We have continued our investigation into the multiplex use of various phases of solid phase micro-extraction probes for improved coverage and rapid sampling for DART-MS analysis.   Here we are looking at the analysis of a sport drink spiked with a mixture of drugs that contained benzocaine, lidocaine, and cocaine.

The fibers were each conditioned in a 50:50 MeOH:H2O mixture for 30 minutes before they were shaken in the sample for 1 hour.  We do this in 12-fold mutiplex and are working to extend this, taking advantage of the rapid analysis by DART. The fibers were then analyzed directly with DART using Helium gas at 350˚C on the Thermo EXACTIVE+ instrument.

Due to the speed of DART, it is simple to look at multiple phases and have a greater ability to detect a broader range of compounds.

If you or an associate would like us to analyze a few samples with our Thermo EXACTIVE+ we are looking for problems to challenge this exciting combination of SPME and DART technology.   Please contact Jeff directly for information or a discussion.

Jeff has over 20 years of experience in sales, marketing and business development in the field of analytical instruments.  Before joining IonSense he had roles at Waters, Perseptive BioSystems, Cohesive Technologies, Thermo Fisher Scientific, and ABSciex, working with researchers in a broad range of markets - pharmaceutical, academic, clinical/toxicology and food/environmental.  

Jeff is joining our team as the Director of Market Development.  With the high level of interest in the DART technology, Jeff's focus will be to work with our customers, collaborators, and other interested researchers looking to extend the DART benefits to their laboratories.

A promising process analytical technology (PAT) tool has been introduced for batch processes monitoring. Direct analysis in real time mass spectrometry (DART-MS), a means of rapid fingerprint analysis, was applied to a percolation process with multi-constituent substances for an anti-cancer botanical preparation. Fifteen batches were carried out, including ten normal operations and five abnormal batches with artificial variations. The obtained multivariate data were analyzed by a multi-way partial least squares (MPLS) model. Control trajectories were derived from eight normal batches, and the qualification was tested by R² and Q². Accuracy and diagnosis capability of the batch model were then validated by the remaining batches. Assisted with high performance liquid chromatography (HPLC) determination, process faults were explained by corresponding variable contributions. Furthermore, a batch level model was developed to compare and assess the model performance. The present study has demonstrated that DART-MS is very promising in process monitoring in botanical manufacturing. Compared with general PAT tools, DART-MS offers a particular account on effective compositions and can be potentially used to improve batch quality and process consistency of samples in complex matrices


Ashton D. Lesiak, Rabi A. Musah, Marek A. Domin, Jason R. E. Shepard
Department of Chemistry, University at Albany, SUNY, Albany, NY, Mass Spectrometry Center, Merkert Chemistry Center, Boston College, Chestnut Hill, MA

Direct analysis in real time mass spectrometry (DART-MS) served as a method for rapid high-throughput screening of six commercially available "Spice" products, detecting various combinations of five synthetic cannabinoids. Direct analysis in real time is an ambient ionization process that, along with high mass accuracy time-of-flight (TOF)-MS to 0.0001 Da, was employed to establish the presence of cannabinoids. Mass spectra were acquired by simply suspending a small portion of sample between the ion source and the mass spectrometer inlet. The ability to test minute amounts of sample is a major advantage when very limited amounts of evidentiary material are available. In addition, reports are widespread regarding the testing backlogs that now exist because of the large influx of designer drugs. This method circumvents time-consuming sample extraction, derivatization, chromatographic, and other sample preparative steps required for analysis by more conventional mass spectrometric methods. Accordingly, the synthetic cannabinoids AM-2201, JWH-122, JWH-203, JWH-210, and RCS-4 were identified in commercially available herbal Spice products, singly and in tandem, at concentrations within the range of 4-141 mg/g of material. Direct analysis in real time mass spectrometry decreases the time necessary to triage analytical evidence, and therefore, it has the potential to contribute to backlog reduction and more timely criminal prosecution.


Gertrud E. Morlock, Petar Ristivojevic, Elena S. Chernetsova
Institute of Nutritional Science, Justus Liebig University Giessen, Heinrich-Buff-Ring 26-32, 35392 Giessen, and Institute of Food Chemistry, University of Hohenheim, Garbenstrasse 28, 70599 Stuttgart, Germany

Sophisticated statistical tools are required to extract the full analytical power from high-performance thin-layer chromatography (HPTLC). Especially, the combination of HPTLC fingerprints (image) with chemometrics is rarely used so far. Also, the newly developed, instantaneous Direct Analysis in Real Time mass spectrometry (DART-MS) method is perspective for sample characterization and differentiation by multivariate data analysis. This is a first novel study on the differentiation of natural products using a combination of fast fingerprint techniques, like HPTLC and DART-MS, for multivariate data analysis. The results obtained by the chemometric evaluation of HPTLC and DART-MS data provided complementary information. The complexity, expense, and analysis time were significantly reduced due to the use of statistical tools for evaluation of fingerprints. The approach allowed categorizing 91 propolis samples from Germany and other locations based on their phenolic compound profile. A high level of confidence was obtained when combining orthogonal approaches (HPTLC and DART-MS) for ultrafast sample characterization. HPTLC with selective post-chromatographic derivatization provided information on polarity, functional groups and spectral properties of marker compounds, while information on possible elemental formulae of principal components (phenolic markers) was obtained by DART-MS.

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 (DART^®) 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.

Phone - 781.484.1043  | info@ionsense.com | http://www.ionsense.com