A 37-year-old woman committed murdered by oral ingestion of hair dye or overdose of some medications were available. A hair dye and many over-the-counter drugs misused in suicide/homicide purpose are uncommon in Libyan society; Women deceased specimens suspected to contain PPD and/or other medication were collected, LCESI- MS analysis were carried out to identify the individual substances present in post-mortem specimens. The present work describes an analytical method for determination of lower traces of para-phenylenediamine (PPD) as a major life threatening compound in hair dye as well as paracetamol in post-mortem biological fluids, this procedure involves the protein crash extraction for urine, blood and stomach contents. As well as colour tests as a routine testing were conducted on urine sample, for paracetamol, and it was detected in urine specimen by the Cresol-ammonia colour test.