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You are here: Home / Archives for Herbal Supplement

Presentation and Posters at PANIC 2014

September 11, 2014 by process nmr 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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Herbal Supplement for Erectile Dysfunction Found to Contain Thio Structural Analog of Sildenafil (Viagra)

December 24, 2013 by process nmr 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.

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

December 22, 2013 by process nmr Herbal Supplement, qNMR

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 maltodextrin. A quantitative 13C NMR method was developed to quantify free fructose content in the complex. Finally, an NMR based product stability study was performed to monitor molecular level stability of the complex at temperature ranging from 35-70oC with exposure lasting from 2-18 hours.

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

December 2, 2013 by process nmr Chemistry, Chemometrics, Herbal Supplement, NMR, Process NMR, qNMR, Reaction Monitoring, TD-NMR

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 value adulterants and the addition of pharmaceuticals to herbal supplements in order to obtain the expected efficacy of a product is surprisingly common in the marketplace today. The development of official test methods utilizing NMR spectroscopy will allow the detailed unequivocal chemical fingerprinting of the NMR spectrum to be combined with qNMR methods to quantify active components and prove authenticity from either direct observation of adulterants or by non-targeted methods such a principal component analysis. We will discuss in detail a method developed on aloe vera juice and powder products to quantify the active components as well as identify the presence of whole leaf or inner gel material in the manufacturing process. The presence of preservatives, degradation products, additives, and adulterants can also be readily identified and quantified by 1H NMR. Statistical analysis can be performed to define the range of concentrations expected in naturally produced materials as well as determine the presence of adulterated material. The utilization of erectile dysfunction pharmaceuticals in herbal supplements to deliver the expected efficacy to the herbal products will described. Finally, the use of 13C NMR to define the authenticity of gum Arabic (acacia Senegal) used as an emulsifier in the beverage industry compared to chemically similar but inferior/cheaper gum products.

and in the poster session he has 3 posters being presented:

Development of an Automated Quantitative Chemical Mixture Analysis Method within Metrelab Research MNova – Internal Standard qNMR Measurements on Aloe Vera Raw Materials, Aloe Containing Products, Finished Beer and Samples from the Different Points in the Brewing Process

John C. Edwards, Adam J. Dicaprio, Process NMR Associates, Michael A. Bernstein, Mestrelab Research

Small Molecule Chemistry of Spontaneously Fermented Coolship Ales

Adam J. Dicaprio, John C. Edwards, Process NMR Associates

John will also chair a session on Online/At-Line NMR

ONLINE/AT LINE NMR – Wednesday, February 4

3:20 Session Chair’s Remarks – John Edwards, Ph.D., Process NMR Associates, LLC – Biography

3:25: A Compact, Portable 4.7 T Driven NMR System for Reaction Monitoring

Mark Zell, Ph.D., Senior Principal Scientist & Technical Leader, Structure Elucidation Group, Pfizer – Biography

We have been using a newly developed 4.7T (200 MHz 1H operating frequency) cryogen-free NMR system which utilizes a high-temperature (~14K) superconducting magnet cooled by a standard helium compressor, driven by a high stability power supply, and utilizing a new state-of-the-art single board spectrometer. The system is designed to be portable, allowing for rapid cooling and ramping of the magnet to field without the need for expensive cryogens or a trained engineer. We have been using this system, coupled with a microcoil flow probe to investigate a multitude of samples, ranging from traditional organic compounds to complex reaction mixtures. To date, primarily 1D 1H NMR data on these samples has been acquired. We are working toward utilizing more sophisticated multi-dimensional gradient-based experiments on this system to provide additional information on reaction mixtures in both a “stop-flow” and flow-through mode. This system works well for reaction monitoring, as it provides intermediate resolution between lower resolution 60 MHz spectrometers and traditional higher-field superconducting spectrometers at 400 MHz and above. This poster will provide an overview of this new technology and demonstrate the data we are able to achieve, in comparison to that obtained at both 60 and 400 MHz.

3:55 NMR Well Logging and Downhole Fluid Characterization

Martin Hürlimann, Ph.D., Scientific Advisor, Schlumberger-Doll Research – Biography

Over the last decade, NMR well logging has matured into a significant new commercial application of nuclear magnetic resonance. In this method, an NMR sensor is moved through a borehole to continuously measure the fluids inside the surrounding earth formation. The environmental conditions are exceptionally challenging for NMR measurements. The whole sensor and associated electronics have to fit into the borehole (with a typical diameter of 20 cm) and able to withstand high temperatures and pressures that can reach 175o C and 140 MPa. The sample is located outside the sensor and the applied magnetic fields are necessarily grossly inhomogeneous. Furthermore, the measurements have to be sufficiently robust so that they can be performed in a highly automated manner without the assistance of an NMR specialist and in a wide range of environments, from the arctic to the tropics. In this talk, I will review how these challenges can be overcome with novel hardware design and new measurement techniques. Current state-of-the-art well logging measurements enable the extraction of a wide range of important physical and chemical properties that include the porosity, the distribution of pore size, and estimate of the permeability, the identification and quantification of the different fluid phases occupying the pore space (water brine, crude oil, gas…), the fluid compositions, and the fluid viscosities. I will highlight new relaxation and diffusion measurements to determine two-dimensional relaxation-diffusion distribution functions. These techniques are well suited for other applications in fields beyond the oil field, including process control or the characterization of food products.

4:25 Characterizing a Hydrogenation Reaction: In situ NMR and Mechanistic Modeling

Jonas Buser, NMR Structural Characterization Group, Eli Lilly and Company – Biography

The development of a robust manufacturing process typically involves a joint effort between engineering, mathematical modeling, process chemistry, and analytical chemistry. This presentation describes the optimization of a hydrogenation reaction observed to have variable reaction completion times at manufacturing scale. On-line flow NMR (ReactNMR) was employed to characterize a detailed reaction mechanism and kinetics. Variables of pH and hydrogen pressure were examined to see how they affected the dynamic mechanism and kinetics of the reaction. A mathematical model was developed to gain further understanding of the process kinetics as well as mass transfer limitations. The model was used to predict experimental conditions capable of minimizing the hydrogenation time. This problem solving approach is being broadly adopted to solve complex reaction problems where traditional means don’t provide a comprehensive understanding of the process.

 

 

Beware of Adulteration of “Herbal Supplements” for Erectile Dysfuntion

November 11, 2013 by process nmr Herbal Supplement, NMR, qNMR

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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