JEOL Resources

Rapid Identification of Smokeless Powders

Wed, 04 Mar 2020 15:40:37 GMT

Experimental

The AccuTOF™ mass spectrometer was operated in positive-ion mode. Polyethylene glycol (PEG-600) was measured as a reference standard within each data file, but separate from the smokeless powder particle measurements. Individual particles sampled with vacuum tweezers were positioned in the DART gas stream for analysis (Figure 2). Disposable vacuum tweezers were constructed by passing a glass capillary through an Eppendorf pipette tip and inserting the pipette tip into a rubber hose connected to a low-vacuum pump. Data were acquired by using JEOL Mass Center software and mass spectra were processed by TSSPro3 software (Shrader Software Solutions, Detroit, MI).

The DART ion source was operated with a gas heater temperature setting of ≤200°C to avoid damaging or detonating the smokeless powder particles. Individual samples could be analyzed within seconds. As long as the gas heater temperature did not exceed 200°C, the samples were not consumed and could be examined or reanalyzed at a later time.

“Laundry Detective”: Identification of a Stain

Wed, 04 Mar 2020 14:40:48 GMT

The AccuTOF-DART™ was recently applied to an unusual analytical problem: finding the cause of oily stains on freshly laundered shirts (Figure 1). No cutting or extraction was required. Stained and unstained regions of the shirt were placed in the DART gas stream and the mass spectra were acquired. The DART parameters were: helium gas, flow 3-4 LPM, gas heater set to 175 degrees C, positive-ion mode, PEG 600 exact mass reference standard. These conditions did not damage the shirt.

Instantaneous Screening for Counterfeit Drugs with No Sample Preparation

Wed, 04 Mar 2020 14:37:59 GMT

Drug counterfeiting is becoming a serious and widespread public health problem. The number of FDA open investigations into drug counterfeiting rose sharply from 2000 to 2001 and has remained high in recent years. Counterfeit drugs are not only illegal, but dangerous; they may contain little or no actual drug content, or they may contain completely different drugs with potentially toxic consequences. The problem is worldwide; it has been reported that nearly 50% of all anti-malarial drugs in Africa are thought to be counterfeit. Direct Analysis in Real Time (DART™) offers a simple solution to screening for counterfeit drugs. DART can detect the presence or absence of drugs in medicines within seconds by simply placing the pill or medicine in front of the mass spectrometer. In combination with the AccuTOF, DART provides exact masses and accurate isotopic patterns that provide elemental compositions for known and unknown substances.

Instantaneous Detection of the “Date-Rape” Drug -- GHB

Wed, 04 Mar 2020 14:34:51 GMT

Gamma hydroxybutyrate (GHB) is a fast-acting central nervous system depressant. Prior to its ban by the FDA in 1990, GHB was sold in bodybuilding formulas. It has been abused as a euphoriant. Because it is colorless and odorless, it can be added to alcoholic drinks of unsuspecting victims. An overdose can result in serious consequences, including respiratory depression and coma. GHB was classified as a Schedule I Controlled Substance in March, 2000. Detection of GHB is problematic. GC/MS and LC/ MS methods are time consuming. A rapid colorimetric assay for GHB has been developed, but this assay suffers from some limitations. For example, ethanol produces the same colorimetric response as GHB. The AccuTOF™ mass spectrometer equipped with Direct Analysis in Real Time (DART™) can rapidly detect GHB anion (C4H7O3 -, m/z 103.0395) on surfaces, in urine, and in ethanol. No solvent extraction, wipes, or chromatography are required. Examples are shown in the figures below.

Instantaneous Detection of Opiates in Single Poppy Seeds

Wed, 04 Mar 2020 14:31:00 GMT

Poppy seed is a common flavoring ingredient that is known to contain small amounts of opiates. Maximum morphine and codeine concentrations are estimated to be about 33 and 14 micrograms respectively per gram of seed. Consumption of typical amounts of baked goods containing poppy seeds has not been shown to cause any ill effects. However, ingestion of poppy seeds may result in false positives from drug tests. Single poppy seeds from different sources were analyzed independently in two different laboratories by using the DART™/AccuTOF™ combination. The resulting mass spectra were nearly identical.

Instantaneous Detection of Illicit Drugs on Currency

Wed, 04 Mar 2020 14:28:14 GMT

The widespread presence of illicit drugs on currency is an indication of the extent of the worldwide substance abuse problem. Remarkably, cocaine can be found on virtually all one-dollar bills in the United States — the upper limit for the general background level of cocaine is estimated to be 13 ng per bill. The Direct Analysis in Real Time (DART™) ion source, combined with the AccuTOF™ mass spectrometer can be used to sample drugs on currency within seconds. No sample preparation (extraction, wipes, etc.) or chromatography is required. The bill is placed in front of the DART and the presence of drugs can be detected immediately. Only a small portion of the bill is sampled at any given time. This allows the analyst to view the distribution of drugs on the surface of a bill, and allows the bill to be retained for reexamination at a later time.

Instantaneous Detection of Explosives on Clothing

Wed, 04 Mar 2020 14:24:54 GMT

The detection of explosives is of vital importance in forensic applications and in preventing criminal or terrorist activity. The analytical detection of explosives on surfaces is normally done by using solvent extractions or wipes and chromatography or chromatography combined with mass spectrometry. This is inefficient because solvent extractions and wipes only result in a partial transfer of material from the surface into the sampling material. Furthermore, the chromatographic analysis can be time-consuming and requires the use of disposable solvents (an environmental concern). The JEOL AccuTOF™ with Direct Analysis in Real Time (DART™) has demonstrated the capability to detect both volatile and involatile explosives on surfaces such as plastic, cloth, concrete, glass, cardboard, metal, and more. No wipes or solvent extractions are required. The method is instantaneous, environmentally friendly, and does not require solvents. An example is shown in this application note.

Fiber analysis by thermal desorption/pyrolysis DART®

Wed, 04 Mar 2020 10:42:12 GMT

Analyzing fiber samples has always been difficult by DART®. The problem has been that there is no easy way to hold the fiber in the gas stream without losing it into the vacuum system. A fiber can be secured in the DART gas stream with forceps or other means, but if the DART gas is too hot, the fiber can break off and be lost into the mass spectrometer vacuum system through the atmospheric pressure interface. A thermal desorption/pyrolysis stage (The Biochromato, Inc. “ionRocket™”) designed for use with DART produces highly reproducible thermal desorption profiles that show outgassing, additives, and high-quality pyrolysis DART mass spectra for materials. Because fiber samples placed in the disposable copper sample “pots” are not positioned directly in the DART gas stream, a single fiber can be analyzed without risk of loss into the vacuum system.

Direct Analysis of Adhesives

Wed, 04 Mar 2020 10:08:57 GMT

All samples were analyzed by acquiring positive-ion mass spectra with the DART source operated with helium and a gas heater setting of 450° C (helium temperature ~350° C). All mass spectra were measured over the m/z range 60-1000 at a resolving power of 6000. Following each analysis, a glass rod coated with PEG 600 was placed in front of the DART source to provide a calibration for exact mass measurements. A nominal mass library of adhesive mass spectra was created by using the software link to the NIST version 2.0 mass spectra database search program. All figures shown here are copied from that library and only integer masses are shown although exact masses were recorded for all peaks.

Detection of the Peroxide Explosives TATP and HMTD

Sun, 23 Feb 2020 15:53:24 GMT

Experimental

Measurements were made with the AccuTOF-DART mass spectrometer operated in positive-ion mode under standard conditions. Little or no heat was required to observe these compounds. Dilute solutions of standard samples of TATP and HMTD were analyzed by dipping melting point tubes into the liquid and dangling the melting point tubes in the DART ion source. Dilute aqueous ammonium hydroxide on a cotton swab was held in the DART gas stream to enhance detection of TATP as the ammoniated molecule.