Miniature mass spectroscopy for the masses is a dream of Graham Cooks, Henry B. Hass professor in analytical chemistry at Purdue University, Indiana, US. Cooks specialises in the construction of mass spectrometers and their use in fundamental studies and applications. Speaking at the PittCon conference in Orlando, in March 2012, he said, ‘there are billions of items of commerce that are not being analysed including food, medicine and household items. This is an area where more high quality instruments are needed’.
Early in his career, Cooks contributed to the development of tandem mass spectrometry and to desorption ionisation, especially matrix-based methods. His interest in minimising sample work-up and avoiding chromatography contributed to the development of ambient ionisation methods, including desorption electrospray ionisation (DESI). Applications of DESI in tissue imaging, forensics and pharmaceutics are under way, and have also led to the construction of miniature ion trap mass spectrometers and their application to trace chemical analysis.
Cooks’ aim is to provide both the general public and laboratory professionals with a chip-based tandem mass spectrometer in a hand-held format at an affordable price for applications in the home and for security and industrial markets, including food and environmental safety, water treatment, refineries, chemical plants, pharmaceutical manufacturing and process control.
In the lab, chemists initiate multi-hour reactions and periodically withdraw samples for analysis traditionally in an open access mass spectrometry lab. This remote analysis takes hours, decreasing the usefulness of the information and building workflow inefficiencies. Additionally, the large numbers of sample add to the central lab burden, further slowing vital feedback.
Miniature mass spectroscopy
The mass spectrometer manufacturers have been quick to respond to Cooks’ dream of miniaturisation. 1st Detect launched a miniature mass spectrometer, the MMS-1000, a research laboratory instrument capable of detecting trace levels of volatile compounds in approximately 5s. The company was formed by Astrotech to develop and commercialise miniature mass spectrometer technology originally for use on the International Space Station (ISS).
Torion Technologies displayed the latest version of its TRIDION-9 at PittCon, claiming it to be the world’s fastest and most portable capillary gas chromatograph–toroidal ion trap mass spectrometer (GC–TMS). The instrument features a low thermal mass capillary gas chromatograph (GC) with high speed temperature programming (>2ºC/s) and a miniature toroidal ion trap mass spectrometer with a nominal unit mass resolution in the 50–500Da range.
Meanwhile mass spectrometer manufacturer, Advion has come up with the expression ‘personal’ single quadrupole mass spectrometer that can rapidly identify compounds in normal phase chromatography fractions. The mass spectrometer, which has been designed for the research and process development phases in the synthetic organic chemistry market, can be used in a fume hood or next to existing bench instrumentation, enabling users to identify and monitor compounds as they are made.
Traditional mass spec
The drive for miniaturisation has not, however, deflected suppliers from developing the more traditional laboratory mass spectrometers. Shimadzu Scientific Instruments introduced the GCMS-QP2010 SE, its advanced standard gas chromatograph–mass spectrometer. The ion optical system of the GCMS-QP2010 SE comprises a high-performance quadrupole mass filter, and Shimadzu’s Optdesign simulation program provides high-quality mass spectra. Fully automated MS tuning allows users to optimise parameters easily and constantly to ensure stable mass spectra can always be obtained.
Thermo Fisher Scientific launched its Q Exactive benchtop quadrupole-Orbitrap LC-MS/MS, offering an alternative to quadrupole time-of-flight (Q-TOF) mass spectroscopy. The Q Exactive can conduct three experiments at once – identification, measurement and confirmation – in a system that is fully compatible with ultra-high performance liquid chromatography (UHPLC) separations. The technology can confirm trace level metabolites, contaminants, peptides and proteins in complex mixtures in one analytical run.
AB Sciex introduced a triple quadropole system, the TripleQuad 4500, capable of delivering 10x better sensitivity over competitive triple quadropole systems in the same mid-level class. To simplify the adoption of this next generation of LC–MS–MS technology, AB Sciex also unveiled Accelerated Lab Integration Packages at PittCon. These packages consist of not only the mass spectrometer, but also the standards, software, training, validation services and a liquid chromatography (LC) system, including the new Eksigent ekspert ultra 100 and 100-XL systems.
Liquid & gas chromatography
The Eksigent ekspert ultraLC 100 and 100-XL UHPLC systems are for high-throughput UHPLC–MS–MS analysis of residues, impurities, drugs and other analytes in complex matrices. They have been designed specifically for use in clinical research, forensic and food safety applications.
AB Sciex also unveiled the Eksigent ekspert microLC 200 System, a dedicated micro-UHPLC designed to deliver up to five times faster separations and up to four times improved sensitivity while reducing sample consumption by up to 10 times. It is stackable on the new 4500 systems and existing 5500 series systems, reducing the use of laboratory space and mobile phase costs by up to 95%.
Microfluidics specialist SFC Fluidics demonstrated its Handy LC, a portable low-cost, low pressure liquid chromatograph, which uses interchangeable and disposable columns. The company is also working on a hand-held version, the Pocket LC, which performs chromatographic separations on-a-chip.
Thermo Fisher Scientific introduced the TRACE 1300 Series GC, a compact, versatile gas chromatography system that is designed to increase productivity and lower cost in QA/QC laboratories, working on environmental, chemical and food safety applications. The TRACE 1300 GC’s simplified interface requires minimal user interaction, and can run 24/7 with limited staff.
Chemical contaminants and microparticulates that may be introduced by the sample, mobile phase or system, can reduce column lifespan and method sensitivity. Separation specialist, Phenomenex introduced SecurityGuard Ultra, a protection system that extends UHPLC column life, ideal for almost any manufacturer’s sub-2-micron or core-shell columns, including the company’s own Kinetex products.
New separation science
Waters’ Acquity UPC2 system promises to expand the applications of reversed phase liquid chromatography (LC) and of gas chromatography (GC) separations. UltraPerformance Convergence Chromatography (UPC2) is a potential tool for tackling tough-to-analyse compounds, including hydrophobic and chiral compounds, lipids, thermally labile samples and polymers.
The primary mobile phase for UPC2 is compressed carbon dioxide (CO2) which offers numerous major advantages over liquid mobile phases or carrier gases that are used with LC and GC. It is non-toxic and cheaper than volatile organic solvents and allows separations to occur at lower temperatures. Used alone, or combined with a co-solvent, CO2 is a low viscosity mobile phase that can achieve higher diffusion rates and enhanced mass transfer than liquids used in HPLC.
Hand-held spectrometers
Miniaturisation is not just the realm of mass spec. Rigaku Raman Technologies introduced the Xantus-2, a dual wavelength handheld Raman spectrometer designed to overcome the intrinsic fluorescence issues found in many materials. It is suitable for a range of applications, from the identification of illicit drugs and explosives to hazardous materials and chemical spills.
Spectro demonstrated the FluidScan direct infrared handheld spectrometer, which uses a patented optical wedge design, developed for rugged environments where moving parts are not desired. Infrared measurement is in the 950 to 4000cm-1 range,with high sensitivity in the mid infrared range.
Cole-Palmer introduced the picoSpin 45L NMR spectrometer, a miniature FT–NMR spectrometer at a cost that will enable students to gain hands-on experience of NMR technology. The technology will only handle small liquid samples but does not require cryogenics, compressed gases or a special environment.
Thermo Fisher launched the NanoDrop Lite, a compact, personal UV-Vis microvolume spectrophotometer that is designed to complement the full-featured NanoDrop 2000/2000c and 8000 instruments. The instrument is small enough to fit in a drawer, but powerful enough to help accelerate life science workflows related to sequencing, PCR/qPCR, protein isolation, antibody production, HLA typing and other applications. While NanoDrop Lite is designed with fewer features than the 2000 or 8000 series, it can deliver rapid, accurate and reproducible microvolume measurements without the need for dilutions.
Shimadzu revealed its compact UV-2600 and UV-2700 UV-Vis spectrophotometers, which feature advanced optical systems and Lo-Ray-Light diffraction gratings. In response to feedback that typical spectrophotometers are too large, these instruments are ca 28% smaller in overall size, while maintaining the same sample compartment size. In addition, they use 10% less power.
Information & laboratory management
‘Perhaps the biggest informatics challenge our customers face is seamlessly linking analytical data to enterprise-level information to facilitate business decisions,’ said Mary Ellen Goffredo, senior director, systems marketing, Waters. ‘There are software products for every analytical instrument, for laboratory workflow, for results visualisation as well as general purpose spreadsheets and word processing software. However, with so many software applications and connection points, science-driven organisations lack the ability to collect, process, consolidate and distribute laboratory data freely and efficiently.’
Waters introduced the NuGenesis 8 featuring LE (Laboratory Execution) Technologies, a workflow and documentation solution designed to overcome these problems by linking analytical laboratory data systems to business information systems. The LE technology enables global scientific organisations to stay informed, standardise processes, and implement best practices across laboratories around the world.
The technology guides laboratory analysts through routine standard operating procedures. An electronic worksheet takes them through the prescribed workflow, ensuring that they complete every step and verifying that all inputs meet established criteria. The completed task is submitted for approval and the results automatically shared with business systems such as LIMS (laboratory information management systems) and ERP (enterprise resource planning).
The efficient management of liquid and gas chromatography (LC/GC) data is essential as more industries need to comply with guidelines and regulations set out by governing bodies like the US Food and Drug Administration. LabSolutions DB software from Shimadzu Scientific Instruments provides one solution. The software can be used by laboratories that need ER/ES (electronic records and signatures) compliance but lack the IT staff required for full client/server installations.
Finally, Thermo Fisher launched Unity Lab Services, which combines laboratory support services into a single solution for customers to optimise productivity and reduce the total cost of operations.
Unity offers a range of capabilities, from traditional laboratory instrument and equipment services to enterprise-level support, including management of laboratory staffing and consumables inventory. These services can be implemented across a broad range of laboratory environments and can be scaled from service on a single instrument to a highly customised, comprehensive service programme at the laboratory, site or enterprise level.
Protein assays
Merck Millipore, the life science division of Germany’s Merck, launched the Direct Detect system for rapid, simplified protein measurement. The system measures infrared spectra of amide bonds in protein chains, without relying on amino acid composition, dye-binding properties, or redox potential. Conventional assays based on UV-Vis spectroscopy rely on absorbance by a protein’s aromatic amino acids and therefore have limited utility.
Samples are spotted directly onto a hydrophilic polytetrafluoroethylene (PTFE) membrane cards which absorb in the infrared region. The assay cards can be stored in ambient conditions without appreciable change in readout.
Protein can be detected in biological samples, including buffered solutions, in the presence of reducing agents and detergents, in the 0.2-5mg/mL range accurately and reproducibly within seconds, without any bio- or immunochemical staining.
Food testing
AB Sciex and Phenomenex are collaborating to improve food testing through the creation of a joint rapid response team. This partnership will support efforts to prevent the spread of tainted food and help increase safety of the global food supply.
Recent food contamination crises have increased the demand for faster, higher quality results and less expensive tests. Scientists from Phenomenex’s method development team and AB Sciex’s total solutions group will work with food industry experts in pesticides, antibiotics, allergens and natural toxins, to provide labs worldwide with verified analytical methodologies.
iMethods have been designed to provide the instructions and parameters of a test to identify food contamination with the highest confidence. The rapid response resource will be accessible to analysts around the world via the Internet to help them solve LC/MS issues that they face in their own laboratories.
Among the application-specific experts is Michael Quilliam at the National Research Council of Canada in Halifax, an expert on shellfish toxin analysis. He is working with AB Sciex to develop an iMethod application to improve the identification and measurement of shellfish toxins. The application will involve the National Research Council’s analytical methodology and certified reference materials.
Scientists in the rapid response unit have already developed the first comprehensive method using LC/MS/MS (liquid chromatography-tandem mass spectrometry) to test orange juice for the presence of the chemical fungicide carbendazim.
The problem has recently been in the news in North America as a result of governmental concerns that shipments from Brazil, the biggest orange juice exporter in the world, were tainted with the fungicide.
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