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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Solid-State 13C NMR of Drug API and Tablets

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…

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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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