The petroleum ether extract of dried ground seeds of Piper nigrum Linn. and some column fractions of this extract were subjected to GC and GC-MS analysis, resulting in the identification of fourteen compounds (1-14) by using NIST Mass spectral search program 1998 and the Kovat's retention indices. Ten of the compounds (1, 2, 4-12) are reported for the first time from this plant. All the fractions showed insecticidal activity against the fourth instar larvae of Aedes aegypti and against the fourth instar larvae of Anopheles stephensi Liston, determined by the WHO method.