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Presentation and Posters at PANIC 2014

by Beer, Chemometrics, Herbal Supplement, NMR, qNMR

“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.
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“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.
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“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.
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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”, Boris Nemzer, John C. Edwards, presented at the 2nd PANIC, Charlotte, NC, February 3-5, 2014.
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John Edwards to be Guest Editor of 2 Special Issues of Magnetic Resonance in Chemistry Dedicated to Benchtop NMR

by NMR, Process NMR, qNMR, TD-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 on spectrometers, magnets, educational, industrial, academic applications, chemometrics, automated approaches, reaction monitoring, online/at-line utilization, 2D NMR, combined spectral/relaxation applications.

The second will be on low resolution benchtop NMR but I would like to exclude applications that have been around for decades (H content, SFC, oil content, spin finish). I would like to encourage new applications to be submitted and they should include hardware, magnets, spectrometers, probes, 1D/2D Laplace inversion (I’d love a review/overview of that software aspect), applications. Again – all vendors and all users of commercial and home grown benchtop TD-NMR systems please submit.

We’re looking for articles on FPGA spectrometers, software approaches (1D/2D Laplace, chemometrics), magnet design and construction, dedicated rheology analysis instruments, field cycling NMR, unilateral NMR, core analyzers, applications of all whether educational, academic, industrial.

The types of articles can be Reviews, Mini-Reviews, Tutorial, Historical, Spotlight, Perspective, Communication, Article, Application Note, Case Report, Spectral Assignments, Correspondence.

Here is the official word on the use of color (note you can have all the color figures you wish in the online version but the print version is restricted): two colour illustrations per submission are allowed free of charge, however further colour illustrations are allowed at the Editors discretion and where they are justified. Authors can have as much colour as they like in the online version as the restrictions are just for the print version.

Please contact me directly if you would like to make a submission of your work to either of the two issues: john@process-nmr.com

I have posted the authors instructions for special Issues that I was given on my website at:
https://process-nmr.com/pdfs/MRC_Submission_instrux.pdf

The MRC author guidelines can be found at:
http://onlinelibrary.wiley.com/journal/10.1002/%28ISSN%291097-458Xa/homepage/ForAuthors.html

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

by Chemistry, Herbal Supplement, NMR, qNMR

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 we have one more for the list that the FDA keeps on such dangerously adulterated products.

Solid-State 13C NMR of Drug API and Tablets

by NMR

We have an excellent solid-state Doty Scientific Supersonic 7mm CP-MAS probe for our Varian UP-200 spectrometer. This is a nice field strength for solid-state 13C analyses as it allows for spectra at higher sensitivity than a 100 MHz but still has the advantage that 7 kHz is enough to push the aromatic MAS sidebands beyond 0 ppm so that more accurate aromaticity values can be calculated. The probe is still working after 20 years and we are using the original rotors and have never had to replace any of the capacitors. We have run approaching 20,000 experiments with this probe. Here are some of the nice spectra we have been getting recently on drug API and tablets.

Above: Solid-State 13C NMR of Rapamycin API

Above: Solid-State 13C NMR of Ranitidine HCl – Zantac Tablet

Above: Solid-State 13C NMR of Simvastatin 20 mg Tablet

Solid-State 13C NMR of Tylenol 3 – Acetamenaphin + Codeine

Above: Solid-State 13C NMR of Amoxicillin Capsules

Above: Solid-State 13C NMR of Diovan 50 mg Tablet

Above: Solid-State 13C NMR of Divalproex Tablet

Above: Solid-State 13C NMR of Herbal Supplement Capsule Found to Contain Thioaildenafil – A Structural Analog of Sildenafil (aka Viagra)

Above: Solid_State 13C NMR of Famotidine Tablet

Above: Solid-State 13C NMR of Metroprolol 50 mg Tablet

Above: Solid-State 13C NMR spectrumof Azithromycin Tablet

Solid-State 13C NMR of Ibuprofen – Generic 200mg Tablet

Above: Solid-State 13C NMR of Atorvastatin

 

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

by Chemistry, Chemometrics, NMR, PAT, Process NMR, qNMR, Reaction Monitoring, TD-NMR

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