Chemical Fingerprints of Cider – Cidercon 2018 Technical Presentation – Recorded and Presented on the Cider Chat Podcast

John Edwards presented a talk on the chemical analysis of ciders at Cidercon 2018. The talk was recorded by Ria Windcaller who produces the Cider Chat Podcast which specializes in interviews and news from the world of commercial and amateur cider making. Here is the information to listen or watch the presentation. I have set up your presentation as a full podcast episode and as a video recording, without the podcast. It totally works! Yay. :) Via the podcast your presentation begins around 13:02 minutes into this week’s episode. I learned so much about a area of study I didn’t even knew existed. I’m excited to think that your work will boost cider’s study as it does for the wine industry. There are lots of listening options to share as you please via Cider Chat- http://ciderchat.com/chemical-fingerprints/ This link above provides the description and a photo. It is set up to work with social media. I have posted it at the Cider Chat Facebook page if you want to see what it looks like, before sharing. Listen via: iTunes: https://apple.co/2yBsrz5 For Android the following Apps need to be downloaded to listen to podcasts. Stitcher: http://bit.ly/1OvdrDq Google Play: https://play.google.com/music/m/Ine7dtqx57ephmbncwrtubpkyt4?t=Cider_Chat and the Spotify…

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The Chemical Fingerprint of Beer from a Single Experiment with Minimum Sample Preparation – A Rapid Quantitive Analysis by 1H NMR Spectroscopy

NMR Spectroscopy is the premier tool utilized by chemists to obtain detailed chemical information on molecular structure and is used extensively in molecular structure verification, chemical purity analysis, and complex mixture analysis. We have developed a quantitative NMR analysis that yields a chemical fingerprint that brewers can utilize to follow detailed variations in the chemistry observed in the various stages of the brewing process (malting, mashing, boiling, fermentation, ageing, and blending). The analysis observes all molecules in the beer at the same time and each molecular component (acids, alcohols, amino acids, malt-oligosaccharides) yields a unique spectral fingerprint pattern that is related to the structure of the molecule. Though the spectrum consists of a large number of overlapped individual fingerprints it is possible to identify and quantify individual components because many components have signals that appear at unique and specific points in the spectrum. The quantitative analysis is performed by comparing the area under the individual molecule signals to that of an internal standard (Maleic Acid 99%). Molecular components are quantified on a weight/volume basis in mg/L (parts-per million). Ethanol is also quantified on a %volume/volume basis. The technique is not only applicable to the brewing process but is also being…

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References to 1H qNMR Applied to Fruit Juices and Alcoholic Beverages

qNMR “Validation of quantitative NMR”, F Malz, H Jancke, J Pharm Biomed Anal,  38, 813–823, (2005) “Quantitative 1H NMR spectroscopy”, S K Bharti, R Roy, Trends in Anal Chem, 35, 5-26 (2012) “NMR-based plant metabolomics: where do we stand, where do we go?”  H-K Kim, Y-H Choi, R Verpoorte Trends Biotech, 29(6), 267 (2011). “Universal quantitative NMR analysis of complex natural samples”, C Simmler, J G Napolitano, J B McAlpine, S-N Chen and G F Pauli, Current Opinion Biotech, 25, 51–59 (2014) “Quantitative 1H NMR: Development and Potential of a Method for Natural Products Analysis” G F Pauli, B U Jaki, D C Lankin, J. Nat. Prod., 68, 133-149 (2005) Juices “High-Field Proton NMR Studies of Apple Juices”, P S Belton, I Delgadillo, A M Gil, P Roma, F Casuscelli, I J Colquhoun, M J Dennis M Spraul, Mag Res Chem, 35, S52-S60 (1997) “Quantitative determination of (-)-epicatechin in cider apple juices by 1H NMR”, I Berregi , J I Santos , G del Campo , J I Miranda, Talanta 61 (2003) 139-145 “Use of the 1H Nuclear Magnetic Resonance Spectra Signals from Polyphenols and Acids for Chemometric Characterization of Cider Apple Juices”, G del Campo, J. I Santos, N…

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Quantitative 1H NMR Analysis of “Off-the-Shelf” Commercial Kombucha Beverages for Ethanol, Organic Acids and Residual Sugars Analysis

Over the past few years our analytical NMR service has been developing a detailed chemical fingerprint analysis of alcoholic beverages by quantitative 1H NMR (qHNMR). Beyond the typical analyses of beer, wine, port, hard cider, sake and spirits, we have been looking at other fermented beverages such as kombucha, kefir, kvass, mead, ginger beer and perry. As well as the final fermented beverages we have been actively investigating the various starting materials such as malt wort, apple juice, honey, grape juice, fruit juices, and tea. The NMR analysis can provide a rapid quantitative analysis without any sample preparation based on the molar ratio of integration value of unique molecular fingerprint peaks with the integrated signal of an internal standard. In our case we typically use maleic acid as an internal standard as it’s singlet signal peak appears in a non-overlapping are of the spectrum to the chemistry we are interested in following. The information that can be derived from the NMR experiment covers a wide dynamic range of component molecule concentrations from 10-100,000 ppm. The analysis observes all fully dissolved chemical constituents and the spectral response is linear with regard to all chemical types. As a primary analytical method the…

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PANIC NMR Validation Group – Website, Meetings and Organization

Validation of NMR: No Need to PANIC - Workshop held February 13, 2015, La Jolla, CA, U.S.A In conjunction with the 3rd PANIC conference in La Jolla, California, a 1-day NMR validation workshop was held that attracted approximately 80 interested participants. The agenda of the meeting is provided at this link (http://www.nmrvalidation.org/index.php/events/event-review) and registered participants can now download the presentations presented at the meeting. At the meeting it was decided to proceed with the idea of founding an organization dedicated to the development of validate NMR methods for use throughout all industry sectors. Organizational Scope: NMR spectroscopy provides a means to evaluate material with high compound and high material specificity. Information as to the chemical structure, stereochemistry, quantity, material composition, and material identity is encoded in the NMR spectrum. The high reproducibility of NMR spectroscopy from instrument to instrument and lab to lab makes NMR an excellent tool for material validation. Approaches to utilizing NMR as a material validation tool include using (1) targeted approaches, the identification and quantification of specific components, and (2) non-targeted approaches, the use of chemometric methods to evaluate the spectrum as a whole. Efforts to increase the number and the speed of validated NMR methods…

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1H qNMR of Alcoholic Cider – Analysis of Small Molecule and Residual Sugar Chemistry

1H quantitative NMR (qNMR) has been utilized to assess the the small molecule and carbohydrate chemistry of a number of home-brewed and commercial alcoholic ciders. A quantitative chemistry distribution of the products of the various fermentations that occur in cider making. Malolactic fermentation as well as fermentation by saccharomyces and wild yeasts occur in the cider making process which traditionally occurred without the intentional addition of yeast by the manufacturer. The distribution of small molecules produced by the yeast and bacterial metabolomes at work in the process can yield information of the sensory perception of ciders produced in different ways. An investigation of the residual sugar chemistry of commercial ciders gives some indication of the process of sweetening commercial cider products with sugar additions after fermentation is complete. These typical commercial ciders are very different in chemistry distribution compared to very dry cider styles such as those found in the Basque region of Spain where fermentation is taken to the extreme resulting in complete conversion of sugars to alcohol but also glycerols to 1,3 propandiol. Finally it was decided to determine how much quantitative chemistry information could be obtained from benchtop NMR systems operating in the 60 MHz range. These…

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PNA to Present 4 Topics at the 2015 ACS North East Regional Meeting

John Edwards of Process NMR Associates will be presenting 4 papers at the 2015 ACS Northeast Regional Meeting that will be held in Ithaca, NY, June 10-13, 2015. ABSTRACT ID: 2283171 ABSTRACT TITLE: 1H qNMR of Alcoholic Cider - Analysis of Small Molecule and Residual Sugar Chemistry (final paper number: 43) SESSION: Food Chemistry SESSION TIME: 5:00 PM - 9:00 PM PRESENTATION FORMAT: Poster DAY & TIME OF PRESENTATION: Wednesday, June, 10, 2015, 5:00 PM - 9:00 PM ROOM & LOCATION: Emerson Suites - Campus Center ABSTRACT ID: 2283063 ABSTRACT TITLE: Nutritional Supplement and Diesel Fuel Application Development for Benchtop NMR Systems Operating at 42, 60, and 80 MHz – Equivalency with Supercon NMR (final paper number: 336) SESSION: Analytical Chemistry SESSION TIME: 9:00 AM - 11:30 AM PRESENTATION FORMAT: Oral DAY & TIME OF PRESENTATION: Friday, June, 12, 2015 from 9:45 AM - 10:05 AM ROOM & LOCATION: 222 - Williams Hall ABSTRACT ID: 2283105 ABSTRACT TITLE: Survey of Low Field NMR Spectrometer Platforms for Successful Screening of Sexual Enhancement and Weight Loss Supplements for Adulteration with Drugs and Drug Analogs (final paper number: 386) SESSION: Medicinal Chemistry SESSION TIME: 1:00 PM - 3:20 PM PRESENTATION FORMAT: Oral DAY…

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Essential Oil Analysis – Comparison of 1H NMR from Benchtop and Supercon NMR Systems

1H NMR shows excellent promise to be utilized in the quality control and authentication of essential oils. In order to ascertain if benchtop NMR systems reveal adequate "1H spectral fingerprints" for this purpose we have run several hundred essential oils at 300 MHz (Varian Mercury-300 MVX by 1H, 13C, COSY, HETCOR, DEPT)  as well as at 82.3 MHz (Picospin 80), 60 MHz (Aspect-60), and 42.5 MHz (Magritek Spinsolve). The results plainly show that the spectrometers all yield similar proton line-widths with the difference in field strength leading to different levels of spectral dispersion and resolution. Though each spectrum is different it can plainly be seen that they all contain the same information with varying degrees of overlap. Chemometric and database comparative methods are being developed to allow identification of various essential oils as well as screening and quantifying different levels of adulteration. The figures below show examples from 6 different essential oils showing spectra obtained from all 4 spectrometers and plotted in the normalized chemical shift scale (ppm) as well as the absolute frequency scale (Hz).

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Polyalphaolefin Hydrogenation – Residual Olefin Analysis – 1H NMR versus Bromine Number

1H NMR is an excellent tool for monitoring the residual olefin content of polymers after hydrogenation reactions. The fact that the olefin fall in a unique region of the spectrum means that it is a straightforward measurement to quantify the %H present as olefin or to correlate that olefin content with other analyses such as bromine number. Here is an example of a polyalphaolefin residual olefin analysis. The olefin proton content (%H) was plotted against bromine number values obtained on each of the samples. A linear correlation was obtain but two different correlations were observed that were dependent on the viscosity index of the polyalphaolefin being analyzed. Figure 1 shows the 1H NMR spectra obtained on neat samples on a Picospin-80 spectrometer operating at 82.3 MHz. The methyl and methlene protons of the polymer backbone are plainly seen and the olefin and alpha-olefin protons are observed.   Figure 2 shows the linear correlation between %H olefin and bromine number with the two correlations caused by different VI grade being indicated. The analysis shows that for the two viscosity grades the grade can be identified from the linear correlation that the data falls onto and the %H olefins content can directly…

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Residual Catalytic Cracker – Heavy Petroleum Feedstream Properties from 1H NMR at 43 MHz

Back in October we presented a talk at Gulf Coast Conference that concerned the prediction of the chemical and physical properties of heavy petroleum feeds being converted to higher value product in a residual catalytic cracker (RCC). Over the years we have analyzed these materials by 300 and 60 MHz NMR and obtained good PLS-regression models that can adequately predict properties for real-time process control and optimization in a petroleum refinery. With the advent of a large number of new benchtop NMR systems we have been convincing ourselves that these types of analyses can be performed by systems such as the Magritek Spinsolve 43 MHz. We ran a series of samples that had been sitting around our lab for 15 years by dissolving them at about 50 volume% in a 50/50 CDCl3/CS2 solvent system. For each sample we had laboratory test data for a number of chemical and physical properties of interest to process engineers. We regressed the lab data variability against the variability in the Magritek 43MHz 1H NMR spectra and obtained cross-validated PLS models. The presentation material is given here at this link - Gulf Conference Presentation - 43 MHz RCC Feedstream Regression Models

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Beer and Cider Analysis – Example of Spectral Repeatability of Benchtop 60 MHz NMR System

Here is an example of spectral reproducibility. We are doing a lot of beer NMR at the moment on our 300 MHz NMR and for "giggles" we are running many samples through the various bench-top systems in our lab. We have been quantifying small organic acids (lactic, acetic, succinic , malic, citric, etc.) as they can give some idea of yeast activities and health during fermentation. We are also quantifying  and studying the 1,4/1,6 linkage distribution of residual dextrins. The series of superimposed spectra below consists of 28 spectra of a freeze dried beer sample (a unique Belgian Dubbel. Each spectrum was 128 pulses and took approximately 30 minutes per spectrum. So the superimposed data represents a 14 hour continuous stability test.The data was automatically processed with 16K zero-fill and autophase.It looks pretty damn good.   We've been looking at a lot of sour beers - here is a home-brewed Flemish Red aged in an oak barrel - note the high lactic and acetic content. We've also been analyzing a lot of hard ciders - commercial and home-brewed varitieties of various styles - very different from one sample to another in the small molecule and sugar chemistry.     1H…

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Nutritional Supplement and Diesel Fuel Application Development for Benchtop NMR Systems Operating at 42, 60, and 80 MHz – Equivalency with Supercon NMR

Benchtop high-resolution NMR systems are available at a number of field strengths and probe configurations. However beyond the obvious academic instruction market for these instruments very few applications have been demonstrated across all available platforms and thus proving the general applicability of benchtop NMR technology to industrial quality control. We will present two chemometric-based applications that have been developed at 4 different field strengths utilizing Varian Mercury 300 MHz, Magritek Spinsolve 42 MHz, Aspect AI 60 MHz, and Thermo Picospin 80 MHz NMR systems. Partial-least-squares (PLS) regression correlations were obtained on all 4 platforms relating to: 1) Omega-3 fatty acid composition of samples taken from various points in a nutritional supplement manufacturing process. Excellent correlations were obtained on all 4 NMR instruments proving that NMR technology is applicable to in-lab, at-line. or on-line analysis of fish oil derived omega-3 fatty acid supplements. The 40 second NMR analysis effectively replaces a 60+ minute GC analysis. 2) Physical and chemical property determination of diesel fuels where excellent correlations were obtained between 1H NMR variability and parameters such as density, aromatic content by GC, hydrogen content by 1H TD-NMR (ASTM D7171 method), and sulfur content. Many more physical and chemical properties can be…

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From Atoms to Flavour: The Chemistry of Beer

Adam DiCaprio (ex PNA) gave an excellent Science Cafe Talk under the auspices of the ACS North Carolina Section at the Busy Bee Cafe in downtown Raleigh on December 2, 2014. CHanging gears from his previous talks he centered the discussion on malt and hop chemistry as well as an start-to-finish NMR analysis of production runs of a bottled commercial tavern ale. If you are interested in having Adam give a detailed chemistry seminar on beer at your section meetings please contact him directly at adam@process-nmr.com. A PDF version of his talk is available here .... ACS Science Cafe Talk - Dicaprio - Busy Bee Cafe - Raleigh NC - 12-2-14

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Comparison of 1H NMR Spectra Obtained at 42, 60, 82, and 300 MHz – Fish Oil Omega-3 Ethyl Ester Supplement Example

Process NMR Associates is currently developing NMR applications based on direct measurement of chemometric modeling on NMR data obtained on numerous NMR platforms. Our intention is to develop solutions that can be executed on any NMR platform. With this in mind we are currently developing a fish oil analysis application that can provide the EPA and DHA omega-3 fatty acid content of fish oil supplements manufactured by an ethyl ester esterification process. We have obtained data at 42 MHz, 60 MHz, 82 MHz and 300 MHz. The chemometric modelling yielded PLS models for all 4 field strengths that yield effectively the same result - DHA can be measured to +/- ~1.1 wt% and EPA can be measured to +/- ~2.2 wt% by a 40 second 1H NMR measurement. THe correlation is derived from a  regression of the 1H NMR variability with primary GC analysis values. This analysis has been shown for the 300 and 60 MHz data in a previous post on this blog. The same analysis was also obtained, with similar results, on 42 and 82 MHz platforms proving that individual applications can be automated and provided at all relevant frequencies of NMR analysis whether on superconducting lab systems or permanent…

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Presentations at SMASH 2014

"Beer Manufacturing and Analysis by NMR", John C. Edwards and Adam Dicaprio, Presented at the Mestrelab MNova Users, Meeting - SMASH, Atlanta, GA, September 7, 2014 Get PDF Here “Survey of Low Field NMR Spectrometer Platforms for Successful Screening of Sexual Enhancement and Weight Loss Supplements for Adulteration with Drugs and Drug Analogs", John C. Edwards, Kristie Adams, Anton Bzhelyansky , Presented at SMASH Conference, Atlanta, GA, September 7-10, 2014. Get PDF Here

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Presentation and Posters – Magnetic Resonance in Food Conference 2014 – Cesena Italy

“Liquid and Solid-State 27Al qNMR of an Elemin Senonian Trace Minerals Supplement for Identification, Chemical Structure, Quantitation of Active Ingredient in the Product, and Product Stability”, Boris Nemzer, John C. Edwards, presented at XII International Conference on the Applications of Magnetic Resonance in Food Science: Defining Food by Magnetic Resonance, Cesena, Italy, May 20-23, 2014. Get PDF Here “Liquid and Solid-State Multinuclear 13C and 11B qNMR FruitexB Fructoborate Complex Nutritional Supplement. Identification, Chemical Structure, Quantitation of Active Ingredient in Product, and Product Stability”, Boris Nemzer, John C. Edwards, presented at XII International Conference on the Applications of Magnetic Resonance in Food Science: Defining Food by Magnetic Resonance, Cesena, Italy, May 20-23, 2014. Get PDF Here “1H qNMR of EPA and DHA Omega-3 Fatty Acid Esters - PLS Regression Models Obtained by 60 and 300 MHz NMR - At-Line and On-Line Monitoring of a Fish Oil Nutritional Supplement Manufacturing Process”, John C. Edwards, Paul J. Giammatteo, invited oral presentation at XII International Conference on the Applications of Magnetic Resonance in Food Science: Defining Food by Magnetic Resonance, Cesena, Italy, May 20-23, 2014. “Application of High Field and Cryogen-Free Bench-Top NMR Platforms to the Monitoring and Quantitation of PDE5 Inhibitor Adulteration of…

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Presentation and Posters at PANIC 2014

“NMR Based Authentication of Nutraceuticals, Herbal Supplements, and Food Additives: Economic- and Efficacy-Driven Adulteration of Aloe Vera, Herbal Erectile Dysfunction Supplements, and Acacia Gum”, John C. Edwards, invited presentation at the 2nd PANIC, Charlotte, NC, February 3-5, 2014. Get PDF Here “Development of an Automated Complex Mixture Analysis qNMR Method within Mestrelab MNova - Application to Aloe Vera and the Beer Brewing Process", John C. Edwards, Adam J. Dicaprio, Michael A. Bernstein, presented at the 2nd PANIC, Charlotte, NC, February 3-5, 2014. Get PDF Here “Small Molecule Chemistry of Spontaneously Fermented Coolship Ales”, Adam J. Dicaprio, John C. Edwards, presented at the 2nd PANIC, Charlotte, NC, February 3-5, 2014. Get PDF Here “Liquid and Solid-State 1H, 13C, and 11B qNMR Analysis of Fruitex-B®– A Calcium Fructoborate Comple: Chemical Structure and identification, quantitative analysis and stability study”, Boris Nemzer, John C. Edwards, presented at the 2nd PANIC, Charlotte, NC, February 3-5, 2014. Get PDF Here

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John Edwards to be Guest Editor of 2 Special Issues of Magnetic Resonance in Chemistry Dedicated to Benchtop NMR

I have been invited to be a guest editor for Wiley publishing to pull together 2 special issues of Magnetic Resonance in Chemistry. I am putting out a general “call for papers” but I will harass people personally. We are looking for 10-20 papers for each issue. The deadline for submission of the papers is June 30 so no-one has an excuse that there isn't enough time. I do ask that you email me at the contact below to let me know that you are thinking of submitting and a title would be nice also (though I won't hold you to it). We hope to have the review and revide papers (if necessary) by late October and then publish by December 2014. The first will be on high resolution benchtop NMR in which I would like to include all permanent magnet systems capable of obtaining a spectrum. This is an open invitation to all the vendors and their customers of (in no particular order) Anasazi, Nanalysis, One Resonance Sensors, Magritek/ACT, Aspect, Qualion, Picospin, Resonance Systems, Oxford Instruments, Bruker, home built devices, I would also make the exception that HTS systems be included as they are also cryogen free. Any papers…

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Herbal Supplement for Erectile Dysfunction Found to Contain Thio Structural Analog of Sildenafil (Viagra)

A herbal supplement marketed to alleviate erectile dysfunction was recently submitted for testing in our laboratory because it was surprisingly effective considering it should only contain the traditional herbals utilized for this problem such as Oyster, 2-Deoxy-D Glucose, Barberry, Snow Lotus, Bombyx Mori L., Ginger Root, Salfron Crocus. Above: 1H NMR of ED Herbal Supplement - this is an extract of the powder from  the capsules into 80:20 CD3CN:D2O - Observed suspicious specific small molecule peaks - herbals are usually broad featureless complex mixture spectra. This is something in different - a specific drug material appears to have been added.Comparison with the spectrum of Viagra (Sildenafil Citrate) below shows a strong similarity between the 2 active ingredients. We also obtained the COSY, 13C and DEPT NMR Spectra on the ED herbal supplement. These are shown below. The analysis of the NMR data led us to find that the extractable components of the sample contained predominantly Sulfoaildenafil (thioaildenafil) which is a strutural analog of Sildenafil (Viagra) and is not approved by any health regulation agency for use in erectile dysfunction medicines or supplements. Apparently these structural analogs to Viagra are found widely in herbal supplements sold for this malady. I guess…

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Liquid and Solid-State 1H, 13C, and 11B qNMR Analysis of Fruitex-B®– A Calcium Fructoborate Comple: Chemical Structure and identification, quantitative analysis and stability study

A poster on the following abstract will be presented at the 2nd PANIC Conference, Charlotte NC, Feb 3-5, by Boris Nemzer, Futureceuticals Inc., Momence IL, John C. Edwards, Process NMR Associates, Danbury CT Fruitex-B® is a patented plant mineral complex that is marketed as a nutritional supplement with potential health benefits for conditions linked to inflammation such as bone, joint and cardiovascular conditions. The product is a calcium fructoborate complex formed by the reaction of boric acid with fructose and calcium carbonate. Liquid and solid-state 13C and 11B NMR was utilized to establish a baseline for product quality and to establish a robust testing method for both identification and quantification of the mono-complex and the di-complex present in the product, as well as free borate and free fructose that is present in the finished product. The effect of varying the molar ratio of the complex components was studied by 11B and 13C NMR to establish the relative amounts of free borate, free fructose, and mono-/di-complex present in the products formed by the manufacturing recipe changes. A quantitative 11B NMR method was developed to quantify the amount of Fruitex-B®present in products where it was tableted or capsuled with magnesium stearate or…

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Special Issue on Benchtop NMR systems in Wiley Journal “Magnetic Resonance in Chemistry” – please consider submitting a technical or review paper

I was just asked by Roberto Gil (Carnegie Mellon) to pull together a special issue if Magnetic Resonance in Chemistry" on the topic of Benchtop NMR. I will personally be hitting up everyone I know who is working in this area to provide technical papers on their work in this area. I also wanted to extend an invitation to the members of this group to submit a paper for this special issue. All topics will be considered but I would like to stay away from "traditional" 1H TD-NMR and restrict 1H TD-NMR applications to new approaches. On the high resolution side (45, 60, 80 MHz) I am hoping that applications with some real meat might be submitted rather than brochure type papers with just spectra of solvents and small molecules. Please feel free to contact me directly if you have ideas on submissions. My contact information is listed below. Sincerely, -- John C. Edwards, Ph.D. Manager, Process and Analytical NMR Services Process NMR Associates, LLC 87A Sand Pit Rd, Danbury, CT 06810, USA Tel: +1 (203) 744-5905 Cell: +1 (203) 241-0143 Skype: jcepna e-mail: john@process-nmr.com

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Register to Attend PANIC 2014 ! Deadline for Poster Submissions is December 20

The 2nd Annual Practical Applications of NMR in Industry Conference (PANIC) will be held February 3-5 in Charlotte, NC. An excellent scientific agenda has been put together (see here). The Brochure is available here. Take note of the early registration (January 10, 2014) and poster submission (December 20, 2013) deadlines. John Edwards of Process NMR Associates is on the organizing committee of PANIC and has been appointed as Treasurer of the Conference company. John will be presenting an oral presentation in the one of the Nutraceutical Session:                NMR-Based Authentication of Nutraceuticals, Herbal Supplements, and Food Additives: Economic- and Efficacy-Driven Adulteration of Aloe Vera, Herbal Erectile Dysfunction Supplements, and Acacia Gum                                                                                                 John Edwards, Ph.D., Process NMR Associates, LLC - Biography Multinuclear NMR spectroscopy offers an outstanding ability to perform targeted and non-targeted analysis of nutraceuticals, herbal supplements, and food additives. Economic adulteration of these materials with lower…

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Trans Fat Analysis by 300 MHz 1H NMR

This topic has become pertinent again with the interest of FDA in trans-fat content in processed foods - more information here.Back in 2006 we performed a cursory analysis of trans fat reference materials that we purchased from AOCS. We performed a series of 1H NMR analysis and performed a chemometric PLS analysis correlating the 1H NMR spectral variability to trans fat content, PUFA (polyunsaturated fatty acid content), SAFA (saturated fatty acid content), and MONO (monounsaturated fatty acid content). Excellent correlations were obtained between wt% values obtained by GC analysis and the rapid 1H NMR analysis (2 minutes on a 300 MHz NMR). 1H NMR spectra on the standard samples are shown in the figures below as well as the GC data that was used in the regressions. A PCA analysis of  the NMR data nicely categorized the various types of samples as well as the trans fat contents of the samples with nice separation being shown in the PC1 vs PC2 score plot. The various correlations for trans fat, SAFA, PUFA, and MONO are shown below.    

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Beware of Adulteration of “Herbal Supplements” for Erectile Dysfuntion

We recently performed an analysis of a competitive product for a company working on developing "herbal supplements" for erectile dysfunction. They ended up not paying for the analysis so we thought we would just publish it generically as a "point of interest". It was described to us that the product worked incredibly well which immediately made it suspicious ... NB: we didn't actually try it out ourselves. The bottom line is that the product was not "herbal" at all .. it was thiosildenafil an analog of Viagra. "Herbal Supplement" Viagra Stacked comparison plot. COSY Beware out there. If you are on alpha-blockers for heart condition and buy an innocent looking "herbal" for ED issues .. it may actually be pharmaceutical grade viagra with all the use warnings that go with it.

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MestreLab MNova Users Meeting – SMASH 2013 – PNA NMR Presentation

"Utilization of MNova in a Commercial NMR Testing Laboratory for: 1) Development of Automated Quantitative Analysis Methods by Direct Internal Standard NMR Measurements, and 2) Pre-Processing of Large NMR Datasets for Chemometric Regression Analyses to Derive Chemical and Physical Properties" - presented by John Edwards at the MNova Users Meeting - SMASH 2013 - Santiago de Compostela, Spain, September 22, 2013 PDF of Presentation Automated 1H qNMR analysis of complex mixtures - example of aloe vera powder 200x Final automated analysis output for aloe vera analysis - assignments and quantitative output. Chemometric analysis - spectrum processing and X-matrix preparation performed in MNova - ascii output imported into Eigenvector Research Solo for PLS regression or PCA analysis. Correlation of 1H NMR at 300 or 60 MHz with GC analysis of EPA and DHA content (wt%).  

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