WHAT'S NEW WITH DART MS?                                         April 2014  
 The Latest Developments in Direct Analysis in Real Time Mass Spectrometry 

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We are refining a new approach for analysis by DART using solid phase micro-extraction (SPME) and direct analysis with DART.  We have a number of kits available and we are providing these at no charge to a limited number of researchers.  See the details below.

There are two upcoming events that you may find of interest.  In cooperation with Agilent Technologies and RTI International, a webinar on DART-MS of drugs-of-abuse is available On -Demand.  Also there are two DART presentations at the upcoming AOCS conference in San Antonio.

As usual, your colleagues have published a number of new and interesting papers.

Please have a read and feel free to contact me if you have any questions or comments.  Thanks.


Brian Musselman, Ph.D.
President and CEO

New SPME-DART Kits Available to First 5 Researchers
We are developing a new sample preparation kit for the detection of impurities and materials in complex matrices such as juices, soils, and urine.  These solid phase microextraction kits contain a number of coated fibers that are immersed in the fluids to concentrate and separate the materials of interest.  Direct DART analysis of the fibers yields rapid results.

If you wish to receive a kit to test out, please send an email to Joe LaPointe at briefly describing the measurements you would like to attempt.  We will provide the kits to the first 5 respondents, with the expectation that you would provide us feedback on how the kit worked for your application.  

On-Demand Webinar: 
Increasing Quality While Maintaining Efficiency in Drug Chemistry with DART-TOF MS Screening

In case you weren't able to attend this March 27 presentation, it is now available on-demand.  Please click below for more info and to register.  Brought to you by Agilent Technologies and RTI International's Center for Forensic Sciences


DART-TOF for Analysis of Bulk Drugs

Presenter: Dr. Eric Shonsey
Alabama Department of Forensic Sciences

On-Demand Webinar Event


CLICK HERE for more information and to register


A Direct Analysis in Real Time (DART) ion source coupled to an Agilent time of flight (TOF) mass spectrometer (MS) provides an instrument capable of screening a multitude of sample types without any sample preparation necessary.  Using the Agilent DART-TOF MS, the analysis time per sample is 4 minutes including a blank resulting in a tremendous amount of reviewable data with minimal analysis time and sample preparation. At ADFS, a scientist averages 40 samples in a 4 hour period including data analysis.

This initial screening procedure has been incorporated into the Drug Chemistry work flow for all incoming cases with the exception of marijuana and pharmaceutical tablets. The DART-TOF MS screen has streamlined the batching process for Drug Chemistry cases, allowing the laboratory to meet demanding quality standards without sacrificing efficiency.

DART-MS at the AOCS Annual Meeting
Here are two DART presentations at the upcoming AOCS Meeting in San Antonio. 

Determination of Supplement Identity and Quality by Using DART-Mass Spectrometry for Rapid Triglyceride Analysis

Wednesday morning, May 7th 
Brian Musselman, Joseph Lapointe, Robert Goguen and Crystal Hart
IonSense, Inc. , Saugus, MA, USA, and Boston University Forensics Program, Boston, MA, USA
Abstract: Nutritional supplements incorporate a wide variety of plant materials. Some supplements are single plant but often different tea leaves and even chemicals are added to produce products with the desired composition. As the quality control of these materials must improve with new regulations the need for relevant chemical test increases the burden on small manufacturers and exporters.  We have completed analysis of a wide variety of medicinal supplements utilizing Direct Ionization in Real Time ambient ionization mass spectrometry. The method provides an easy means to complete chemical analysis with little sample prep. During these investigations we have been able to generate lipid profiles for the triglycerides in just seconds per sample. Statistical analysis of the data can be used to determine the presence / absence of different plant materials. The method affords a rapid means to check for sample composition and even quality as detection of irregular lipid profiles is made possible even when small concentrations of lipids are present as in the case of dried leaves.

Identification of Lipid Oxidation Products Using SPME-DART-QTOF
Wednesday morning, May 7th
Susan Seegers, T. West
Bunge North America, Bradley, IL, USA
Abstract: Typically, a variety of gas chromatography (GC) methods have been used to evaluate oxidation products in edible oils.  There are many different ways to introduce the sample into the GC such as cold-trapping, gas sampling, and more recently, solid-phase microextraction (SPME).  Coupled to a mass spectrometer, these methods can concentrate, separate, and identify oxidation products.  Direct analysis in real time (DART) is an ambient ionization technology used to introduce samples into a mass spectrometer.  When used in conjunction with a quadrupole time of flight (QTOF) mass spectrometer, samples can be quickly analyzed with high mass accuracy.  This methodology was applied to oxidation products in edible oils. Because these oxidation products are in low concentrations, SPME was also employed to concentrate the volatiles and used in conjunction with the DART.  The SPME fiber was then directly desorbed in the DART stream and the oxidation products introduced into the QTOF.
Recent Publications on DART MS

Jacob L. Easter, Robert R. Steiner

Virginia Department of Forensics Science, 700N Fifth St., Richmond, VA 23219


Pharmaceutical analysis comprises a large amount of the casework in forensic controlled substances laboratories. In order to reduce the time of analysis for pharmaceuticals, a Direct Analysis in Real Time ion source coupled with an accurate mass Time-of-Flight (DART-TOF) mass spectrometer was used to confirm identity. DART-TOF spectral data for pharmaceutical samples were analyzed and evaluated by comparison to standard spectra. Identical mass pharmaceuticals were differentiated using collision induced dissociation fragmentation, present/absent ions, and abundance comparison box plots; Principal Component Analysis (PCA) and Linear Discriminant Analysis (LDA) were used for differentiation of identical mass mixed drug spectra. Mass assignment reproducibility and robustness tests were performed on the DART-TOF spectra. Impacts on the forensic science community include a decrease in analysis time over the traditional gas chromatograph/mass spectrometry (GCMS) confirmations, better laboratory efficiency, and simpler sample preparation. Using physical identifiers and the DART-TOF to confirm pharmaceutical identity will eliminate the use of GCMS and effectively reduce analysis time while still complying with accepted analysis protocols. This will prove helpful in laboratories with large backlogs and will simplify the confirmation process.

Radostina K. Manova, Sweccha Joshi, Aline Debrassi, Nagendra S. Bhairamadgi, Esther Roeven, Jacinthe Gagnon, Muhammad N. Tahir, Frank W. Claassen, Luc M.W. Scheres, Tom Wennekes, Karin SchroŽn, Teris A. van Beek, Han Zuilhof, and Michel W. F. Nielen

Laboratory of Organic Chemistry, Wageningen University, Dreijenplein 8, 6703 HB Wageningen, The Netherlands; Food Process Engineering Group, Wageningen University, Bomenweg 2, 6703 HD Wageningen, The Netherlands; Surfix BV, Dreijenplein 8, 6703 HB Wageningen, The Netherlands

A better characterization of nanometer-thick organic layers (monolayers) as used for engineering surface properties, biosensing, nanomedicine, and smart materials will widen their application. The aim of this study was to develop direct analysis in real time high-resolution mass spectrometry (DART-HRMS) into a new and complementary analytical tool for characterizing organic monolayers. To assess the scope and formulate general interpretation rules, DART-HRMS was used to analyze a diverse set of monolayers having different chemistries (amides, esters, amines, acids, alcohols, alkanes, ethers, thioethers, polymers, sugars) on five different substrates (Si, Si3N4, glass, Al2O3, Au). The substrate did not play a major role except in the case of gold, for which breaking of the weak Au-S bond that tethers the monolayer to the surface, was observed. For monolayers with stronger covalent interfacial bonds, fragmentation around terminal groups was found. For ester and amide-terminated monolayers, in situ hydrolysis during DART resulted in the detection of ions characteristic of the terminal groups (alcohol, amine, carboxylic acid). For ether and thioether-terminated layers, scission of C-O or C-S bonds also led to the release of the terminal part of the monolayer in a predictable manner. Only the spectra of alkane monolayers could not be interpreted. DART-HRMS allowed for the analysis of and distinction between monolayers containing biologically relevant mono or disaccharides. Overall, DART-HRMS is a promising surface analysis technique that combines detailed structural information on nanomaterials and ultrathin films with fast analyses under ambient conditions.

Xianjiang Li, Jiawei Xing, Cuilan Chang, Xin Wang, Yu Bai, Xiuping Yan and Huwei Liu

Beijing National Laboratory for Molecular Sciences, the Key Laboratory of Bioorganic Chemistry and Molecular Engineering of Ministry of Education, Institute of Analytical Chemistry, College of Chemistry and Molecular Engineering, Peking University, Beijing, China; State Key Laboratory of Medicinal Chemical Biology, and Research Center for Analytical Sciences, College of Chemistry, Nankai University, Tianjin, China

MIL-101(Cr) is an excellent metal-organic framework with high surface area and nanoscale cavities, making it promising in solid-phase extraction. Herein, we used MIL-101(Cr) as a solid-phase extraction packing material combined with fast detection of direct analysis in real time mass spectrometry (DART-MS) for the analysis of triazine herbicides. After systematic optimization of the operation parameters, including the gas temperature of DART, the moving speed of the 1D platform, solvent for desorption, amount of MIL-101(Cr) and extraction time, this method can realize the simultaneous detection of five kinds of triazine herbicides. The limits of detection were 0.1∼0.2 ng/mL and the linear ranges covered more than two orders of magnitude with the quantitation limits of 0.5∼1 ng/mL. Moreover, the developed method has been applied for the analysis of lake water samples and the recoveries for spiked analytes were in the range of 85∼110%. These results showed that solid-phase extraction with metal-organic frameworks is an efficient sample preparation approach for DART-MS analysis and could find more applications in environmental analysis.

About IonSense
IonSense, Inc. provides OpenSpot Mass Spectrometry™ solutions to the fields of food safety, forensics, drug development, and chemical analysis. We manufacture and develop direct analysis in real time (DARTģ) technology licensed from JEOL USA, Inc. and atmospheric solids analysis probe (ASAP™) licensed from M&M Consulting.

DART and ASAP Sources are available for most commercial LC/MS systems.  Look here to see if your system is DART-ready.  And  check here to see if your system is ASAP-ready.

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