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Volume 87 Issue 13 | pp. 46-50
Issue Date: March 30, 2009

Cover Stories: Weathering The Crisis

New And Notable At Pittcon

Scientific instrumentation and more
Department: Science & Technology
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PITTCON EDITORS’ AWARD WINNERS

(1) The Pittcon Editors’ Gold Award for best of show this year went to inXitu for Terra, the first commercially available portable X-ray powder diffraction/X-ray fluorescence system. Technology for the instrument was originally developed by inXitu in cooperation with NASA for analyzing minerals and soils during space missions; Terra has been rebranded and is now being marketed by X-ray fluorescence specialist Innov-X Systems. Terra is designed for using X-ray diffraction to determine mineral crystalline structures and X-ray fluorescence to determine the elemental composition (Ca to U) of samples with up to 400-µm grain size. It is suitable for geological and archaeological studies or for mining operations, as well as for forensic, environmental, pharmaceutical, and petrochemical uses. The 30-lb instrument operates with a low-power X-ray source and charge-coupled device detector, runs on exchangeable lithium-ion batteries, can be controlled in person or remotely, and requires access to a spectral library.

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(2) OI Analytical and Picarro teamed up to unveil the iTOC-CRDS for total organic carbon analysis with the additional benefit of determining carbon isotope ratios in samples. The tandem instrument, which garnered the Pittcon Editors’ Silver Award, integrates OI’s total organic carbon combustion/oxidation analyzer with Picarro’s cavity ring-down spectroscopy analyzer (an alternative to a mass spectrometer)—hence the name iTOC-CRDS. The system vaporizes a solid or liquid sample to produce CO2, then determines the 13C/12C ratio of the sample. The data can be used like a fingerprint to pinpoint the origin or check for signs of adulteration of food products such as orange juice and edible oils. The iTOC-CRDS also is targeted for research on global carbon cycles to track the sources and effects of greenhouse gases and for forensic analysis of hair and teeth, among other potential applications.

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(3) Shimadzu introduced the IG-1000 particle-size analyzer that applies the novel principle of induced grating (IG) to measure nanoparticles with improved sensitivity and reproducibility over traditional light-scattering techniques. The invention received this year’s Pittcon Editors’ Bronze Award. Light-scattering sensitivity decreases sharply for particles smaller than 100 nm and requires knowing the refractive index of the sample, making it difficult to analyze unknowns. The IG method eliminates these problems by using an electrode system to organize the particles into a grid in solution, which creates an in situ diffraction grating. When the electrodes are switched off and the grating decays, the instrument uses a photodiode detector to measure the change in intensity of diffracted laser light shining through the sample. The change in light intensity depends on particle diffusion rate, which is tied directly to particle size. With this approach, particles in the 0.5- to 200-nm range can be accurately measured with equal sensitivity, even mixtures of particles or contaminated samples.

MASS SPECTROMETRY

At Pittcon 2009, instrument makers displayed the latest additions to their stables of mass spectrometers. As is usual, some of these instruments were initially launched at the American Society for Mass Spectrometry (ASMS) meeting, which was held in June 2008.

Bruker Daltonics launched the Edmass Ultra and Edmass Micro time-of-flight (TOF) mass spectrometers with matrix-assisted laser desorption ionization (MALDI) for rapid Edman protein sequencing validation. The classical Edman technique has been indispensible for N-terminal protein sequencing for decades and is currently used for sequence validation in recombinant protein production. The Edmass Ultra is a tandem MALDI-TOF/TOF instrument that is unique in its ability to map both C- and N-terminal sequences of intact proteins. The Micro is an easy-to-use, cost-effective benchtop MALDI-TOF model designed for general research and quality control. Bruker also showcased the maXis, unveiled at ASMS, an electrospray TOF mass spectrometer for MS and MS/MS operation that the company created to meet the challenging demand of coupling ultrahigh mass resolution with ultrafast chromatographic separations for quantitative proteomics, peptide, and intact protein analysis.

Shimadzu introduced the LCMS-2020 single-quadrupole instrument, which the company touts as having the world’s fastest scanning ability (15,000 daltons per second) for a single-quadrupole mass spectrometer. The LCMS-2020’s technology enables switching between positive and negative ion modes in 15 milliseconds to keep pace with ultrafast chromatography using Shimadzu’s Prominence UFLC chromatographs. To that end, the LCMS-2020 has higher sensitivity than other single-quadrupole spectrometers for accurate mass detection at the faster scan rates, which is useful for detecting impurities in very small amounts of pharmaceuticals or trace contaminants in environmental samples.

Waters exhibited its Xevo line of tandem mass spectrometers that the company expects will aid researchers in responding to FDA guidelines for understanding and eliminating sample matrix effects in bioanalytical assays, among other uses. Introduced at ASMS, the Xevo TQ MS is a tandem quadruple spectrometer for quantitative applications that features Waters’ ScanWave ion-mobility technology, which collects product ions from the first quadrupole and synchronizes their release with the scanning of the second quadrupole to improve signal intensity. The benchtop Xevo QTof MS, introduced in January, is a single-quadrupole time-of-flight spectrometer for exact mass measurements that lays claim to being the most sensitive benchtop QTof system. Paired with Waters’ Aquity ultraperformance liquid chromatograph, the QTof MS is the only commercially available system with UPLC/MS/MS capability.

JEOL unveiled the AccuTOF-GCv, a high-resolution GC/MS instrument billed as being the most sensitive for a gas chromatograph/time-of-flight mass spec combination. The AccuTOF-GCv (v stands for versatile) provides rapid data acquisition of 25 average spectra per second, high signal-to-noise ratio, and mass accuracy of 5 ppm for exact mass measurements to the 1 pg level. A key feature of the instrument is an electron impact/field ionization/field desorption ionization (EI/FI/FD) combination ion source option in addition to the standard EI and optional chemical ionization (CI) sources. The EI/FI/FD ion source eliminates the need to exchange ion sources when switching between ionization modes, which avoids disrupting the instrument’s vacuum and permits higher sample throughput.

Agilent highlighted the 7000A, which the company notes is the first triple-quadrupole instrument designed specifically for use with gas chromatography rather than being modified for GC/MS from an LC/MS system. Introduced at ASMS, the 7000A incorporates Agilent’s flagship 7890A GC to provide high sensitivity and selectivity for compounds down to the femtogram level, even for impure samples.

Thermo Fisher featured the Exactive, a benchtop LC/MS system first introduced at ASMS that incorporates the company’s patented Orbitrap ion control and mass analysis technology. The instrument is designed for everyday compound screening and identification applications in the toxicology, environmental, and drug development arenas. The Orbitrap setup in Exactive provides sub-parts-per-million mass accuracy with resolving power up to 100,000, which is comparable to high-resolution Fourier transform ion-cyclotron resonance spectroscopy, the company says. These parameters permit users to deconvolute overlapping ion peaks in a single experiment by reanalyzing data at a higher resolution.

Applied Biosystems and MDS Analytical Technologies displayed the AB SCIEX Triple Quad 5500 and QTRAP 5500 triple-quadrupole MS systems. The companies promote these instruments, introduced last fall, as providing complete workflow solutions to challenging analyses in drug discovery, protein biomarker analysis, food-testing applications, and environmental studies. Both instruments incorporate new electronics and ion optics into layouts that take up about half as much space as their predecessors. The QTRAP 5500 includes novel ion-trap technology called the Linear Accelerator Trap, which allows users to conduct qualitative and quantitative analysis to identify and confirm results in a single experiment. The QTRAP 5500 also features proprietary TripleTrap Scanning that permits scientists to switch between triple-quadrupole mode and the more sensitive ion-trap mode in less than a millisecond to do multiple experiments on the same instrument.

PITTCON POTPOURRI

Hamilton showcased the BioLevitator, the first benchtop 3-D cell-culture system on the market. The machine was created to facilitate culturing and storing primary and stem cells for drug discovery and biomedical research. BioLevitator couples Hamilton’s automated fluid-handling expertise and Global Cell Solutions’ Global Eukaryotic Microcarrier technology into a unit that effectively replaces traditional planar cell-culture systems that require incubators and centrifuges. In the BioLevitator, cells anchor to silica-coated iron particles for high-density growth, which is facilitated by suspending the particles in solution with the aid of magnets. The system’s four 50-mL culture tubes permit four cell lines to be grown at once or larger scale production of a single cell line, with an option for automated preparation of well plates for downstream assays. It features real-time monitoring and control of temperature, CO2 levels, and other parameters via a touch-screen interface.

Lumencor introduced the Aura line of “light engines” that are designed to replace traditional light sources in optical instrumentation, in particular for bioanalytical applications. These devices employ an excitation light source and a luminescent light pipe that directs the light into an optical cable for delivery to the instrument optical system. The type of excitation source and chemical dopant used in the light pipe depend on the desired wavelength and intensity of light. According to Lumencor, Aura light engines have an advantage over traditional light sources such as arc lamps, lasers, and LEDs, which have issues that include limited wavelengths, instability, generating unwanted heat and vibration, insufficient intensity, high cost, and limited lifetime. Lumencor’s low-power, palm-sized devices produce stable monochromatic light with little heat and at low lifetime cost relative to other light sources. Different wavelength configurations are available covering the UV to near-IR spectral region to match the wavelengths of common fluorescent dyes, making Aura light sources amenable to DNA sequencing, quantitative PCR, lab-on-a-chip technologies, and fluorescence microscopy.

PerkinElmer presented a series of differential scanning calorimeters designed to improve accuracy and sensitivity of phase-transition and sample-degradation measurements during materials research and development. The offering makes PerkinElmer the only supplier to offer both single- and double-furnace technologies. The DSC 4000 is a single-furnace unit for routine applications in academic, polymer, and pharmaceutical areas; the DSC 6000 picks up where the DSC 4000 leaves off with the addition of a modulated temperature feature and other accessories enabling users to separate kinetic events from thermal events. At the top end are the DSC 8000 and DSC 8500 (shown), which sport a proprietary double-furnace design and superfast scanning rates. These two instruments are capable of rapidly heating and cooling materials—the DSC 8500 can heat samples 750 °C per minute and cool samples 2,100 °C per minute—to reduce analysis times for applications such as replicating polymer molding processes or high-throughput testing of pharmaceutical formulations.

Concoa debuted a fully automated gas distribution and management system, the IntelliSwitch II, which provides seamless gas supply for analytical labs, industrial biotech facilities, and chemical plants. IntelliSwitch II is the first of a new generation of gas-supply control systems that feature an onboard Web server and embedded software. The system hardware, which includes patented pressure switches (not transducers), and software were developed for continuously checking gas cylinders, cryogenic liquid storage containers, and other supply sources and automatically switching back and forth between the primary source and a backup as needed to maintain consistent gas flow and pressure. The system notifies managers and gas suppliers by e-mail if action is needed. The company projects that IntelliSwitch II will reduce costs by preventing waste, especially from venting idle cryogenic tanks or from replacing cylinders before they are completely empty. Although suitable for any continuous gas-supply needs, Concoa is promoting IntelliSwitch II for the biotech arena, in particular for maintaining optimum CO2 levels for large-scale cell-culture growth and storage operations.

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CHROMATOGRAPHY & SEPARATIONS

(4) Agilent unveiled the 1200 series HPLC-Chip II, the second-generation of the company’s fluidic chip technology that combines nanoflow liquid chromatography with electrospray ionization for mass spectrometry. The credit-card-sized polyimide-based HPLC-Chip, which slides into the instrument, is offered as an alternative to gel electrophoresis and is compatible with the company’s entire line of mass spectrometers. Agilent currently offers 12 versions of the HPLC-Chip for applications that include peptide quantitation, biomarker discovery, and monoclonal antibody characterization. The first versions incorporating the new HPLC-Chip II design are a phosphopeptide chip for post-translational modifications, a large-capacity protein ID chip, and the ultra-high-capacity chip. The new chip technology doubles the lifetime of the original HPLC-Chip to beyond 1,000 sample injections and improves chip-to-chip and run-to-run reproducibility.

Malvern Instruments introduced a photodiode array detector with the Viscotek TDAmax gel-permeation chromatography/size-exclusion chromatography system, the first time a multiwavelength UV-Vis detector has been used for GPC/SEC, according to the companies. UV-Vis detection in conjunction with viscosity and light-scattering detection is routine for characterizing polymers and biomolecules such as proteins as they elute from GPC/SEC columns. But until now absorbance measurements have been made at a single wavelength. With simultaneous data from across the 190-500-nm wavelength range, TDAmax (TDA can stand for triple or tetra detector array) captures a “time slice” of sample as it elutes from the column, providing a 3-D graphical fingerprint of absorbance versus wavelength. The resulting data give a high level of detail about molecular weight distribution, viscosity, polymer chain branching and cross-linking, and biomolecule conjugation in a single run rather than making multiple runs at different wavelengths. The new setup is ideal for analyzing polymer blends and complex copolymers, as well as for identifying protein conjugates and complexes.

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(5) Grace Davison Discovery Sciences launched the Reveleris flash chromatography system aimed at streamlining sample purification during the design and synthesis of lead compounds in the drug discovery process. Reveleris uses two UV detectors and an evaporative light-scattering detector to optimize peak detection and trigger the collection of sample fractions in less time. The multiple detector design overcomes limitations of single UV detector flash chromatography systems in detecting impurities and/or nonchromophoric compounds. The separation cartridges (rated at up to 200-psig pressure) and fraction trays used with the system have radio-frequency ID tags that contain downloadable flow-rate and run-time parameters and permit sample tracking.

Dionex made several new product introductions across its portfolio of chromatography products. Dionex’ Viper is a stainless steel, finger-tight fitting for capillary chromatography columns. It is the first commercially available universal fitting system that doesn’t rely on ferrules or ferrule-shaped parts, according to the company. Viper can withstand pressures to 100 MPa for HPLC and UPLC systems and is compatible with any common HPLC column hardware or injection/switching valve platform. Dionex also unveiled three updated Reagent-Free Ion Chromatography (RFIC) systems that include automated sample preparation, expanding its lineup of eluent generation and eluent regeneration ion chromatographs that allow users to prepare high-purity buffered solutions on-line or to recycle spent eluent for weeks without servicing. In addition, Dionex featured new pumps for its UltiMate 3000 LC system, which now allows users to work over a broad pressure range at rates up to 5 mL per minute to cover the full gamut of conventional LC to UPLC on one system.

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PerkinElmer debuted the Swafer, a new microchannel wafer switching technology for controlling multiple capillary columns and detectors in gas chromatography. Two versions of the device, which is about the size of a nickel, were designed to provide users of PerkinElmer’s Clarus 500 and 600 GCs with greater flexibility in analytical separations. The D-Swafer is based on the classical Dean’s switch principle and can be used for “heart cutting” selected peaks for analysis within a complicated sample mixture. It also can be configured to switch detectors, vent solvent, backflush samples, and swap carrier gases. The S-Swafer is a scalable splitting device with a programmable pressure regulator that can divert a sample to multiple columns for different separations or connect up to four detectors to one column, among other operations.

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MOLECULAR SPECTROSCOPY

(7) Bruker BioSpin premiered the Avance Solid-State DNP-NMR spectrometer, the first commercially available solid-state NMR system that takes advantage of the heightened sensitivity provided by dynamic nuclear polarization of a sample. The improvement is provided by irradiating the sample with 263-GHz microwaves, which induces the transfer of the much larger polarization of electron spins to the nuclear spins in the sample molecules, resulting in a 50- to 150-fold NMR signal enhancement. The system is made up of Bruker’s Avance III spectrometer configured for solid-state NMR combined with Bruker’s high-powered gyrotron microwave generator and low-temperature DNP-NMR probe. The technique permits researchers to study solid samples that have weak NMR signals, including compounds that normally are inaccessible to NMR, such as some membrane proteins and nanomaterials that are available in small quantities.

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(8) Thermo Fisher unveiled the NanoDrop 2000c UV-Vis spectrophotometer, which is the first instrument to offer the dual capability of using a standard cuvette for sample analysis or placing undiluted liquid sample (as little as 0.5 µL) directly onto an optical pedestal. When the lid shuts on NanoDrop’s patented pedestal, it takes advantage of the surface tension of the liquid to draw the sample into a tiny column that functions like a virtual cuvette for spectral analysis. NanoDrop has a footprint about the size of a lab notebook, covers a spectral range of 190–840 nm, and boasts the broadest sample concentration range for a spectrophotometer of 0.4 to 15,000 ng per µL. The instrument can be used for any UV-Vis application, including kinetics studies, but it’s geared toward analyzing nucleic acids, proteins, and peptides.

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(9) MicrOptix Technologies announced the launch of a near-IR version of its versatile iLab visible spectrophotometer, which was introduced at Pittcon 2008 as the first handheld device for analyzing and monitoring liquids and colored surfaces and materials in the visible wavelength range. The near-IR S860 model (left) covers 650–1,050 nm to complement the visible S560 model (right) that covers 400–700 nm. The iLab instruments, which use several sample interface adapters, weigh just 7.4 oz and run on three AA batteries that power LED light sources, a proprietary spectral imaging chip, and an onboard computer. The devices can store up to 500 spectra at a time, which permits users to compare spectral measurements, and use a USB port to download methods and transfer data. The scientists developing the iLab system envision the spectrophotometers as ideal tools for the lab, plant floor, field, or classroom. To promote education, they are developing student lab experiments built around the iLab system, with the methods downloadable to the spectrophotometers.

 
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