strychnine and acetonitrile

Strychnine is an alkaloid with strong toxic properties. Poisoning results in muscular contractions and death through asphyxiation. Intentional or accidental poisonings with strychnine occur mainly in small animals, especially dogs and occasionally cats. Strychnine can be detected in the liver or stomach contents. Unfortunately, the determination of strychnine in these matrices, especially in postmortem examination, is subject to a significant matrix effect that makes it difficult to confirm the presence of the substance being determined. Therefore, we developed a new liquid chromatography method combined with mass spectrometry. One-gram homogenized samples were extracted and partitioned after adding acetonitrile and 5-mol solution of ammonium acetate. After extraction, the samples were analyzed using high-pressure liquid chromatography-MS/MS/MS. The results of validation fulfil the requirement of the confirmatory criteria according to SANTE/11945/2015 regarding apparent recoveries (98.97% to 104.0%), repeatability (2.9%-4.1%), and within-laboratory reproducibility (3.3%-4.6%). The method can be successfully applied to confirm strychnine poisoning cases.

Topics: Acetates; Acetonitriles; Animals; Autopsy; Chromatography, Liquid; Dogs; Liver; Reproducibility of Results; Strychnine; Tandem Mass Spectrometry

An easy, rapid method for simultaneous determination of strychnine and brucine in Strychnos nux-vomica L. and its preparation was developed by nonaqueous capillary electrophoresis (NACE) without pretreatment for the first time. Optimum separation was achieved with a fused-silica capillary column (50 cmx75 microm i.d.) and a running buffer containing 30 mM ammonium acetate, 1.0% acetic acid and 15% acetonitrile (ACN) in methanol medium. The applied voltage was 30.0 kV. The analytes were detected by UV at 214 nm. The effects of concentration of ammonium acetate, acetic acid and organic modifier on electrophoretic behavior of the analytes were studied. The established method with sophoridine as internal standard was linear in the range of 5-1000 mg/mL for both strychnine and brucine. The extracts of Strychnos nux-vomica and its preparation could be directly injected for determination with recoveries ranging from 94.5 to 104%.

Topics: Acetates; Acetonitriles; Buffers; Central Nervous System Stimulants; Drugs, Chinese Herbal; Electrophoresis, Capillary; Hydrogen-Ion Concentration; Methanol; Reproducibility of Results; Solvents; Spectrophotometry, Ultraviolet; Strychnine; Strychnos nux-vomica; Time Factors

The enantiomeric resolution of (+/-)-ibuprofen into its enantiomers was achieved by TLC on silica gel plate using optically pure (-)-brucine as a chiral selector and acetonitrile-methanol (5:1, v/v) as the solvent system. Spots were located in an iodine chamber. The detection limit was 4.9 microg. The effect of concentration of the chiral selector, temperature and pH on resolution has been studied.

Topics: Acetonitriles; Anti-Inflammatory Agents, Non-Steroidal; Chromatography, Thin Layer; Hydrogen-Ion Concentration; Ibuprofen; Indicators and Reagents; Methanol; Solvents; Stereoisomerism; Strychnine; Temperature