From extraterrestrial organics to pharmaceuticals and drugs of abuse, DART is helping researchers and scientist rapidly find answers.  Come to the annual DART Forum at ASMS in Baltimore on June 15 to hear the latest from leaders in the field.

Hye Jin Kim, Yong Taek Seo, Sang-il Park, Se Hee Jeong, Min Kyoung Kim, Young Pyo Jang 
María Eugenia Monge, Prabha Dwivedi, Manshui Zhou, Michael Payne, Chris Harris, Blaine House, Yvonne Juggins, Peter Cizmarik, Paul N. Newton, Facundo M. FernándeZ, David Jenkins

School of Chemistry and Biochemistry, Georgia Institute of Technology, Atlanta, Georgia USA; Product Quality and Compliance, FHI 360, Durham, North Carolina USA; Lao-Oxford-Mahosot Hospital-Wellcome Trust Research Unit, Microbiology Laboratory, Mahosot Hospital, Vientiane, Lao PDR; Centre for Tropical Medicine, Churchill Hospital, University of Oxford, Oxford, United Kingdom; WorldWide Antimalarial Resistance Network, Churchill Hospital, University of Oxford, Oxford, United Kingdom

Reproductive health has been deleteriously affected by poor quality medicines. Emergency contraceptive pills (ECPs) are an important birth control method that women can use after unprotected coitus for reducing the risk of pregnancy. In response to the detection of poor quality ECPs commercially available in the Peruvian market we developed a tiered multi-platform analytical strategy. In a survey to assess ECP medicine quality in Peru, 7 out of 25 different batches showed inadequate release of levonorgestrel by dissolution testing or improper amounts of active ingredient. One batch was found to contain a wrong active ingredient, with no detectable levonorgestrel. By combining ultrahigh performance liquid chromatography-ion mobility spectrometry-mass spectrometry (UHPLC-IMS-MS) and direct analysis in real time MS (DART-MS) the unknown compound was identified as the antibiotic sulfamethoxazole. Quantitation by UHPLC-triple quadrupole tandem MS (QqQ-MS/MS) indicated that the wrong ingredient was present in the ECP sample at levels which could have significant physiological effects. Further chemical characterization of the poor quality ECP samples included the identification of the excipients by 2D Diffusion-Ordered Nuclear Magnetic Resonance Spectroscopy (DOSY ¹H NMR) indicating the presence of lactose and magnesium stearate.


Xin Wang , Xianjiang Li , Ze Li , Yiding Zhang , Yu Bai , and Huwei Liu

Beijing National Laboratory for Molecular Sciences, 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 100871, People's Republic of China

Online coupling of in-tube solid phase microextraction (IT-SPME) with direct analysis in real time mass spectrometry (DART-MS) was realized for the first time and applied in the analysis of triazine herbicides in lake water and orange juice. We incorporated single-wall carbon nanotubes (SWNTs) into a polymer monolith containing methacrylic acid (MAA) and ethylene dimethacrylate (EDMA) to form a novel poly(methacrylic acid-co-ethylene dimethacrylate-co-single wall carbon nanotubes) (poly(MAA-EDMA-SWNT)) monolith, which was then used in IT-SPME for enrichment of six triazine herbicides from water samples. With the online combination of IT-SPME with DART-MS, the analytes desorbed from the monolith were directly ionized by DART and transferred into MS for detection, thus rapid determination was achieved. Compared with regular DART-MS method, this online IT-SPME-DART-MS method was more sensitive and reproducible, because of the IT-SPME procedures and the isotope-labeled internal standard used in the experiment. Six triazine herbicides were determined simultaneously using this method with good linearity (R² > 0.998). The limit of quantification (signal-to-noise ratio of S/N = 10) of the six herbicides were only 0.06-0.46 ng/mL. The proposed method has been applied to determine triazine herbicides in lake water and orange juice, showing satisfactory recovery (85%-106%) and reproducibility (relative standard deviation of RSD = 3.1%-10.9%).

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.

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