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 (Mw) 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. Despite the immense resolution difference between high-field and low-field NMR instruments, the results demonstrate that the calibration transfer from high- to low-field is feasible in the case of a physical property, namely, the molecular weight, achieving validation errors close to the original calibration (down to only 1.2 times higher root mean square errors). These results introduce new perspectives for applications of benchtop NMR, in which existing calibrations from expensive high-field instruments can be transferred to cheaper benchtop instruments to economize.

The qNMR Summit 5.0: Proceedings and Status of qNMR Technology.

The goal of the qNMR Summit is to take stock of the status quo and the recent developments in qNMR research and applications in a timely and accurate manner. It provides a platform for both advanced and novice qNMR practitioners to receive a well-rounded update and discuss potential qNMR-related applications and collaborations. For over a decade, scientists from academia, industry, nonprofit institutions, and governmental bodies have focused on the standardization of qNMR methodology, as well as its metrological and pharmacopeial utility. This paper reviews key content of qNMR Summits 1.0 to 4.0 and puts into perspective the outcomes and available transcripts of the October 2019 Summit 5.0, with attendees from the United States, Canada, Japan, Korea, and several European countries. Summit presentations focused on qNMR methodology in the pharmaceutical industry, advanced quantitation algorithms, and promising developments.

Lignins Isolated via Catalyst-Free Organosolv Pulping from Miscanthus x giganteus, M. sinensis, M. robustus and M. nagara: A Comparative Study.

As a low-input crop, Miscanthus offers numerous advantages that, in addition to agricultural applications, permits its exploitation for energy, fuel, and material production. Depending on the Miscanthus 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 M. x giganteus, M. sinensis, M. robustus and M. nagara using a catalyst-free organosolv pulping process. The lignins from different plant constituents are also compared regarding their similarities and differences regarding monolignol ratio and important linkages. Results showed that the plant genotype has the weakest influence on monolignol content and interunit linkages. In contrast, structural differences are more significant among lignins of different harvest time and/or season. Analyses were performed using fast and simple methods such as nuclear magnetic resonance (NMR) spectroscopy. Data was assigned to four different linkages (A: ß-O-4 linkage, B: phenylcoumaran, C: resinol, D: ß-unsaturated ester). In conclusion, A content is particularly high in leaf-derived lignins at just under 70% and significantly lower in stem and mixture lignins at around 60% and almost 65%. The second most common linkage pattern is D in all isolated lignins, the proportion of which is also strongly dependent on the crop portion. Both stem and mixture lignins, have a relatively high share of approximately 20% or more (maximum is M. sinensis Sin2 with over 30%). In the leaf-derived lignins, the proportions are significantly lower on average. Stem samples should be chosen if the highest possible lignin content is desired, specifically from the M. x giganteus genotype, which revealed lignin contents up to 27%. Due to the better frost resistance and higher stem stability, M. nagara offers some advantages compared to M. x giganteus. Miscanthus crops are shown to be very attractive lignocellulose feedstock (LCF) for second generation biorefineries and lignin generation in Europe.

Qualitative and quantitative 1 H NMR spectroscopy for determination of divalent metal cation concentration in model salt solutions, food supplements, and pharmaceutical products by using EDTA as chelating agent.

This paper introduces an 1 H NMR method to identify individual divalent metal cations Be2+ , Mg2+ , Ca2+ , Sr2+ , Zn2+ , Cd2+ , Hg2+ , Sn2+ , and Pb2+ in aqueous salt solutions through their unique signal shift and coupling after complexation with the salt of ethylenediaminetetraacetic acid (EDTA). Furthermore, quantitative determination applied for the divalent metal cations Ca2+ , Mg2+ , Hg2+ , Sn2+ , Pb2+ , and Zn2+ (limit of quantification: 5-22 µg/ml) can be achieved using an excess of EDTA with aqueous model salt solutions. An internal standard is not required because a known excess of EDTA is added and the remaining free EDTA can be used to recalculate the quantity of chelated metal cations. The utility of the method is demonstrated for the analysis of divalent cations in some food supplements and in pharmaceutical products.

Collaborative Study to Validate Purity Determination by 1H Quantitative NMR Spectroscopy by Using Internal Calibration Methodology.

NMR spectroscopy has recently been utilized to determine the absolute amounts of organic molecules with metrological traceability since signal intensity is directly proportional to the number of each nucleus in a molecule. The NMR methodology that uses hydrogen nucleus (1H) to quantify chemicals is called quantitative 1H-NMR (1H qNMR). The quantitative method using 1H qNMR for determining the purity or content of chemicals has been adopted into some compendial guidelines and official standards. However, there are still few reports in the literature regarding validation of 1H qNMR methodology. Here, we coordinated an international collaborative study to validate a 1H qNMR based on the use of an internal calibration methodology. Thirteen laboratories participated in this study, and the purities of three samples were individually measured using 1H qNMR method. The three samples were all certified via conventional primary methods of measurement, such as butyl p-hydroxybenzoate Japanese Pharmacopeia (JP) reference standard certified by mass balance; benzoic acid certified reference material (CRM) certified by coulometric titration; fludioxonil CRM certified by a combination of freezing point depression method and 1H qNMR. For each sample, 1H qNMR experiments were optimized before quantitative analysis. The results showed that the measured values of each sample were equivalent to the corresponding reference labeled value. Furthermore, assessment of these 1H qNMR data using the normalized error, En-value, concluded that statistically 1H qNMR has the competence to obtain the same quantification performance and accuracy as the conventional primary methods of measurement.

Effect of natural antioxidants on the physicochemical properties and stability of freeze-dried microencapsulated chia seed oil.

BACKGROUND: Chia oil possesses a very high content of polyunsaturated fatty acids, mainly α-linolenic acid. This characteristic makes this oil possess beneficial properties to health but gives it a high susceptibility to the oxidation process. Microencapsulation and the addition of natural antioxidants are alternatives to protect chia oil against oxidative deterioration. The aim of this study was to investigate the physicochemical characteristics and the oxidative stability of chia seed oil microencapsulated with different natural antioxidants (Guardian Chelox, which is a commercial blend of extracts from chamomile and rosemary, and essential oils from Origanum vulgare, Origanum x majoricum, and Mentha spicata) by freeze-drying using sodium caseinate and lactose as wall materials. RESULTS: The main physicochemical properties of the microencapsulated chia oil were similar regardless of the presence of antioxidant. The moisture content was 38.1 ± 4.0 g kg-1 ; the microencapsulation efficiency was higher than 85% in all cases. The freeze-drying microencapsulation significantly enhanced (P ≤ 0.05) the oxidative stability of the chia oil. The addition of natural antioxidants conferred chia oil additional protection against lipid oxidation, depending on the type and concentration (500 or 1000 mg kg-1 of the emulsion previous to freeze-drying) of the antioxidant. Among them, Guardian Chelox (1000 mg kg-1 ), presented the highest induction time obtained by the Rancimat accelerated oxidative stability test and the lowest peroxide values after 90 days of storage (33% relative humidity, 25 ± 2 °C). Overall, the microparticles with antioxidants presented a lower degree of yellowing during storage than the control system. CONCLUSION: The use of different natural antioxidants confers freeze-dried microencapsulated chia seed oil additional protection against lipid oxidation. This information is relevant for the application of this oil, which is a rich source of omega-3 fatty acids, in the food industry. © 2018 Society of Chemical Industry.

Automated multicomponent phospholipid analysis using 31P 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. Automated routines were written in MATLAB environment for quantification of phosphatidylcholine (PC), phosphatidylinositol (PI), lyso-phosphatidylcholine (LPC), phosphatidylserine (PS), phosphatidylethanolamine (PE), diphosphatidylglycerol or cardiolipin (DPG), phosphatidylglycerol (PG), and lyso-phosphatidylethanolamine (LPE) in lecithin and of PC, PC-ether, LPC, PE, N-acyl phosphatidylethanolamine (APE), and LPE in krill oil matrix. The routine includes NMR spectra import, extraction of data points, peaking of local minima and local maxima in the data, integration, quantitation against internal standard, reporting of results as Word file, and their importing in our internal database. Our extensive studies on a representative set of more than 1000 lecithin (soy, rape, sunflower) and krill samples showed that the routine can automatically and accurately calculate the concentrations of all PLs. No systematic or proportional differences between automated and manual evaluation were detected. The developed automated program produces accurate results and requires less than 5 s for each analysis. This tool is already used in high-throughput PL analysis of krill and lecithin and will be adjusted to other matrices (egg, milk, chocolate, etc.) as well.

Monitoring daily routine performance in quantitative NMR (qNMR) spectroscopy: Is the system suitability test necessary?

Nuclear magnetic resonance spectrometry (NMR) finds numerous applications in pharmacy, cosmetic, and food control as well as in developing tools for "big data" analysis. However, there remains a need for automated tools to assess instrument system suitability in real time for each particular routine sample. An automated procedure has been introduced to monitor a number of characteristics (resolution, symmetry, and half width) in real time after the measurement of two samples distributed by the vendor (0.3% CHCl3 in acetone-d6 with tetramethylsilane and 2 mM sucrose in H2 O-D2 O). The results over 11 months were discussed in terms of average values, standard deviations, and spectrometer variability. Moreover, multivariate statistical procedure was implemented to evaluate metrics generated from three NMR spectrometers. Performance of three NMR spectrometers (500 MHz with BBO Prodigy Cryoprobe, 500 MHz with BBFOPLUS SmartProbe, and 600 MHz with BBO Cryoprobe) differed significantly. The developed routine was also applied to calculate the performance characteristics during routine quantitative NMR experiments. The procedure was evaluated for NMR spectra of 659 active pharmaceutical ingredients dissolved in CDCl3 , DMSO, and CH3 OD. This test is more preferable than the routine procedure using standard solutions because the performance is estimated separately for each matrix at the specific time point of measurements. Our automated routine is the ideal tool for any NMR laboratory. In full automation, the NMR data are validated directly for each sample, making unnecessary daily measurements of standard solutions and manual evaluation to their NMR spectra.

Determination of 2'-Fucosyllactose and Lacto-N-neotetraose in Infant Formula.

Human milk oligosaccharides (HMO) are the third most abundant solid component of human milk. It is likely that they are responsible for at least some of the benefits experienced by breast-fed infants. Until recently HMO were absent from infant formula, but 2'-fucosyllactose (2'-FL) and lacto-N-neoteraose (LNnT) have recently become available as ingredients. The development of formula containing these HMO and the quality control of such formula require suitable methods for the accurate determination of the HMO. We developed two different approaches for analysis of 2'-FL and LNnT in formula; high performance anion exchange chromatography with pulsed amperometric detection (HPAEC-PAD) and hydrophilic interaction liquid chromatography with fluorescence detection (HILIC-FLD). In lab trials using blank formula spiked with the two oligosaccharides, both approaches worked well with recoveries of 94⁻111% (HPAEC-PAD) and 94⁻104% (HILIC-FLD) and RSD (iR) of 2.1⁻7.9% (HPAEC-PAD) and 2.0⁻7.4% (HILIC-FLD). However, when applied to products produced in a pilot plant, the HPAEC-PAD approach sometimes delivered results below those expected from the addition rate of the ingredients. We hypothesize that the oligosaccharides interact with the formula matrix during the production process and, during sample preparation for HPAEC-PAD those interactions have not been broken. The conditions required for labeling the HMO for detection by the FLD apparently disrupt those interactions, and result in improved recoveries. It is likely that both analytical approaches are appropriate if a suitable extraction process is used to recover the HMO.

Blood species discrimination using proton nuclear magnetic resonance spectroscopy.

Blood species identification is an important challenge in forensic science. Conventional methods used for blood species analysis are destructive and associated with time-consuming sample preparation steps. Nuclear magnetic resonance (NMR) spectroscopy is known for its nondestructive properties and fast results. This research study presents a proton (1H) NMR method to discriminate blood species including human, cat, dog, elephant, and bison. Characteristic signals acting as markers are observed for each species. Moreover, the data are evaluated by principle component analysis (PCA) and support vector machines (SVM). A 100% correct species recognition between human and nonhuman species is achieved using radial basis kernel function (RBF) and standardized data. The research study shows that 1H NMR spectroscopy is a powerful tool for differentiating human and nonhuman blood showing a great significance to forensic science.

Facilitating the performance of qNMR analysis using automated quantification and results verification.

Quantitative nuclear magnetic resonance (qNMR) is considered as a powerful tool for measuring the absolute amount of small molecules in complex mixtures. However, verification of the accuracy of such quantification is not a trivial task. In particular, preprocessing and integration steps are challenging and potentially erroneous. A script was developed in Matlab environment to automate qNMR analysis. Verification of the results is based on two evolving integration profiles. The analysis of binary mixtures of internal standards as well as pharmaceutical products has shown that all common artifacts (phase and baseline distortion, impurities) can be easily recognized in routine qNMR experiments. In the absence of distortion, deviation between automatically (mean value of several integrals) and manually calculated values was generally below 0.1%. The routine is independent of multiplet pattern, solvent, spectrometer, nuclei type and pulse sequence used. In general, the usage of the developed script can facilitate and verify results of routine qNMR analysis in an automatic manner. Copyright © 2017 John Wiley & Sons, Ltd.

Practical guide for selection of 1 H qNMR acquisition and processing parameters confirmed by automated spectra evaluation.

In our recent paper, a new technique for automated spectra integration and quality control of the acquired results in qNMR was developed and validated (Monakhova & Diehl, Magn. Res. Chem. 2017, doi: 10.1002/mrc.4591). The present study is focused on the influence of acquisition and postacquisition parameters on the developed automated routine in particular, and on the quantitative NMR (qNMR) results in general, which has not been undertaken previously in a systematic and automated manner. Results are presented for a number of model mixtures and authentic pharmaceutical products measured on 500- and 600-MHz NMR spectrometers. The influence of the most important acquisition (spectral width, transmitter [frequency] offset, number of scans, and time domain) and processing (size of real spectrum, deconvolution, Gaussian window multiplication, and line broadening) parameters for qNMR was automatically investigated. Moderate modification of the majority of the investigated parameters from default instrument settings within evaluated ranges does not significantly affect the trueness and precision of the qNMR. Lite Gaussian window multiplication resulted in accuracy improvement of the qNMR output and is recommended for routine measurements. In general, given that the acquisition and processing parameters were selected based on the presented guidelines, automated qNMR analysis can be employed for reproducible high-precision concentration measurements in practice.

Transfer of multivariate regression models between high-resolution NMR instruments: application to authenticity control of sunflower lecithin.

In recent years the number of spectroscopic studies utilizing multivariate techniques and involving different laboratories has been dramatically increased. In this paper the protocol for calibration transfer of partial least square regression model between high-resolution nuclear magnetic resonance (NMR) spectrometers of different frequencies and equipped with different probes was established. As the test system previously published quantitative model to predict the concentration of blended soy species in sunflower lecithin was used. For multivariate modelling piecewise direct standardization (PDS), direct standardization, and hybrid calibration were employed. PDS showed the best performance for estimating lecithin falsification regarding its vegetable origin resulting in a significant decrease in root mean square error of prediction from 5.0 to 7.3% without standardization to 2.9-3.2% for PDS. Acceptable calibration transfer model was obtained by direct standardization, but this standardization approach introduces unfavourable noise to the spectral data. Hybrid calibration is least recommended for high-resolution NMR data. The sensitivity of instrument transfer methods with respect to the type of spectrometer, the number of samples and the subset selection was also discussed. The study showed the necessity of applying a proper standardization procedure in cases when multivariate model has to be applied to the spectra recorded on a secondary NMR spectrometer even with the same magnetic field strength. Copyright © 2016 John Wiley & Sons, Ltd.

Authentication of the origin of sucrose-based sugar products using quantitative natural abundance (13) C NMR.

BACKGROUND: Due to possible falsification of sugar cane products with cheaper alternative (sugar beet) on the market, a simple analytical methodology needs to be developed to control the authenticity of sugar products. RESULTS: A direct (13) C nuclear magnetic resonance (NMR) method has been validated to differentiate between sucrose-based sugar products produced from sugar beet (C3 plant) and sugar cane (C4 plant). The method is based on calculating relative (13) C content of the C1, C2, C5, and the C1, C4, C5, C6 positions of the glycosyl and fructosyl moieties of the sucrose molecule, respectively. NMR acquisition parameters and data processing have been optimized to reach a high level of intraday and interday precision (<0.2%). Good linearity (R(2) = 0.93) was obtained for the beet sugar-cane sugar blends containing from 0 to 100 wt% of beet sugar. The method was applied to ten commercial sucrose-based sugar products of different botanical origin. Principal component analysis (PCA) was applied to the relative peak areas for replicate measurements to visualize the difference between studied products. CONCLUSION: The (13) C NMR method is a good alternative to complex isotope ratio mass spectrometry measurements for routine detection and semi-quantification of adulteration of commercial cane sugar (C4 plant) with less expensive beet sugar (C3 plant). © 2015 Society of Chemical Industry.

Phospholipids from herring roe improve plasma lipids and glucose tolerance in healthy, young adults.

BACKGROUND: Herring roe is an underutilized source of n-3 polyunsaturated fatty acids (PUFAs) for human consumption with high phospholipid (PL) content. Studies have shown that PL may improve bioavailability of n-3 PUFAs. Arctic Nutrition's herring roe product MOPL™30 is a PL: docosahexaenoic acid (DHA)-rich fish oil mixture, with a DHA:eicosapentaenoic acid (EPA) ratio of about 3:1, which is also rich in choline. In this pilot study, we determined if MOPL30 could favorably affect plasma lipid parameters and glucose tolerance in healthy young adults. METHODS: Twenty female and one male adults, between 22 and 26 years of age, participated in the study. Participants took encapsulated MOPL30, 2.4 g/d EPA + DHA, for 14 days, and completed a three-day weighed food record before and during the capsule intake. Plasma lipids and their fatty acid (FA) composition, plasma and red blood cell (RBC) phosphatidylcholine (PC) FA composition, acylcarnitines, choline, betaine and insulin were measured before and after supplementation (n = 21), and one and four weeks after discontinuation of supplementation (n = 14). An oral glucose tolerance test was performed before and after supplementation. RESULTS: Fasting plasma triacylglycerol and non-esterified fatty acids decreased and HDL-cholesterol increased after 14 days of MOPL30 intake (p < 0.05). The dietary records showed that PUFA intake prior to and during capsule intake was not different. Fasting plasma glucose was unchanged from before to after supplementation. However, during oral glucose tolerance testing, blood glucose at both 10 and 120 min was significantly lower after supplementation with MOPL30 compared to baseline measurements. Plasma free choline and betaine were increased, and the n-6/n-3 polyunsaturated (PUFA) ratio in plasma and RBC PC were decreased post-supplementation. Four weeks after discontinuation of MOPL30, most parameters had returned to baseline, but a delayed effect was observed on n-6 PUFAs. CONCLUSIONS: Herring roe rich in PL improved the plasma lipid profile and glycemic control in young adults with an overall healthy lifestyle.

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. In the majority of cases, quantification results obtained on the low-field NMR spectrometer are similar to those obtained with high-field 500-600 MHz NMR devices. Validation results in terms of accuracy, precision, reproducibility, limit of detection and recovery demonstrated that the developed method is fit for purpose for the marketed products. The NMR method was extended to the analysis of methylsulfonylmethane, adulterant maltodextrin, acetate and inorganic ions. Low-field NMR can be a quicker and cheaper alternative to more expensive high-field NMR measurements for quality control of the investigated dietary supplements. High-field NMR instrumentation can be more favorable for samples with complex composition due to better resolution, simultaneously giving the possibility of analysis of inorganic species such as potassium and chloride.

Edible insects as a novel source of lecithin: Extraction and lipid characterization of black soldier fly larvae and yellow mealworm.

Edible insects with high fat and phosphorus content are a potential novel source of lecithin, however, studies on their minor lipids are limited. In this study, lecithin was extracted from black soldier fly larvae and yellow mealworm. Herein, the effects of lecithin extraction method, matrix and ultrasound pretreatment were explored based on the fatty acid composition and phospholipid profile with soy lecithin as a reference. The use of a wet matrix and ultrasound pretreatment increased the extraction efficiency of total PLs from both insects. Insect lecithin contained a considerable amount of sphingomyelin compared to soy lecithin. In insect lecithin, a total of 47 glycerophospholipid and sphingomyelin molecular species, as well as four molecular species of fatty acyl esters of hydroxy fatty acid, were detected. This study is the first comprehensive investigation of insects as a new source of lecithin with applications in food, cosmetics and in the pharmaceutical industry.

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. The methodology was used to analyze 20 authentic porcine heparinoid samples having heparin content between 4.25 w/w % and 64.4 w/w %. The characterization of crude heparin products was further extended to a simultaneous analysis of these common ions: sodium, calcium, acetate and chloride. A significant, linear dependence was found between anticoagulant activity and assayed heparin content for thirteen heparinoids samples, for which reference data were available. A Diffused-ordered NMR experiment (DOSY) can be used for qualitative analysis of specific glycosaminoglycans (GAGs) in heparinoid matrices and, potentially, for quantitative prediction of molecular weight of GAGs. NMR spectrometry therefore represents a unique analytical method suitable for the simultaneous quantitative control of organic and inorganic composition of crude heparin samples (especially heparin content) as well as an estimation of other physical and quality parameters (molecular weight, animal origin and activity).

Multinuclear NMR screening of pharmaceuticals using standardization by 2H integral of a deuterated solvent.

NMR standardization approach that uses the 2H 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 23Na (35Cl) NMR integral and 2H NMR signal of deuterated solvent, D2O, acquired using the specific spectrometer hardware. As an alternative, the possibility of 133Cs standardization using the addition of Cs2CO3 stock solution is shown. Validation characteristics (linearity, repeatability, sensitivity) are evaluated. A holistic NMR profiling of heparin products can now also be used for the quantitative determination of inorganic compounds in a single analytical run using a single sample. In general, the new standardization methodology provides an appealing alternative for the NMR screening of inorganic and organic components in pharmaceutical products.

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. For its successful implementation into process streams, a quick, easy, and reliable method is needed for its molecular weight determination. Here we present a method using 1H spectra of benchtop as well as conventional NMR systems in combination with multivariate data analysis, to determine lignin's molecular weight (Mw and Mn) and polydispersity index (PDI). A set of 36 organosolv lignin samples (from Miscanthus x giganteus, Paulownia tomentosa and Silphium perfoliatum) was used for the calibration and cross validation, and 17 samples were used as external validation set. Validation errors between 5.6% and 12.9% were achieved for all parameters on all NMR devices (43, 60, 500 and 600 MHz). Surprisingly, no significant difference in the performance of the benchtop and high-field devices was found. This facilitates the application of this method for determining lignin's molecular weight in an industrial environment because of the low maintenance expenditure, small footprint, ruggedness, and low cost of permanent magnet benchtop NMR systems.