The Role of NMR in FDA Mandated Identity Testing of Nutritional Supplements

Process NMR Associates Offers Testing, Consultation, and Support in Meeting Your Identity Testing, Laboratory Methodology, and Process Analytical Requirements for FDA DS CGMP Rule Compliance. In conjunction with 21 CFR 111, the FDA’s Office of Nutrition, Labeling and Dietary Supplements has instituted the Dietary Supplement Current Good Manufacturing Practice Rule (DS GCMP Rule) and the Interim Final Rule effective December 2010. Laboratory compliance, including identity testing and analytical method protocols are now required for any manufacturer, packager, labeler or holder of dietary supplements without the previous exemption based on number of full time employees within the company. Smaller companies, typically without in-house laboratory and testing facilities, now need to obtain such services to meet the new compliance rules. Process NMR Associates (PNA), the process analytical consulting company and analytical testing company with over 45 years of experience in the field of nuclear magnetic resonance spectroscopy ("NMR") and organic spectroscopy (FTIR, NIR, ESR) is now offering expanded services for DS GCMP Rule compliance. As an example, The International Aloe Science Council (IASC), a trade association representing the global aloe vera industry, has selected Process NMR Associates, LLC (PNA) as its primary provider for Nuclear Magnetic Resonance (NMR) spectroscopic measurement of aloe…

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60 MHz NMR of Essential Oils from Benchtop System – Comparison to 300 MHz NMR Data

A comparison of the non-spinning 60 MHz NMR data compared with that obtained on a superconducting 300 MHz system are shown below for 10 Essential Oils - those essential oils are: Copaibo Balsam, Dill Weed, Citronella, Parsely Seed, Cinnamon Leaf, Balsam (Peru), Ginger, Eucalyptus Globulus, Petitgrain, Vetiver. We currently have a database of 1H (60 and 300 MHz) and 13C NMR data of around 110 essential oils. For further details on NMR analysis of essential oils please contact John Edwards

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Solid-State 13C NMR Analysis of Herbal Supplements

Solid-state 13C NMR is an excellent way to investigate what chemical functionality is present in herbal supplements. The large resonances at 60-105 ppm are due to cellulose/polysaccharides and some sugars. The peaks in the 0-60 ppm region are aliphatic carbons in fatty acid chains. Peaks in the 110-140 ppm region are alkene and aromatic carbons, while peaks in the 140 ppm and 150 ppm region are due to substituted aromatics and phenolic carbons. Peaks in the 160-200 ppm region are due to carboxylic acids, esters and amides. Solid-state NMR is a relatively simple technique that involves no sample preparation and observes the sample carbon chemistry in it's entirety. The analysis reveals relative amounts of chemical functionality that can be utilized for product-to-product comparison or batch-to-batch manufacturing comparison. The chemical specificity of the technique also means that adulterants can readily be detected and identified. A few examples of "off the shelf" herbal supplements are shown below. Figure 1: 13C CP-MAS NMR of Cranberry Extract, Green Tea Extract, and Milk Thistle Extract Figure 2: 13C CP-MAS NMR of Black Cohosh Root Extract, Echinecea Powder, and Bilberry Extract Figure 3: 13C CP-MAS NMR of Valerian Root Extract, Ginseng Extract, Saw Palmetto Extract, Grape…

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Benchtop Permanent Magnet High Resolution NMR Systems

The latest buzz in the NMR news release world has been the emergence of the 45 MHz picoSpin (www.picospin.com) miniature NMR system that boasts shoe box size dimensions, a resolution of 80 ppb (3.5 Hz at peak half height), and a tiny 300 micron probe dimension. The sample can be injected with a syringe or pump. A number of application examples and spectra are posted on the application pages of the company website. It is noted that the spectra require the signal averaging of 24-200 pulses requiring an estimated experimental time of 3-10 minutes The system claims to be the first miniature NMR system but I guess that depends on how you define "miniature". A number of "relatively small" high resolution permanent magnet NMR systems operating at 60 MHz have been around since the early '90s (Elbit-ATI, FoxboroNMR, Qualion, ASPeCT-MR, and ACT). The picoSpin NMR is definitely the first spectrometer to deliver high resolution NMR from such a small footprint permanent magnet combined with a capillary probe. The S/N of the picoSpin system is approximately 300:1 on a one pulse spectrum of water. On our 60 MHz systems we are routinely obtaining, non-spinning, one pulse spectra without signal apodization with…

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IFPAC Conference: Process NMR Associates and University of California, Davis to Present Process NMR and MRI Short Course Prior to Meeting

Short Course on Process NMR and MRI to be presented at the IFPAC Meeting (http://www.ifpac.com/) When: Monday, January17, 1:00pm to 5:00pm, and continues on Tuesday January 18, 8:00AM to 12 noon Location: Baltimore Marriott Waterfront Instructors: Michael J. McCarthy, Professor of Engineering, University of California, Davis, CA Paul J. Giammatteo, Ph.D., Process NMR Associates LLC, Danbury, CT The course is specifically designed and organized for industry professionals who want to add to their knowledge-base on magnetic resonance and process analytical technology. Topics include compositional analysis, rheological characterization, measurement of the state of mixing, visualizing transport and product stability as well as recent advances in process magnetic resonance sensors. This course will bring you up-to-date on the latest information concerning the applications and state-of-the art instrumentation for process magnetic resonance. Outline: * Introduction to Process NMR Magnetic resonance theory - Time-domain, High resolution, Diffusion, Imaging * Hardware - Spectrometers, magnets, probes * Coupling the sensor to the process * Applications will include: - Composition measurement - Property measurement - Rheology measurement - Product structure For Details contact Paul Giammatteo Tel: (203) 744-5905 or Michael McCarthy Tel: (530) 752 8921

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Press Release: IASC Chooses Process NMR Associates to Provide Analytical Services for Certification Program

The International Aloe Science Council (IASC), a trade association representing the global aloe vera industry, has selected Process NMR Associates, LLC (PNA) as its primary provider for Nuclear Magnetic Resonance (NMR) spectroscopic measurement of aloe vera in regards to the organizations seal-based certification program. PNA’s services include measurement of aloe vera concentration, sacharride distributions, formulation ingredients, and, contaminant/degradation products, in aloe vera powders, whole leaf extracts, whole leaf and inner leaf gel concentrates, drink concentrates, and, ready to drink formulations. The IASC certification program, which offers manufacturers the ability to place a seal on products demonstrating that it meets the established standards for quality and purity of aloe vera products available in the marketplace, has elected to use quantitative 1H NMR analysis as a means to determine compliance. “We are pleased to partner with Process-NMR Associates for providing analytical services related to the certification program,” said Devon Powell, Executive Director of the IASC. “PNA has demonstrated its capability to provide excellent analytical services in a timely manner to the organization and aloe vera industry at-large.” PNA performs the NMR methodology prescribed by IASC, quantifying constituents such as acemannan, and glucose, identifying breakdown products such as acetic acid, lactic acid, pyruvic…

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Process NMR Associates to Present at 3 Meetings

I will be presenting a poster and two invited talks at three meetings this Summer and Fall. The first meeting is Petrophase XI 2010 (11th International Conference on Petroleum Phase Behaviour and Fouling) in Jersey City, NJ, June 13-17 - my poster is entitled: "Improved Approach to the Calculation of Average Molecular Descriptions of Heavy Petroleum Hydrocarbons by Combined Analysis by Quantitative 13C and DEPT-45 NMR Experiments". The poster describes a new methodology for 13C NMR analysis of heavy petroleum materials based on quantitative 13C and DEPT experiments which can be used in combination to calculate an average aromatic cluster size that is consistent with other analysis techniques. Published approaches being used currently underestimate the size of the aromatic groups in heavy petroleum materials. In July I will be presenting an invited talk: "A Self-Employed Application Chemists Odyssey in the World of Analytical Instrument Development The Viability of a $50K High Resolution NMR and $15K ESR Spectrometers", at the University of South Dakota, Vermillion, SD. The date has yet to be set. I will be presenting an invited talk in a session on reaction monitoring with NMR at SMASH 2010 in Portland Oregon, September 26-29 - my talk is entitled:…

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Process NMR Associates – Journal Article Published

An article by Dr. John Edwards of Process NMR Associates and researchers at the Southern Regional Research Center of the US Department of Agriculture (Dr. H.N. Cheng, Lynda H. Wartelle, K. Thomas Klasson) has been accepted for publication in the Elsevier Journal Carbon. The paper entitled "Solid state NMR and ESR studies of activated carbons produced from pecan shells" is available at the following link: Carbon Paper . Process NMR Associates provided the solid-state 13C NMR, TD-NMR, and ESR spectroscopy for the analysis of the activated carbons derived from pecan shells.

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Permanent Magnet Based NMR for Omega-3 Fatty Acid Analysis

We are currently developing a spinner system for the process NMR system in order to improve spectral resolution sufficiently to quantify omega-3 fatty acids in fish oils. The omega-3 fatty acid methyl group can be discerned in the 1H spectra currently produced by the spectrometer but improvement can be made with sample spinning which will improve the quantitation.

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NMR Post-Processing Freeware

It was announced this week that the ACD NMR Processor Academic Edition is freely available for non-commercial use and can be downloaded from the ACD Website. Other Windows based NMR processing software packages are available and here is a listing of where they can be downloaded: 1) SpinWorks - written by Kirk Marat at the University of Manitoba - Download Here 2) GSim - written by Vadim Zorin Download Here 3) RNMR (Requires R Statistical Freeware Package) - Download Here - R Software can be obtained here 4) MatNMR (Requires MATLAB) - Download Here 5) Hires - Download Here

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Digital Spectrometers Will Change the Marketplace for NMR Technology

Digital Spectrometers based on field programmable gate arrays will soon change the face of NMR spectroscopy as a routine use analytical instrument. Stan Sykora in his excellent blog (http://www.ebyte.it/stan/blog07.html#07jun14) describes how the transition of NMR spectrometers to digital electronics has drastically reduced the footprint and price of NMR spectrometers and increased the potential complexity of the RF synthesis as well as the NMR post processing on the same chip. In fact single chips can hold multiple spectrometers enabling the building of single spectrometers that can perform experiments on multiple magnet systems. One of the best journal articles on the topic is by Kazuyuki Takeda "OPENCORE NMR: Open-source core modules for implementing an integrated FPGA-based NMR spectrometer", Journal of Magnetic Resonance, 192(2), 218-229, 2008. This gentleman also included all the core modules, console software, pulse programs and board designs required to build your own spectrometer (see Opencore Website). The availability of superconducting NMR magnets are still the barrier to entry for cheaper high field NMR systems but in the lower field NMR area these spectrometers will enable a drastic reduction in instrumentation cost and perhaps lead to a larger NMR market. In the near future I feel that NMR systems in…

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Reaction Monitoring by Process NMR

Presented here are several simple reactions monitored by 60 MHz process NMR performed in a 5 mm NMR tube. Reaction #1: Acetic Anhydride in Water - Reacts to form Acetic Acid NMR Monitored Reaction Profile Reaction #2: Acetic Anhydride + Excess of Methanol + Acid - Yields Acetic Acid and Acetic Methyl Ester First Reaction was Performed without Shaking the Sample before Observation NMR Monitored Reaction Profile Second Reaction was Performed with a vigorous shake of the NMR tube before observation. NMR Monitored Reaction Profile For More Information Contact John Edwards

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Examples of 60 MHz Process NMR Spectral Resolution

These are non-spinning spectra obtained on a Qualion process NMR spectrometer operating at 58 MHz. The spec on water at this shim level is 1.5/5/20 Hz at 50%/10%/0.5% peak height. The first spectrum is of 91% isopropyl alcohol in water - store bought pharmacy product. The second spectrum shows the comparison of a 300 MHz 1H NMR spectrum of Advil compared to a non-spinning 58 MHz spectrum.

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