A procedure is described for the rapid extraction and quantification of amphetamine and methamphetamine from meconium using ISOLUTE HM-N-supported liquid extraction columns and gas chromatography-mass spectrometry (GC-MS). Because of the matrix complexity of meconium samples, extraction and sample preparation prior to instrumental analysis can prove difficult and time-consuming. The present study introduces a novel sample preparation technique for the simultaneous quantification of amphetamine and methamphetamine in meconium using GC-MS. Extraction of both analytes was achieved using ISOLUTE HM-N-supported liquid extraction columns containing a modified form of diatomaceous earth. Limits of detection for both analytes were 30 ng/g and the lower limit of quantitation was 75 ng/g. Linearity was achieved over the range 75-3000 ng/g. The methodology showed excellent intrarun precision with %CV values ranging from 2 to 8% for both analytes. Interrun precision experiments produced %CV values between 7 and 10% for both analytes. The reported methodology proved suitable for the accurate quantification of amphetamine and methamphetamine in meconium samples and greatly reduced the sample preparation time normally required for traditional solid-phase extraction. The development and validation of such analytical methodologies will prove beneficial for the identification of prenatal substance abuse, which is an ongoing concern across socioeconomic lines.