Forensic Analysis of Stains on Fabric Using Direct Analysis in Real-time Ionization with High-Resolution Accurate Mass-Mass Spectrometry.

A rapid technique using direct analysis in real-time (DART) ambient ionization coupled to a high-resolution accurate mass-mass spectrometer (HRAM-MS) was employed to analyze stains on an individual's pants suspected to have been involved in a violent crime. The victim was consuming chocolate ice cream at the time of the attack, and investigators recovered the suspect's pants exhibiting splatter stains. Liquid chromatography with mass spectral detection (LC-MS) and stereoscopic light microscopy (SLM) were also utilized in this analysis. It was determined that the stains on the pants contained theobromine and caffeine, known components of chocolate. A shard from the ceramic bowl that contained the victim's ice cream and a control chocolate ice cream sample were also found to contain caffeine and theobromine. The use of DART-HRAM-MS was useful in this case due to its rapid analysis capability and because of the limited amount of sample present as a stain.

Analysis of Hypodermic Needles and Syringes for the Presence of Blood and Polydimethylsiloxane (Silicone) Utilizing Microchemical Tests and Infrared Spectroscopy.

Suspect hypodermic needles and syringes were seized from an unlicensed individual who was allegedly injecting patients with silicone (polydimethylsiloxane [PDMS]) for cosmetic enhancement. Since control syringe barrels and needles often contain an interfering PDMS lubricant, a risk for false positives of foreign PDMS exists. The focus of this report was to minimize this risk and determine a quick and reliable test for the presence of blood in PDMS matrices. Using ATR-FT-IR spectroscopy, the risk for false-positive identification of foreign PDMS was reduced by (i) overfilling the sampling aperture to prevent spectral distortions and (ii) sampling a region of the suspect syringe/needle assembly where manufacturer-applied PDMS is not typically located. Analysis for blood indicated that the Teichman microchemical test was effective for detecting blood in the presence of PDMS. Overall, detecting PDMS established intent and detecting blood established that the needle containing the PDMS had been used for injection.

A multidisciplinary approach for the analysis of an adulterated dietary supplement where the active pharmaceutical ingredient was embedded in the capsule shell.

Fourier transform infrared (FT-IR) microspectroscopic imaging, Raman microspectroscopy, optical microscopy and high performance liquid chromatography with mass spectrometric (LC/MS) detection were employed to examine a dietary supplement adulterated with an undeclared active pharmaceutical ingredient (API). While a trace level of the API was detected in the capsule contents, a higher concentration of API was found in the capsule shell, which indicated the use of an unconventional manufacturing process to hide the API and thus avoid detection. This study demonstrates the need for a multidisciplinary approach to provide a complete assessment of a suspect adulterated dietary supplement.

Evaluation of the renal effects of experimental feeding of melamine and cyanuric acid to fish and pigs.

OBJECTIVE: To determine whether renal crystals can be experimentally induced in animals fed melamine or the related triazine compound cyanuric acid, separately or in combination, and to compare experimentally induced crystals with those from a cat with triazine-related renal failure. ANIMALS: 75 fish (21 tilapia, 24 rainbow trout, 15 channel catfish, and 15 Atlantic salmon), 4 pigs, and 1 cat that was euthanatized because of renal failure. PROCEDURES: Fish and pigs were fed a target dosage of melamine (400 mg/kg), cyanuric acid (400 mg/kg), or melamine and cyanuric acid (400 mg of each compound/kg) daily for 3 days and were euthanatized 1, 3, 6, 10, or 14 days after administration ceased. Fresh, frozen, and formalin-fixed kidneys were examined for crystals. Edible tissues were collected for residue analysis. Crystals were examined for composition via Raman spectroscopy and hydrophilic-interaction liquid chromatography-tandem mass spectrometry. RESULTS: All animals fed the combination of melamine and cyanuric acid developed goldbrown renal crystals arranged in radial spheres (spherulites), similar to those detected in the cat. Spectral analyses of crystals from the cat, pigs, and fish were consistent with melamine-cyanurate complex crystals. Melamine and cyanuric acid residues were identified in edible tissues of fish. CONCLUSIONS AND CLINICAL RELEVANCE: Although melamine and cyanuric acid appeared to have low toxicity when administered separately, they induced extensive renal crystal formation when administered together. The subsequent renal failure may be similar to acute uric acid nephropathy in humans, in which crystal spherulites obstruct renal tubules.

Outbreak of food-borne illness associated with plant material containing raphides.

BACKGROUND: Many botanicals, particularly ornamental house-plants, contain crystals of calcium oxalate called raphides. Raphides have known toxic effects when chewed, including painful edema, vesicle formation, and dysphagia. We report a food-borne illness outbreak associated with ingestion of raphides. METHODS: On February 24, 2003, the Chicago Department of Public Health was notified of multiple cases of oral burning and facial edema associated with lunch in an office cafeteria on February 21. The investigation included a case-control study, interviews with kitchen staff, an environmental inspection, and laboratory analysis of leftover foods. RESULTS: Ten cases were identified, including one admitted to the Intensive Care Unit for potential airway obstruction secondary to severe edema, and another seen by Emergency Department staff for oral edema and pain. Ten of 10 case-patients reported oral stinging and burning, and 8 of 10 reported dysphagia. Four of 10 case-patients continued to have symptoms 2 weeks later. Food from the cafeteria's international buffet was consumed by 10 of 10 case-patients and by 1 of 22 control subjects (odds ratio=undefined); each of the 10 case-patients reported consumption of a Chinese vegetable entrée from the international buffet and had no other foods in common. Plant material from the Chinese vegetable entrée contained raphides. CONCLUSION: This outbreak was associated with consumption of raphides resembling those from common botanicals. Clinicians and public health practitioners should be aware of raphide-containing plants as a potential cause of food-borne illness.

A method for the determination of syringe needle punctures in rubber stoppers using stereoscopic light microscopy.

The ability to accurately determine the number of syringe needle penetration holes through the rubber stoppers in pharmaceutical vials and rubber septa in intravenous (i.v.) line and bag ports has been a critical factor in a number of forensic cases involving the thefts of controlled substances or suspected homicide by lethal injection. In the early 1990s, the microscopy and microanalysis group of the U.S. Food and Drug Administration's Forensic Chemistry Center (FCC) developed and implemented a method (unpublished) to locate needle punctures in rubber pharmaceutical vial stoppers. In 1996, as part of a multiple homicide investigation, the Indiana State Police Laboratory (ISPL) contacted the FCC for information on a method to identify and count syringe needle punctures through rubber stoppers in pharmaceutical vials. In a joint project and investigation using the FCC's needle hole location method and applying a method of puncture site mapping developed by the ISPL, a systematic method was developed to locate, identify, count, and map syringe punctures in rubber bottle stoppers or i.v. bag ports using microscopic analysis. The method requires documentation of punctures on both sides of the rubber stoppers and microscopic analysis of each suspect puncture site. The final result of an analysis using the method is a detailed diagram of puncture holes on both sides of a questioned stopper and a record of the minimum number of puncture holes through a stopper.