMR assay was developed to determine the total statin content in red yeast rice. The assay can be applied for the determination of statin content for the regulatory control of red yeast rice products. [ABSTRACT FROM AUTHOR]

Abstract: This study presents and discusses the infrared spectroscopic, the nuclear magnetic resonance spectroscopic and mass spectrometric data of the designer drug 3,4 methylenedioxypyrrolidinobutyrophenone (MDPBP), a homolog of 3,4 methylenedioxypyrovalerone (MDPV). MDPBP was first seized in Germany in the year 2009. The structure elucidation of the aliphatic part of MDPBP was carried out by product ion spectrometry of the immonium ion with m/z=112 formed after electron ionization, and by one- and two-dimensional 1H- and 13C NMR spectroscopy. [Copyright &y& Elsevier]

Abstract: Aim of the study: In a preliminary screen of extracts from plants used as antimalarial remedies used in Europe in the 16th and 17th, the ethyl acetate extract of Alisma plantago-aquatica L. (Alismataceae) was active against Plasmodium falciparum K1 strain with 77% growth inhibition at 4.9μg/ml. The aim of this study was to isolate and identify the substances responsible for this antiplasmodial activity. Materials and methods: With HPLC-based activity profiling in combination with HPLC hyphenated methods (HPLC–PDA, –MSn, HR–MS, and off-line microprobe NMR) the activity was assigned to time windows, and the substances contained therein were characterised chemically. The active compounds were isolated with semi-preparative HPLC and structures were elucidated with high resolution mass spectrometry, and 1D and 2D NMR spectroscopy. Results: Four compounds were isolated and identified as protostane triterpenoids alisol A, alisol B 11-monoacetate, alisol B 23-monoacetate, and alisol G. Their IC 50s against Plasmodium falciparum ranged from 5.4 to 13.8μM. Conclusions: This is the first report of antiplasmodial activity from protostanes triterpenoids, and the first result of our ongoing project of screening for antiprotozoal natural products from remedies used in European renaissance medicine. [Copyright &y& Elsevier]

Abstract: In 2008, some 900 cases of adverse events associated with the use of heparin were reported to the Food and Drug Administration of USA and the Federal Institute of Drugs and Medical Devices in Germany. 238 patients died from heparin in the USA. In March 2008, oversulfated chondroitin sulfate (OSCS) was identified to be responsible for these cases. NMR spectroscopic evaluation of heparin samples revealed OSCS, dermatan sulfate (DS), chondroitin sulfate A and C as well as various residual solvents to be present in heparin batches, which could not be identified by means of conventional methods described in various pharmacopoeias at that time. In order to evaluate the situation on the German market, 145 representative samples were collected in 2008 and analyzed by means of 1H NMR spectroscopy, water determination, optical rotation and sheep plasma clotting assay. 66 samples were found to contain pure heparin, 51 samples heparin plus DS, 5 samples heparin plus OSCS, and 23 samples heparin, DS and OSCS, each in varying amounts. In 94 out of 145 batches especially ethanol was found in strongly varying amounts up to about 9.5%. Traces of acetone and formic acid were found with concentrations up to 0.04%, as well as sodium acetate and methanol up to 0.5%. Additionally, in many batches the content of water was found to be relatively high. Whereas the optical rotation was able to identify samples with a high contamination of OCSC, all samples tested fulfilled the requirements of the anticoagulation potency assay of the European Pharmacopoeia 6.0. The presented analysis of a representative set of heparin samples proves the suitability of 1H NMR spectroscopy for the quality control of heparin of both glycosaminoglycans and residual solvents. [Copyright &y& Elsevier]

Abstract: On January 22nd 2009, the German Health Authorities prohibited several non-traditional cannabinoids, that proved to be the active components in popular “Bio-Designer-Drugs” like “Spice” and analogous products. The recent detection of CP 47,497-C8 in Europe and Japan documents that these products have already spread world wide. We synthesized several potentially interesting alkylaminoindoles (alkylchain C3 to C7) and isolated CP 47,497-C8 from “Spice Gold”. The compounds were purified and characterized by NMR and mass spectrometry methods. With the aid of these authentic references we were able to detect and quantify added psychoactive compounds in different herbal blends. All samples that were acquired before the prohibition in December 2008 contained either CP 47,497-C8 (5.4–11.0mg/g) or JWH-018 (2.3mg/g). Some samples acquired in March 2009, 4 weeks after the prohibition took place, still contained CP 47,497-C8 (3.0–3.3mg/g) but JWH-018 was not detected anymore. Instead it was replaced by its non-regulated C4-homolog JWH-073 (5.8–22.9mg/g). Furthermore some of the new products did not contain any non-traditional cannabinoids. To our knowledge this is the first report of the appearance JWH-073 as a new designer drug. The data and method presented here will facilitate and accelerate the detection of these compounds in complex matrices. [Copyright &y& Elsevier]

This article discusses the microbial biodegradation of organic wastes in landfill in Bavaria, Southern Germany. The authors analyzed the chemical composition, degree of transformation and moisture content using carbon isotope nuclear magnetic resonance spectroscopy for carbohydrates, lipids, proteins and lignins. According to the authors, chemical and spectroscopic variables indicate a generally low extent of transformation and biodegradation at all sites. More than half of the carbohydrate organic matter showed a high potential for methane emissions and energy production. They recommend seepage water cleaning and recirculation systems to optimize moisture contents for energy production.

1H NMR spectroscopy coupled with in situ laser irradiation has been used together with density functional theory (DFT) computation to examine the structures of the photoisomers of a series of sulfonated reactive azo dyes. Assignment of 1H NMR spectra acquired at the photostationary state has allowed, for the first time, NMR characterisation of unstable cis isomers of commercially relevant water-soluble azo dyes. Structural features of the two isomeric forms predicted by DFT calculations are clearly reflected in the experimental NMR data. The trans–cis photoisomerisation process could be unambiguously identified in each case, based on the large chemical shift change observed for resonances associated with aromatic protons adjacent to the azo linkage. [ABSTRACT FROM AUTHOR]

We describe a laser spectroscopy station that has been proposed to exploit the high yields of radioactive beams at the future FAIR facility at GSI, Darmstadt. Exotic nuclei produced in the Super-Fragment-Recoil-Separator (S-FRS) are stopped in a gas cell, extracted, reaccelerated and transported to the LaSpec setup. Here, collinear spectroscopy on ions and atoms, β-NMR experiments or laser-desorbed resonance ionization can be applied to these rare isotopes. [ABSTRACT FROM AUTHOR]

Unlabelled: Treatment of hyperphenylalaninaemias due to phenylalanine hydroxylase deficiency with a low phenylalanine (Phe) diet is highly successful in preventing neurological impairment and mental retardation. There is consensus that, for an optimal outcome, treatment should start as early as possible, and that strict blood Phe level control is of primary importance during the first years of life, but for adolescent and adult patients international treatment recommendations show a great variability. A working party of the German Working Group for Metabolic Diseases has evaluated research results on IQ data, speech development, behavioural problems, educational progress, neuropsychological results, electroencephalography, magnetic resonance imaging, and clinical neurology. Based on the actual knowledge, recommendations were formulated with regard to indication of treatment, differential diagnosis, and Phe level control during different age periods. The development of the early-and-strictly-treated patient in middle and late adulthood still remains to be investigated. Therefore, the recommendations should be regarded as provisional and subject to future research. Efficient treatment of phenylketonuria has to go beyond recommendations for blood Phe level control and must include adequate dietary training, medical as well as psychological counselling of the patient and his family, and a protocol for monitoring outcome.Conclusions: Early-and-strictly-treated patients with phenylketonuria show an almost normal development. During the first 10 years treatment should aim at blood Phenylalanine levels between 40 and 240 micromol/L. After the age of 10, blood phenylalanine level control can be gradually relaxed. For reasons of possible unknown late sequelae, all patients should be followed up life-long. [ABSTRACT FROM AUTHOR]

1H NMR spectroscopy, in combination with chemometric methods, was used to analyze the methanol/acetonitrile (1:1) extract of walnut (Juglans Regia L.) regarding the geographical origin of 128 authentic samples from different countries (France, Germany, China) and harvest years (2016–2019). Due to the large number of different metabolites within the acetonitrile/methanol extract, the one-dimensional (1D) 1H NOESY (nuclear Overhauser effect spectroscopy) spectra suffer from strongly overlapping signals. The identification of specific metabolites and statistical analysis are complicated. The use of pure shift 1H NMR spectra such as PSYCHE (pure shift yielded by chirp excitation) or two-dimensional ASAP-HSQC (acceleration by sharing adjacent polarization-heteronuclear single quantum correlation) spectra for multivariate analysis to determine the geographical origin of foods may be a promising method. Different types of NMR spectra (1D 1H NOESY, PSYCHE, and ASAP-HSQC) were acquired for each of the 128 walnut samples and the results of the statistical analysis were compared. A support vector machine classifier was applied for differentiation of samples from Germany/China, France/Germany, and France/China. The models obtained by conduction of a repeated nested cross-validation showed accuracies from 58.9% (±1.3%) to 95.9% (±0.8%). The potential of the 1H-13C HSQC as a 2D NMR experiment for metabolomics studies was shown. [ABSTRACT FROM AUTHOR]

The objective of this study was to compare the physicochemical, enzymatic, and metabolic properties of two control wheat malts imported from Germany and the US to those of malts made from three Korean wheat varieties: Triticumaestivum L., var. Anzunbaengi, Jokyung, and Keumkang. The qualities and enzyme activities of the Korean wheat malts were generally similar to those of the control wheat malts. The Korean wheat malts had slightly lower diastatic power and enzyme activities related to saccharification. The analysis of metabolites in the wheat malt samples was performed using 1H nuclear magnetic resonance (NMR) metabolomics, which identified 32 metabolites that differed significantly among the samples. Most amino acids and lipids were more abundant in the Korean wheat malts than in the control wheat malts. These differences among malts could influence the quality and flavor of wheat beers. Further brewing studies are necessary to identify the association between beer quality and individual malt metabolites. [ABSTRACT FROM AUTHOR]

Objectives: Face painting in the colours of the national flags has become a mass phenomenon during international mega sporting events. Face paints, belonging to the group of lipophilic decorative cosmetics, pose an analytical challenge, especially in the sample preparation steps to obtain sample extracts of the colouring agents of low solubility., Methods: In the context of official cosmetics control, a sample of German flag-coloured face paints (n = 42) offered during the soccer world cup 2014 was analysed. Sample-clean-up of hydroalcoholic and dichloromethane sample extracts was conducted using preparative thin-layer chromatography (TLC). For identification, analytical TLC, spectrophotometry considering bathochromic effects, and high-performance liquid chromatography (LC) with diode array detector were applied. Nuclear magnetic resonance (NMR) spectroscopy and LC-tandem mass spectrometry (LC-MS/MS) were used in positive cases for confirmatory analysis. NMR spectroscopy was also applied to determine the identity and purity of reference substances. Risk assessment was provided using the margin of exposure (MOE) methodology., Results: The prohibited red colouring agent CI 15585 (D&C Red No. 9, Pigment Red 53:1), which is carcinogenic in animals, was positively identified in 40% of the analysed samples. Per face painting event, about 0.04 mg kg(-1) bw (adult) or 0.11 mg kg(-1) bw (child) of CI 15585 is systemically absorbed. Assuming an annual use of five times (adult) or 20 times (child), the exposure would be 5.8E-04 mg kg(-1) bw per day (adult) or 5.8E-03 mg kg(-1) bw per day (child). The MOE in these worst-case scenarios would be 6871 (adult) and 695 (child). Because the mechanism of CI 15585 is non-genotoxic and the MOE is higher than a safety factor of 100, CI 15585 does not pose a serious health risk to the consumer, but should be avoided for reasons of precautionary public health protection., Conclusion: An analytical strategy to determine colouring agents in face paints was developed and non-compliance with the European Union (EU) cosmetic products regulation in a considerable number of products was detected. An increased control frequency especially at the points of entry into the EU is recommended., (© 2014 Society of Cosmetic Scientists and the Société Française de Cosmétologie.)

The article focuses on the use of nuclear magnetic resonance (NMR) spectroscopy in forests. Stephan Appelt, a scientist, and his colleagues took their homemade NMR spectrometers into a forest in Germany. The new instrument proved to be more simple and useful than the previous earth's field NMR spectrometers. The earth's magnetic field is very weak, and cannot polarize magnetic spins for NMR. So, in order to produce a measurable signal, spins must be prepolarized. Appelt used a Halbach magnet to prepolarize the nuclear spins. The main limitation of earth's field spectroscopy is the presence of stray magnetic fields. Appelt and colleagues decided to perform their experiments in a forest, because of the presence of destructive stray magnetic fields in human environments. In laboratories, there is a need to shield against the stray magnetic fields, which is not there in the case of forests. In earth's field NMR, lithium is difficult to study because of its low signal. The researchers detected lithium for the first time by the earth's field NMR. They proposed that due to the high sensitivity of lithium's relaxation time to temperature and concentration, earth's field NMR could be used to generate a map of neuron channels in the brain.