Nicole Kruse (Bruker) What can NMR do for the chemist? Introduction to experiments beyond 1D proton and carbon spectra
Topics will include
– 2D experiments commonly used for structure verification
– Examination of NMR active nuclei for inorganic chemist
– Introduction to Magic Angle Spinning (HR-MAS and MAS) methods
– Triple resonance bio-molecular NMR
Sonya Havens (IISD Experimental Lakes) The Experimental Lakes Area: Whole ecosystem aquatic research since 1968
– Richard Shoemaker (Bruker) What’s New with Bruker in 2017 ?
– Scott Kroeker (University of Manitoba) Expanding the NMR palette: multinuclear magnetic resonance of glasses, coordination polymers and paramagnetic solids
– Melanie Martin (University of Winnipeg) Measuring the Microscopic Using Magnetic Resonance Imaging
Who should attend
Scientists, Industry, NMR managers & NMR Facility Technologists, Post-doctoral Fellows and Graduate Students
Registration fee: $30 (including lunch), free registration for students
To celebrate the re-opening of QANUC (Quebec / Eastern Canada High-Field NMR Facility) with the installation of the new 800 MHz NMR instrument and the addition of EPR to the McGill Chemistry Magnetic Resonance Facility, we are holding a symposium on Friday July 21st.
In the morning, NMR talks will start off with an opening lecture by Prof. Christian Griesinger (MPI Gottingen) and include talks from local users Kathy Borden, Nick Doucet, Pascale Legault and the QANUC Director, Anthony Mittermaier. In parallel, an EPR workshop run by Bruker will take place in the EPR lab.
Lunch and lab tours will be followed by EPR talks featuring John McCracken (Michigan State University), Gunnar Jeschke (ETH Zurich), Sushil Misra (Concordia), and Scott Bohle (McGill). The theme is “What EPR Can Do For You” and anyone interested in EPR is welcome! Also in the afternoon, Tara Sprules will lead a workshop on multi-dimensional data processing using NMRPipe (geared towards grad students/postdocs that are actively working on an NMR project).
Visit the website for more information and to sign up (required). Contact Robin Stein for information about the EPR workshop and talks and Tara Sprules for information about the NMR workshop and talks, and please forward this to anyone who might be interested.
Using NMR-based screening for quality and authenticity analysis
With food authenticity of growing concern, honey is one of the foods under increasing scrutiny and its production is now subject to a number of regulations designed to ensure authenticity and quality. Honey producers and quality control laboratories now require increasingly sophisticated methods of analysis. Here we explore how nuclear magnetic resonance (NMR) based screening provides a cost efficient, complete analysis, which can be used reliably to ensure the honey that reaches consumers is ‘exactly what it says on the tin’.
Honey production challenges
The rules and regulations surrounding the content, labeling and even the very nature of components within honey are the subject of growing debate. With numerous contested environmental, ecological and personal health issues to consider, modern honey manufacturers are faced with the challenge of meeting a host of variable regulations and ensuring consumer protection.
Honey is in high demand but low supply, and we have seen the number of adulterated products in the market rise sharply in recent years. Adulteration can include the addition of other sugars, such as high-fructose corn syrup, as well as the declaration of the wrong geographic region of origin, and is becoming much more difficult to detect.
The authentication of food products is of primary importance for both consumers and the food industry, spanning all levels of the production process. With a number of food scandals in recent years, the European Commission now encourages the use of analytical methods to determine the authenticity and quality of honey products. To beat the fraudsters, honey producers and quality control laboratories therefore require increasingly sophisticated methods of analysis. Here we explore how nuclear magnetic resonance (NMR) based screening provides a cost efficient complete analysis, covering all aspects related to authenticity, quality control and quantification.
The quality and authenticity of honey
Honey is defined as the natural sweet substance produced by honeybees and consists mainly of sugars, but also contains acids, minerals, vitamins and amino acids. The composition of honey is mostly dependent on its floral source, and this also enables the region of production to be determined. The supply of honey is greatly influenced by fluctuations in weather, and this factor combined with the declining bee population and its high production cost, makes honey particularly susceptible to adulteration.
The addition of sweetening agents to a product labelled and sold as honey is both illegal and unethical. This is a form of economic adulteration as it is done for financial gain by decreasing the value of the product without notifying the buyer. This method is particularly damaging to the industry as a whole as it affects consumer opinion.
Due to the increasingly international nature of the food market, the import and export of honey has significantly increased over recent years. This extends concerns beyond domestic honey production and authenticity to issues of product quality and global quality standards. There is rising demand for international bodies and governments to intervene in the quality control of food products to protect the health and safety of consumers, particularly as some common honey adulterants, including gluten and beet sugar, are allergenics.
Analyzing honey – a new approach
There are several methods available for the determination of honey authenticity. However, many techniques provide insufficient sensitivity and poor selectivity when faced with complex food matrices, and so cannot be used to simultaneously determine authenticity and adulteration. Now, NMR can provide an efficient and cost-effective turnkey solution.
A development from Bruker demonstrates how NMR may be used for comprehensive honey analysis. Using the new Honey Profiling module of the FoodScreener platform, both targeted and non-targeted analysis was conducted. This allowed for the simultaneous identification and quantification of a large number of compounds in one single measurement needing only one calibration standard.
Based on 400 MHz NMR spectroscopy, the principle relies on the acquisition of the spectroscopic fingerprint specific for each individual sample. This method has already proved successful for providing a sample type-specific and fully automated push button solution for fruit juice and wine, delivering reliable targeted and non-targeted multi-marker analyses with reduced cost per sample.
Using the NMR based technique on honey, it proved possible to identify and quantify more than 30 parameters, including proline, sucrose and valine, as shown in Figure 1. The table also includes a visualization of the comparison against the distribution taken from the reference database for each compound. This enables the direct detection of atypical concentrations.
Verification models were used for non-targeted analysis by comparing the whole NMR profile of a specific sample with the corresponding group reference spectra database. All spectral data points are taken into account irrespective of whether the signals are caused by previously identified molecules or not, resulting in a NMR profile such as the one shown in Figure 2.
Figure 1 shows representative chromatograms of all nine sulfonamides investigated at 0.1 ppb in honey with peak-to-peak (PP) S/N ratio. The S/N ratio for all nine sulfonamides in honey matrix at 0.1 ppb was well above 10, while Figure 2 clearly shows the blank honey matrix contained none of the targeted sulfonamides.
The origin of production plays a crucial role in the analysis of the authenticity of honey samples. Figure 3 shows the validation of the geographical origin of a polyfloral honey from Central America. By incorporating extensive databases it is possible for NMR based screening solutions to incorporate stringent validation conditions including participation in ringtests.
By simultaneously combining targeted and non-targeted analysis, NMR based screening of honey provides the complete solution for quality control and the detection of frauds, such as added syrups or sugar solutions, including unexpected and even unknown frauds. This makes the technique particularly cost efficient as it reduces the number of samples required and increases laboratory throughput. NMR therefore provides the ideal screening solution for quality control and government regulatory laboratories, by delivering a reliable, push button solution that even non-experts can use to accurately determine quality and authenticity of honey.
 Codex Alimentarius. 2001. Revised codex standard for honey (No. CODEX STAN 12-1981, Rev 1 (1987), Rev. 2 (2001)).
Business owners, consumers helped by NMR measurements of polyphenols
Olive oil is known to have health benefits, from reducing the risk of heart disease and diabetes to providing anti-inflammatory and cognitive benefits. What is less well known, however, is that the health benefits vary greatly depending on the specifics of the particular olive oil. That’s why consumers who want the health benefits of olive oil could use some guidance when they face dozens of options at the store.
Based on an analysis of scientific studies, the European Food Safety Authority (EFSA) concluded five years ago that the “consumption of olive oil polyphenols contributes to the protection of blood lipids from oxidative damage.” The higher the polyphenol level, the greater the health benefits. Importantly, the processing involved in producing pure, regular or light olive oil destroys the crucial phenols. Only true extra virgin olive oils (EVOO) retain important polyphenols, such as oleacein and oleocanthal. Even among EVOOs, levels vary greatly.
As consumers become savvier shoppers, olive oil producers are increasingly interested in touting the specifics of the oil they make. To avoid misleading labels, some countries set minimum oleocanthal and oleacein requirements for an oil to be termed EVOO. Early harvest EVOOs, which boast some of the highest polyphenol levels, must meet additional standards, including having the olives picked by dates determined based on geography and climate.
Recently, business leaders from the Halkidiki region of Greece asked experts in the Laboratory of Pharmacognosy and Natural Products Chemistry at the University of Athens to measure the polyphenol levels in the region’s current early harvest olive oil. The university employed a method first described in the paper, “Direct Measurement of Oleocanthal and Oleacein Levels in Olive Oil by Quantitative H-1 NMR. Establishment of a New Index for the Characterization of Extra Virgin Olive Oils.” The research, by Evangelia Karkoula, Angeliki Skantzari, Eleni Melliou and Prokopios Magiatis, was published in the Journal of Agricultural and Food Chemistry on November 2, 2012.
When the researchers began, they set out to develop a fast and accurate method of measuring the olive oil content of oleocanthal and oleacein. Because these polyphenols react with water and methanol, commonly used chromatographic methods were problematic. The researchers created a new way to extract polyphenols from olive oil without using any reacting solvents. Then they directly measured oleocanthal and oleacein levels using q1H NMR. They recorded the spectra using a Bruker Avance 600.
The results illustrated that oleocanthal and oleacein levels are highest in oils made from olives harvested early in the season. While most EVOOs are labeled with the date by which the oil is best consumed, few have information about when the olives were harvested. The basic rule of thumb is that olive oil with a slightly bitter taste and greenish hue, sold in a container that shields the oil from light, is more likely to have higher levels of oleocanthal and oleacein. While that basic rule might be somewhat helpful, actual data about polyphenol content is more useful, and useful information was exactly what the olive oil makers from Halkidiki wanted.
To gather data, scientists at the University of Athens laboratory used the q1H NMR methods demonstrated in the pivotal 2012 paper. They found that the average polyphenol content in early harvest Halkidiki olive oil was 495 mg/kg, significantly higher than the international average of 330 mg/kg. With data in hand, producers are making the case to consumers that Halkidiki early harvest olive oil has high nutritional value.
Given the variation in health benefits, as well as differences in price and availability, consumers benefit from knowing the polyphenol content of various olive oils. An NMR-based method, along with increasingly widespread and strict labeling requirements, will help consumers when they find themselves looking at shelves stocked with olive oil offerings.
For more information:
Olive oil as medicine: the effect on blood lipids and lipoproteins Mary Flynn, PhD, RD, LDN and Selina Wang, PhD, March 2015, UC Davis Olive Center at the Robert Mondavi Institute
Baiano A TC, Viggiani I, Nobile MAD. Effects of cultivars and location on quality, phenolic content and antioxidant activity of extra-virgin olive oils. J Am Oil Chem Soc 2013;90:103-111
Hernáez A, Fernández-Castillejo S, Farrás M, et al. Olive oil polyphenols enhance high-density lipoprotein function in humans: a randomized controlled trial. Arterioscler Thromb Vasc Biol 2014;34:2115-9.
Bruker’s TopSpin™ software package for NMR data analysis and the acquisition and processing of NMR spectra. TopSpin was designed with a highly intuitive interface utilizing the most widespread standards familiar from word processing, graphics or presentation programs, providing the same look-and-feel for your NMR applications on Windows®, Linux®, and Mac.
TopSpin for Mac OS X joined Windows and Linux as supported operating systems, providing NMR scientists in academia and industry with the ability to use the operating environment of their choice for processing.
And now academic users have unlimited access to the best tools for NMR processing for free! Click the link to download your free version of TopSpin Processing and start taking advantage of its full capabilities.
Nuclear magnetic resonance (NMR) spectroscopy is a technique that detects the chemical environment of atomic nuclei by the absorption of radio-frequency electromagnetic radiation when in the presence of a high magnetic field. NMR is used in chemistry and related fields for high-resolution molecular structure determination and the study of molecular dynamics.
An international team of researchers has greatly expanded the potential for NMR analysis apparatus. They have made it possible to measure all the signals of a substance with a single, newly developed miniature antenna, while in current equipment several – very expensive – antennas are needed to do so. Moreover, only a few nanolitres of a substance are needed to conduct measurements. Previously, half a millilitre was required. The broadband mini-antenna, with a reduction factor of 20,000, provides unprecedented possibilities for using NMR in scientific research.
Nuclear Magnetic Resonance (NMR) spectroscopy (related to Magnetic Resonance Imaging – MRI– the widely used medical imaging technology) is one of the most powerful analytical technologies for molecular research. Because the various atoms in a molecule each have specific vibrational frequencies, NMR technology can conclusively establish the identity of a molecular structure. The mini antenna, developed by the research team of scientists from Wageningen University, the University of Twente and institutions in Spain and Italy, has a much broader frequency range than the existing apparatus. With this new antenna, the NMR frequencies of all elements can be measured simultaneously, which makes the apparatus not only much easier to use, but also much less expensive.
NMR spectroscopy is crucial to many fields of research, such as in determination of the structure of proteins, in drug research, for developing new materials and optimisation of catalysts. The Netherlands take a leading position in worldwide NMR research. For example, the national NMR-NL consortium (where the universities of Eindhoven, Leiden, Nijmegen, Utrecht and Wageningen join forces) develops state-of-the-art apparatus and applications. The innovative miniature antennas can be used in current and future NMR apparatus, and can also be used in the development of miniaturised NMR equipment.
Molecules consist of atoms of various elements (such as hydrogen, carbon, oxygen, fluorine or phosphorus). In classical NMR apparatus, to measure an element a special antenna must be tuned to the specific frequency of that element. It is analogous to a radio: to listen to a specific radio station (in this analogy, ‘an element’), the radio must be tuned precisely to the frequency of that station. With the new mini-antenna, however, it is possible to ‘listen’ to all frequencies simultaneously. Although listening to all radio stations simultaneously would not be ideal for radio, this innovation provides many new possibilities for studying molecules with NMR apparatus.
Read more at: http://phys.org/news/2014-01-team-refines-nmr-analysis-apparatus.html#jCp
The Fall Training for the new users will take place on Thu. September 24, 2015 at
11:00 a.m. to 4:00 p.m. All new users are required to complete a request
for training form downloadable online and sign up for web site access.
The Training for the new users will take place on Friday May 22, 2015 at 10:30 a.m. to 4:30 p.m. All new users are required to complete a request for training form downloadable online and sign up for web site access at http://whmis.uwinnipeg.ca/nmr/?page_id=67
Please let me know if you have any question and concern.
The Training for the new users will take place on Tuesday September 16, 2014 at 10:30 a.m. to 4:30 p.m. All new users are required to complete a request for training form downloadable online and sign up for web site access at http://whmis.uwinnipeg.ca/nmr/?page_id=67
Please let me know if you have any question and concern.