An analytical strategy is described for analyzing quaternary ammonium neuromuscular blocking agents in a wide variety of biological specimens in a forensic setting. Neuromuscular blocking agents such as succinylcholine, pancuronium, and tubocurarine, often used as paralytic agents during surgery, are occasionally suspected as paralytic poisoning agents involved in suspected homicide and suicide cases. Because suspicion in such cases can develop slowly, the age, nature, and quality of available specimens varies greatly. The compounds are challenging analytically because of their simultaneous precharged yet lipophilic character. An analytical strategy has been devised for extracting these compounds from complex matrices using a combination of a modified Bligh and Dyer liquid-liquid extraction (used in reverse) followed by reverse-phase ion pairing solid-phase extraction using heptafluorobutyric acid as an ion pairing reagent. Final analysis is by LC-MS/MS using a tandem quadrupole orthogonal acceleration time of flight instrument (Q-TOF) with repetitive product ion scanning at high resolution. Native and spiked specimens are compared for both quantitative and especially qualitative purposes. The method has been applied to a wide variety of fluid and tissue specimen types, including numerous specimens from exhumation autopsies. For most specimens, detection limits are in the 2 to 10 ng/g range. Succinylmonocholine has been demonstrated to be present at low levels in normal posthumous kidney and liver. The Q-TOF is an excellent platform for forensic analytical investigations. This analytical strategy should also be applicable to other problematic analytes and sample matrices. (J Am Soc Mass
In a fatal (cardiotoxic) case of oleander extract poisoning of a young female, ethanol extracts of blood and tissue homogenates were purified by lead acetate. After removal of excess lead by ammonium sulfate, oleandrin was extracted into chloroform. Oleandrin in the extract concentrates was detected by thin-layer chromatography, with location by fluorescence and chromogenically by means of p-anisaldehyde. Quantitation was performed on dried extracts reconstituted in water/methanol, reacted with hydrogen peroxide, ascorbic acid, and hydrochloric acid, and analyzed by fluorescence spectrophotometry. Excitation was at 355 nm, and fluorescence scanning from 340 to 580 nm. The fluorescence peak at 460 nm was used for the quantitative measurement. The concentrations of oleandrin measured in blood, stomach wall, colon tissue, liver, heart, lung, brain, spleen, and kidney ranged from 10 to 39 micrograms/g, with 200 micrograms/mL in the total gastric content residue submitted for analysis.
Several fatalities due to fluoxetine combined with other drugs such as ethyl alcohol have been reported. We now report an apparent suicide in which fluoxetine was the only causative agent. Because this drug is widely described as having a wide safety margin, it is important to note concentrations in blood associated with overdose fatalities. The findings by GC/NPD and GC/MS in blood were as follows: fluoxetine 6,000 ng and demethylated metabolite 5,000 ng/mL. Parent compound and metabolite were 13,000 ng/mL each in bile. Details of the analytical method and data from 2,100 National Medical Services cases are also presented.
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