Spectroscopy solutions for food and environmental apps and advanced hybrid systems took center stage at Pittcon 2014.
The 65th annual Pittsburgh Conference and Exposition on Analytical Chemistry and Applied Spectroscopy (Pittcon) brought together more than 16,200 conferees and exhibitor personnel seeking the latest instrumentation and technology offerings in laboratory science. With 935 exhibitors from 32 countries occupying 1,763 booths, there was plenty of innovation to go around.
For the second consecutive year, the Food Labs Conference was held in conjunction with Pittcon. While the Food Lab Conference generally takes a more holistic approach to best practices in food management, Pittcon itself took a decidedly hard turn toward the food industry, debuting dozens of food-specific instruments, methods and applications. 
MicroRaman and other tandem/hybrid systems were also on full display, as well as compact, portable spectrometers and helium shortage solutions.
Importance of food testing
According to Chris Elliott, Chair of Food Safety and Microbiology at Queen’s Univ., Belfast, last year the UK experienced the largest reduction of consumer trust in the food supply since the 1980s. The horsemeat-sold-as-beef scandal rocked Europe, only to have further investigation reveal that 5 percent of all beef sold is contaminated. Additional statistics only worsen the trend: according to the CDC, 48 million people fall ill each year from food poisoning, 128,000 are hospitalized and more than 3,000 die. 
“Food crime is a global phenomena,” says Elliott. “Criminals are now operating in many areas of food supply systems. Currently, we are looking into how advanced mass spectrometry can be used to detect this criminal activity, and developing fingerprinting methods to determine if food has been tampered with.”
In conjunction with the Univ. of Munster, Germany, AB SCIEX, Framingham, Mass., has developed a rapid LCMS/MS method for identification of pig and horse contamination, based on the detection of biomarker peptides that are animal specific. The method uses AB SCIEX’s TripleTOF 5600 system to first identify the protein markers specific to a meat species. It then uses the QTRAP 5500 system to detect and confirm the presence of targeted meat peptides in unknown samples. The QTRAP 5500 system uses multiple reaction monitoring (MRM) to detect each peptide and confirm its identity. The mass spectrometry-based method offers a more accurate and reliable approach than other methods. It can detect markers of multiple, different animal species in a single run versus traditional methods, such as PCR or ELISA, which are prone to false negative or false positive findings. 
Waters Corp., Milford, Mass., debuted two new products that can be used in the food safety arena. The ionKey/MS System brings a new level of sensitivity, robustness and ease-of-use to LCMS. About the size of a smartphone, the ionKey is intended for use with Waters’ ACQUITY UPLC M-Class System and Xevo TQ-S Mass Spectrometer. It “plugs” into the source of the mass spectrometer, physically integrating UPLC separation into the MS, producing an improvement in sensitivity and detection, and allowing the researcher to do more with less sample. The small device contains all the tools needed to perform hundreds of reproducible separations—fluidic connections, electronics, ESI interface, column heater, eCord Intelligent Chip Technology and 1.7-µm UPLC-grade particles packed inside a 150 µm ID channel. Additionally, the system can reduce solvent use up to 90 percent, resulting in lower costs, less solvent waste and more sustainable practices.
Waters’ ionKey/MS system is a new approach for achieving excellent sensitivity, robustness and ease-of-use out of MS for applications as far-ranging as bioanalyses and pharmacokinetic studies to food safety.“Liquid chromatography and mass spectrometry are the two most important platforms in the analytical laboratory,” says Ian King, Vice President of Chemical Operation, Waters Corp. “The ionKey/MS is the first real step in the inevitable integration of the two platforms, creating a new class of product. I would go so far as to say that eventually all LCMS will done this way.”
Waters’ other product—the ACQUITY QDA Detector—won the Silver Pittcon Editors’ Award. The easy-to-use system is a mass detector for chromatographers, enabling every scientist access to mass spectral data regardless of MS experience. With the push of a button, the detector allows chemists the freedom to get mass spectral information for all their samples, on their own with no tuning. Additionally, the detector extends the limits of sample detection for a chromatographic separation by quantifying compounds having no UV response or compounds that are present at levels not detectable and quantifiable by optical detection. 
Bio-Rad Laboratories, Hercules, Calif., announced a partnership with the U.S. Pharmacopeial Convention (USP) at Pittcon 2014. The collaboration resulted in the release of a beta version of USP Spectral Library for raw material identification in food and drug applications. Powered by BioRad’s KnowItAll software technology platform, the project is an interactive, authoritative and comprehensive collection of spectral information on food and drug quality. The applications are numerous—quality standards, counterfeit foods, raw materials in finished products and more. The collaborative testing model USP is known for is executed in the new platform to ensure the highest quality spectra and standards.
Correlative, hybrid and hyphenated systems
If Pittcon 2014 made one thing clear it’s this: microscopy has become a part of the routine analytical process. The ability to measure spectra on increasingly smaller scales and see properties like never before has opened up a whole new dimension for both organic and inorganic chemists. 
JEOL, Peabody, Mass., is a pioneer in the field of correlative microscopy, and it’s increasing link with other microscopy and spectroscopy techniques. 
“Correlative microscopy is not light or electron microscopy (EM) anymore,” says Vern Robertson, JEOL’s SEM Technical Sales Manager. “It’s now mixing any other mode of analysis, whether it’s an optical microscope, an X-ray spectrometer or EDS mapping. That’s true correlative microscopy.”
“We’ve gone beyond the optical linking to the EM. What we are doing is linking organic and inorganic chemistry. For example, an EDS spectrometer gives us inorganic elemental information and MALDI gives us analytical/organic information.”
Texas Instruments’ DLP technology represents an expansion of MEMS technology into the worlds of transmittance and reflective spectroscopy.In a presentation at Pittcon, Robertson and his colleague Chip Cody, MS product manager, illustrated how they used multimodal microscopy on a stamp from 1948. 
Cody performed paper spray ionization on the stamp using JEOL’s AccuTOF DART MS system, and Robertson confirmed the analysis using the Navigator SEM. Then, Cody made a quick attempt to perform chemical imaging on the same stamp using the SpiralTOF MALDI TOF/TOF, which offers the highest available MALDI TOF resolving power up to 75,000. While it may not have been the same spatial information from an SEM, imaging with the SpiralTOF did offer complementary information to that obtained with the electron optic product line, offering unique possibilities for correlative microscopy.
“The next step will be correlation across different disciplines,” says Robertson. “Although Raman plus SEM is still in its infancy, it could be the first step in bringing all the disciplines together.”
Thermo Fisher Scientific, Waltham, Mass., showcased its DXRxi Raman imaging microscope at Pittcon. With applications in pharmaceutical, semiconductor, geology and more, the easy-to-use microscope can quickly reveal molecular structure, chemical composition and sample morphology. It can analyze large areas, providing microscopic detail in just seconds.
Renishaw’s (England) inVia, a research Raman microscope, is fully configurable, including excitations from UV through NIR, 2-D/3-D fast imaging and near-excitation analysis. The microscope can be easily combined with other techniques to perform co-localized sample analysis, including SEM, atomic force microscopy, scanning probe microscopy, confocal laser scanning microscopy and tip-enhanced Raman spectroscopy. The microscope provides a non-destructive means of obtaining chemical/molecular information, with sub-mm spatial resolution; and features accessories and configurations to suit a variety of applications areas, from nanomaterials to biology. 
AB SCIEX also combined technologies to create a unique, integrated workflow solution. CESI-MS technology is a novel combination of capillary electrophoresis (CE) and electrospray ionization (ESI) for biopharmaceutical scientists to more accurately predict efficacy, detect potential problems and reduce time to market. Specifically, CESI-MS improves ionization efficiency and reduces ion suppression as a robust technology that requires no expertise in CE or MS. Importantly, switching between LCMS and CESI-MS has been made simple to help facilitate adoption of the technology. 
The new CESI 8000 System for Biologics Characterization, a high-performance separation-electrospray ionization system for MS, features front-end CESI technology integrated with the company’s TripleTOF 5600 mass spectrometry system. The system provides orthogonal and/or superior results compared to dual-method LCMS-based approaches.  
Ocean Optics’ STS Microspectrometer is a small, CMOS-based unit that is less than 50 mm square and weighs just over 2 ounces.Compact spectrometers
The combination of low cost and small size in a spectrometer can create new applications and open up doors that previously did not exist. Portability of these powerful instruments ensures lab-quality performance in the field and on the manufacturing line. 
Dallas-based Texas Instruments (TI) debuted an innovative technology that had Pittcon attendees talking, as well as the editors, who gave the DLP4500NIR the 2014 Gold Editors’ Award. It is the first device optimized for use with NIR light and corresponding evaluation module (EVM). Incorporating DLP (digital light processing) technology into OEM spectrometers can revolutionize a researcher’s approach to traditional spectroscopy. 
“We continue to push the limits of what DLP technology is capable of, opening it up for use in advanced scientific, industrial and medical solutions,” says Mariquita Gordon, DLP Embedded manager at TI.
There are approximately 100 million digitally programmable micromirrors at the heart of DLP technology, enabling the DLP4500NIR to be a viable substitute for expensive linear detector arrays. Each of the micromirrors can be controlled to produce set patterns, with users having the ability to refine spectral resolution and wavelength ranges. This flexibility allows researchers to employ adaptive scanning techniques, optimizing material analysis for a broader range of substances than before.
The technology enables signal-to-noise ratios greater than 30,000:1 over a set measurement period for faster, more accurate results compared to spectrometers using traditional solutions. Optimized for use with 700- to 2,500-nm light, the DLP4500NIR can be programmed to select and attenuate multiple wavelengths at speeds up to 4 kHz. 
Ocean Optics’ (Dunedin, Fla.) STS-UV Microspectrometer is a compact (40 x 42 x 24 mm), high-performance spectrometer designed for integration into spectroscopy instrumentation, medical devices and other applications seeking a small footprint. The device, optimized for applications in the ultraviolet (190 to 650 nm), is anchored by a 1,024-element detector in a crossed Czerny Turner optical bench. The advanced design and detector make it comparable to much larger, more expensive spectrometer systems. Benefits include: excellent linearity, absorbance repeatability and wavelength accuracy to ensure reproducibility; and a high thermal stability performance and low baseline drift ensure that data stays accurate, even under changing environmental conditions.
“Compact” takes on a whole new meaning with the introduction of Spectroclick’s (Champaign, Ill.) Answers At Hand (AAH) line of spectrometers. The company’s mission is to provide a high-quality, low-cost spectrometer that could be carried around like a cell phone. Want to know if your water is safe to drink? No problem, just reach for your pocket spectrometer and generate a quality spectrum in minutes. 
The AAH-200, which debuted at Pittcon, utilizes a 5-megapixel USB CMOS camera and Windows software. The patent-pending grating solution uses stacked double-axis transmission grating, producing what the company refers to as SpectroBurst. 
SpectroBurst uses a webcam to capture data, then the company’s app processes the spectrum quickly, comprehensively and with more flexibility and portability than any other instrument on the market. 
The 9 x 4-cm instrument is a unique development in truly “handheld” spectrometry. And according to Alexander Scheeline, President and co-founder of Spectroclick, the technology and demand for this type of instrumentation is only going to grow. It will be interesting to see where Spectroclick, the AAH-200 and the overall home spectrometry market are come Pittcon 2015.  
Helium savers
The ongoing helium shortage has party stores, parade organizers and scientists everywhere concerned with the future of the gas. Helium is a finite, non-renewable resource; the question is not if it will run out, it is when will it? In the meantime, laboratories must cope with the increased price, which has tripled or quadrupled in some cases. 
Thermo Fisher Scientific has developed an effective solution to limit the effects of the helium crisis in the GC and GCMS industry. The Thermo Scientific Helium Saver technology—available as an instant connect module the user can easily place into a GC—allows for a single cylinder of helium to last up to 14 years under certain conditions, which is the lifetime of most GCMS instruments. 
The use of helium is optimized via a GC inlet, which is supplied with two gases: helium for the analytical column flow and nitrogen for septum purge, split flow and sample vaporization and introduction, thus eliminating the helium waste typical in a standard GC inlet. The split/splitless injector remains exactly the same, and the helium carrier gas flow through the analytical column remains the same at the specified flow rate. This allows analyses to continue without major supply concerns or extensive costs. 
Bruker Corp., Billerica, Mass., has created the first compact, single-story NMR magnet with active refrigeration technology. The Ascend Aeon 900 is a liquid nitrogen-free, superconducting magnet system with helium reliquefaction technology. It enables long-term operation without user maintenance and with essentially helium-consumption-free operation. The magnets achieve this by combining the active-shielding technology with Bruker’s advanced refrigeration designs, featuring integrated low-vibration cryo-coolers for long-term operation. 
With the Ascend Aeon 900, helium consumption is reduced by about 50 percent compared to normal magnets. Mark Chaykovsky, Executive Vice President of Bruker Corp., referred to the magnets as the “electric cars” of the NMR industry. 
“This product directly addresses helium shortage concerns,” says Chaykovsky. “(Last year), people came to us and they were worried, saying ‘what happens if this shortage continues.’ That’s why we are building this technology and know-how for the future. We expect it to gain in popularity over time.”