Development and practical application of accelerated solvent extraction for the isolation of cocaine/crack biomarkers in meconium samples

作者：Mantovani Cinthia de Carvalho^*; Lima Marcela Bittar; Rodrigues de Oliveira Carolina Dizioli; Menck Rafael de Almeida; de Albuquerque Diniz Edna Maria; Yonamine Mauricio

来源：Journal of Chromatography B-Analytical Technologies in the Biomedical and Life Sciences, 2014, 957: 14-23.

DOI：10.1016/j.jchromb.2014.02.039

• Accelerated solvent extraction
• Fetal exposure
• Cocaine
• Crack
• Meconium
• Gas chromatography-mass spectrometry

A method using accelerated solvent extraction (ASE) for the isolation of cocaine/crack biomarkers in meconium samples, followed by solid phase extraction (SPE) and the simultaneous quantification by gas chromatography-mass spectrometry (GC-MS) was developed and validated. Initially, meconium samples were submitted to an ASE procedure, which was followed by SPE with Bond Elut Certify I cartridges. The analytes were derivatizated with PFP/PFPA and analyzed by GC-MS. The limits of detection CLOD) were between 11 and 17 ng/g for all analytes. The limits of quantification (LOQ) were 30 ng/g for anhydroecgonine methyl ester, and 20 ng/g for cocaine, benzoylecgonine, ecgonine methyl ester and cocaethylene. Linearity ranged from the LOQ to 1500 ng/g for all analytes, with a coefficients of determination greater than 0.991, except for m-hydroxybenzoylecgonine, which was only qualitatively detected. Precision and accuracy were evaluated at three concentration levels. For all analytes, inter-assay precision ranged from 3.2 to 18.1%. and intra-assay precision did not exceed 12.7%. The accuracy results were between 84.5 and 114.2% and the average recovery ranged from 17 to 84%. The method was applied to 342 meconium samples randomly collected in the University Hospital University of Sao Paulo (HU-USP), Brazil. Cocaine biomarkers were detected in 19 samples, which represent 5.6% of exposure prevalence. Significantly lower birth weight, length and head circumference were found for the exposed newborns compared with the non-exposed group. This is the first report in which ASE was used as a sample preparation technique to extract cocaine biomarkers from a complex biological matrix such as meconium samples. The advantages of the developed method are the smaller demand for organic solvents and the minor sample handling, which allows a faster and accurate procedure, appropriate to confirm fetal exposure to cocaine/crack.

• 出版日期2014-4-15