NMR Method Patented to Determine Presence of Organic Sub-Structures in Molecules
Bristol-Myers Squibb researchers have patented a methodology to determine the presence of particular molecular substructures in compounds by PCA analysis of NMR spectroscopy data. This analysis is performed on entire spectra or particular regions defined by the substructures of interest. US Patent 6,895,340
Ex-Situ NMR available for license from Berkley Lab
Ex-situ NMR (US Patent 6,652,833) is currently available for license from the Lawrence Berkely Lab. This NMR analysis is described in a paper presented in Physique and in the following Science article (“High-Resolution NMR Spectroscopy with a Portable Single-Sided Sensor” by J. Perlo, V. Demas, F. Casanova, C. A. Meriles, J. Reimer, A. Pines, and B. Blumich (2005). Science 308: 1279-1279
Spoilage of Wine observed by NMR of Intact Bottles
A large bore superconducting magnet and specialized probe is all that is required to check that your $4500 bottle of Mouton Rothschild 1865 is not a extraordinarily expensive bottle of vinegar US Patent 6,911,822. See also this magazine atricle and the website of the company that is using the first commercial system in Morristown New Jersey – Wine Scanner Inc
Patented NMR Method for Quality Control of Medicinal Natural Products
Pattern recognition technology in conjunction with 1H and 13C NMR spectroscopy is used to determine the standard specification expected for medicinal grade natural products – see US Patent 6,806,090
Food Authentification by SNIF-NMR
Gérard Martin of Eurofins Scientific, CNRS, Nantes University, Nantes – France, writes:” Methodology: No dramatic improvement in NMR instrumentation originated during the last decade where an 11.4 T spectrometer, fitted with dedicated 2H{1H} probe and a 19F locking canal represents a good compromise between cost and efficiency. Since the main challenge for 2H-SNIF-NMR is to overcome its low sensitivity, efforts were directed in this way. The cheapest solution is to avoid the use of an internal reference that spares room in the cell for more molecules of interest and this can be done in two ways. First, the isotope ratios may be computed from the molar ratios of the deuterium isotopomeres, and the overall (D/H) value measured by Mass Spectrometry (IRMS). An alternative is to replace the chemical reference by an electronic signal conveniently generated (ERETIC method).
Wines and juices: Since 1991, the European data bank on wines has been established years after years and contains now the isotopic data of several thousands of wines from the main producing countries in Europe. Illegal enrichment of wines can be checked out and, according to the pertinence of the data bank, geographic origins of QWPSR wines can be controlled. Private ventures took also an interest in building up specific databanks of wines from third countries. The market of fruit juices has been stabilized by SNIF-NMR and the quantity of sucrose added in pure juices has been severely reduced. A joint approach using SNIF-NMR and IRMS is very useful for fighting against other sophisticated frauds.
Aromas and perfumes: The replacement of vanillin from beans (Vanilla Planifolia) by synthetic vanillin is an old practice and during thirty years, isotopic methods (IRMS and SNIF-NMR) were a nightmare to the fraudsters. Biotechnology forms the subject of the last serial of the vanillin saga: vanillin obtained from ferrulic acid by fermentation has been declared “natural” providing that all the steps and ingredients taking part in its manufacture are “natural”. The potentiality of isotopic analysis for solving the problem of the natural status of biotechnological vanillin will be discussed. Progresses in the authentication of aromatic molecules obtained from the shikimate pathway and of monoterpenes bio synthesized according to the deoxyxylulose pathway are also pointed out.
Miscellaneous applications of SNIF-NMR: During the last decade, fats and oils, fishes, dairy products and coffees received a great attention form the official and private laboratories in charge of the consumer protection. Legal (tobacco) and illegal (heroin) drugs have also been authenticated by SNIF-NMR.”
See also – Eurofins Site, and the following papers in The Chemical Educator (Elsevier), and this US Customs Service Report, explain the technique and a simple application very well.
SNIF NMR methodology has actually been patented US Patent 6,815,213, US Patent 4,550,082.
An excellent overview of where NMR analysis fits in the isotopic methods utilized in the European Union to detect fraudin food products is given by the European Commission’s Joint Research Centre
See Process NMR Associates for your NMR analysis needs.
13C NMR Analysis for Authentification of Gum Arabic
35 samples of Gum Arabic (acacia senegal) were analyzed by 13C NMR spectroscopy and the “average 13C NMR peak relative intensities” were calculated. This average 13C NMR signature can be used to determine the authenticity of a gum arabis sample and allows for observation of adulterants which are typically gums from other tropical trees (eg. gum talha (Acacia Seyal), Combretum, etc.). 13C NMR has been suggested as a specification of Gum Arabic quality in the following paper:“Gum arabic (Acacia senegal): unambiguous identification by 13C-NMR spectroscopy as an adjunct to the Revised JECFA Specification, and the application of 13C-NMR spectra for regulatory/legislative purposes.” by Anderson DM, Millar JR, Weiping W., Chemistry Department, University, Edinburgh, UK. Published in Food Additives and Contaminants, 1991 Jul-Aug;8(4):405-21
See Process NMR Associates for your 13c analysis needs.
NMR Database - Essential Oils and Carrier Oils
PNA has created and extensive NMR database comprising 160+ Essential Oils and 40+ Fixed Oils.Process NMR Associates is interested in developing a comprehensive database of NMR data that can be correlated to GC/GCMS data.If you have essential oils that have GC or GCMS data associated with them, we would be happy to provide you with a free 1H/13C analysis in exchange forincluding your EO and analytical data into the current database. Contact John Edwards if you are interested.The database includes 1H and 13C NMR spectra of the following oils:
Essential OilsAjowan EO Trachyspermum copticum – India (seed)Allspice Berry EO Pimenta officinalisAmyris EO Amyris Balsamifera – JamaicaAngelica Root EO Angelica archangelicaAngelica Seed EO Angelica archangelicaAnise Seed EO Pimpinella anisumArmoise EO Artemesia herba alba – MoroccoBalsam Peru EO Myroxylon balsamumBalsam Tolu EO Myroxylon balsamum – El SalvadorBasil EO Ocimum basilicumBay Leaf EO Pimenta racemosaBay Laurel EO Laurus nobilus – JamaicaBenzoin Liquid Resin Benzion Styrax – ChinaBergamot EO Citrus bergamiaBirch Sweet EO Betula lentaBlack Pepper EO Piper nigrum – IndiaBlood Orange EO Citrus sinensis var.Bog Myrtle EO Myrica gale – EuropeCabrueva EO Myocarpus fastigiatus – South AmericaCade EO Juniperus oxycedrus – SpainCajeput EO Melaleuca cajeputiCalamus EO Acorus calamusCamphor EO Cinnamomum camphoraCananga EO Cananga odorataCaraway Seed EO Carum carviCardamom Seed EO Elattaria cardamomumCassia EO Cinnamomum Cassia – ChinaCatnip EO Nepeta catariaCarrot Seed EO Daucus carotaCedarwood EO Cedrus atlanticaCedarwood Atlas EO Cedrus atlantica – MoroccoCedarwood Chinese EO - Cupressus funebris – ChinaCedarwood Himalayan EO Cedrus deodara – HimalayaCedarwood Mexicana EO Juniperus mexicana – Mexico (also Texas Cedarwood)Cedarwood Virginian EO Juniperus Virginiana – USACedar Leaf EO Thuja occidentalis – USACelery Seed EO Apium graveolensChamomile German EO Matricaria chamomillaChamomile Egypt EO Matricaria chamomillaChamomile Spain EO Matricaria chamomillaChamomile Roman EO Anthemis nobilisCinnamon Bark EO CinnamomumCinnamon Leaf EO Cinnamomum zeylanicumCitronella EO Cymbopogon nardusCitronella Sri Lanka EO Cymbopogon nardusCitronella Java EO Cymbopogon winterianusClary Sage EO Salvia sclareaClove Bud EO Eugenia caryophyllataClove Leaf EO Eugenia caryophyllata – MadagascarCopaiba Balsam EO Copaifera officinalisCoriander Seed EO CoriandrumCumin EO Cumimum cymimumCypress EO Cypressus sempervirensCypriol EO Cyperus scariosus – Brazil (Flowers)Davana EO Aretemesia pallensDill Seed EO Anethum sowa – IndiaDill Weed EO Anethum graveolensDragons Blood EO Croton lechleri – South America (Resin)Dwarf Pine EO Pinus mugoElemi EO Canarium luzonicumEucalyptus Citriodora EO Eucalyptus citriodoraEucalyptus Globulus EO Eucalyptus globulusEucalyptus Radiata EO Eucalyptus radiataEucalyptus Spain EO Eucalyptus globulusEucalyptus China EO Eucalyptus globulusEucalyptus Smithii EO Eucalyptus smithii – China (leaf)Fennel Sweet EO Foeniculum vulgareFennel Hungary EO Foeniculum vulgareFennel Spain EO Foeniculum vulgareFennel Rectified EO Foeniculum vulgareFennel Sweet EO Foeniculum vulgareFir Needle EO Abies albaFir Siberian EO Abies sibirica – Austria (Needle)Fir Canadian EO Abies balsamea – USA (Needle)Frankincense EO Boswellia carteriGalbanum EO Ferula galbaniflua – Turkey (Gum)Garlic EO Allium sativum – Mexico (Bulb)Geranium EO Pelargonium graveolensGeranium Rose EO Pelargonium roseum – FranceGinger EO Zingiber officinaleGinger Grass EO Cymbopogon martini – ChinaGrapefruit Pink EO Citrus paradiseGuaiacwood EO Bulnesia sarmienti – ParaguayHelichrysum EO Helichrysum angustifoliumHelichrysum Italicum EO Helichrysum italicumHop EO Humulus lupulusHyssop EO Hyssopus officinalisJuniper Berry EO Juniperus communisLabdanum EO Cistus labdanumLantane EO Lantara camara – MadagascarLavandin EO Lavendula latifoliaLavender EO Lavendula angustifoliaLemon EO Citrus limonLemongrass EO Cymbopogon citratusLemon Myrtle EO Backhousia citriodora – AustraliaLime EO Citrus aurantiumLime (Distilled) EO Citrus aurantifoliaLime (Cold Pressed) EO Citrus aurantifoliaLitsea Cubeba EO Litsea cubeba – ChinaMace EO Myristica fragrans – Spain (Husk)Mandarin EO Citrus reticulataMarjoram EO Origanum majoranaMelissa EO (Lemon Balm) Melissa officinalisMint Brazil EO Mentha arvensisMint China EO Mentha arvensisMint Japan EO Mentha arvensisMugwort EO Artemisia vulgarisMullein EO Verbascum thapsus – India (Leaf)Myrrh EO Commiphora myrrhaMyrtle EO Myrtus communisNeroli EO Citrus Aurantium – EgyptNiaouli (Cineole) EO Melaleuca viridifloraNiaouli (Nerolidol) EO Melaleuca quinquinerviaNutmeg EO Myristica fragransOat EO Avena sativaOpoponax EO Commiphora guidotti – EthiopiaOrange Bitter EO Citrus aurantiumOrange Sweet EO Citrus sinensisOregano EO Thymus capitatusPalmarosa EO Cymbopogon martiniParsley Seed EO Petroselinum sativumPatchouli EO Pogostemon cablinPennyroyal EO Mentha pulegiumPepper Black EO Piper nigrumPeppermint EO Mentha piperitaPetitgrain EO Citrus aurantiumPine Needle EO Abies sibiricaPine Dwarf EO Pinus mugo – Austria (Needle)Pine Scots EO Pinus sylvestris – Hungary (Needle Twig)Pine EO Pinus pinaster – USA (Needle)Ravensara EO Ravensara aromaticaRosalina EO Melaleuca ericifolia – AustraliaRose EO Rosa centifoliaRosemary EO Rosmarinus officinalisRosewood EO Aniba roseaodoraSage EO Salvia officinalisSandalwood EO ( Mysore ) Santalum albumSpearmint EO Mentha spicataSpike Lavender EO Lavandula latifoliaSpikenard EO Nardostachys jatamansiSpruce EO Tsuga canadensisSpruce Black EO Picea mariana – Norway (Needle)Star Anise EO Illicium verumTagetes EO Tagetes minutaTangerine EO Citrus reticulataTarragon EO Dracunculus spp.Tea Tree EO Melaleuca alternifoliaThuja EO Thuja occidentalisThyme Red EO Thymus vulgarisThyme Sweet EO Thymus vulgaris – FranceThyme White EO Thymus vulgaris – SpainTurmeric EO Curcuma longa – IndiaValerian Root EO Val ariana officinalisVerbena EO Lippia citriodoraVetiver EO Vetiveria zizanoidesWintergreen EO Gaultheria procumbenWormwood EO Artemisia absinthiumYarrow EO Achillea Millefolium – BulgariaYlang-Ylang Extra EO Canaga odorataYlang-Ylang I EO Canaga odorataYlang-Ylang III EO Canaga odorata
Carrier oilsApricot Kernel Oil Prunus armeniacaAloe Vera Oil Aloe barbadensis -USAAvocado Oil Persea americanaBorage Oil Borago officinalisCamelina Oil Camelina sativaCamellia Oil Camellia sinesis – Japan (Seed)Canola Oil Brassica napus – CanadaCastor Oil Ricinus communis – India (Seed)Coconut Oil (Fractionated) Cocos nuciferaCoconut Oil (Virgin) Cocos nuciferaCorn OilCottonseed Oil Gossypium seminis – USA (Seed)Emu OilEvening Primrose Oil Oenothers biennisFlax Seed (Linseed) Oil Linum usitatissimum – USAForaha (Tamanu) Calophyllum InophyllumGrapeseed Oil Vitis viniferaHazelnut Oil Corylus avellanaHemp Seed Oil Cannabis SativaJojoba Golden Simmondsia chinensisKukui Oil Aleurites moluccansMacadamia Nut Oil Macadamia integrifolia – AustraliaOlive Oil Olea eurpaea – ItalyPalm Oil Passiflora elacsis – USAPalm Kernel Oil Passiflora aincarnata – MalaysiaPeanut Oil Arachis hypogeae – USAPecan Oil Algooquian paccan – USAPistachio Nut Oil Pistacia vera – USARose Hip Seed Oil Rosa mosquetaSafflower Oil Carthamus tinctorius – GuatamalaSesame Oil Sesamum indicumSoya Bean Oil Soja hispida – USASunflower Oil (High Oleic) Helianthus annuusSweet Almond Oil Prunus dulcisWalnut Oil Juglans ragia – USAWheatgerm Oil Triticum vulgareAlmond Fragrance OilBitter Almond Fragrance OilCoconut Fragrance OilRosemary Oil Extract
NMR Reference: Ref: “Essential Oils Analysis by Capillary Gas Chromatography and Carbon-13 NMR Spectroscopy ” by K.H. Kubeczka and V. Formacek, 2nd Ed, Wiley, NY (2002)
Essential Oil Chemistry Reference: Journal of Essential Oil Research
See Process NMR Associates Essential Oils Page
NMR Acronyms
Excellent NMR Acronym Summary Pages – Oxford University, University of Wisconsin
NMR on a Chip
All you need to purchase with this PCI Card NMR spectrometer is an amplifier, a magnet and probe. Details can be obtained at the Spincore RadioProcessor Page. Benchtop high resolution NMR is very close to being a reality. Combining new spectrometer design with micro-probe and sample automation such as that found at Protasis will make benchtop QA-QC spectrometers a reality and place NMR spectrometers in the hands of people who can utilize them for routine testing at an affordable price.
Fat Content of Live Salmon
MOUSE NMR application on Salmon
Mobile NMR of Polyethylene Pipes
MOUSE NMR application to polyethylene pipes.
Upcoming NMR Meetings for 2006
47th ENC Conference will be held April 23 – 28, 2006, at The Asilomar Conference Center, Pacific Grove, California – Program.
EUROMAR - York will be held July 16-21, 2006 at The University of York Main Campus, Programme
22nd International Conferences on Magnetic Resonance in Biological Systems will be held August 20-25, 2006 in Goettingen, Germany – programme
6th Colloquium on Mobile NMR will be held 6-8 September 2006 in Aachen, Germany – Program
SMASH 2006 will be held September 10-13 at the Sheraton Hotel in Burlington, Vermont – Program
The NMR Symposium of the 48th Rocky Mountain Conference on Analytical Chemistry will be held July 23 – 27, 2006. The conference site is the Beaver Run Resort & Conference Center in Breckenridge, Colorado.
21st Meeting of the Central European NMR Discussion Groups will be held April 23-26, 2006, Valtice, Czech Republic in the hotel HUBERTUS in Valtice Castle
14th ISMRM will be held 6-12 May 2006 in Seattle Washington – program
ANZMAG 2006 will be held February 12-16 at the Murramarang National Park, NSW, Australia – Programme
Fast NMR Field Cycling
Stelar s.r.l of Italy manufacture a fast field cycling NMR spectrometer that shuttles a sample in and out of a varying magnetic field to generate T1 longitudinal relaxation profiles obtained by measuring T1 at a series of different magnetic field strengths. Stelar has developed low-inductance, air-coil magnets and power supplies capable of switching the field electronically to any desired value in a matter of milliseconds while, at the same time, maintaining the high field stability and homogeneity required by NMR. This allows the link between NMR relaxation phenomena and molecular dynamics to explored initially in the following application fields: the hydration of paramagnetic metal ions and organometallic complexes, the dynamics of liquid crystals, and the dynamics of proteins.
