Simultaneous Determination of 14 Antipsychotic and Sedative Substances in Human Nails Using Microwave-assisted Extraction Combined with Liquid Chromatography-Tandem Mass Spectrometry

KeyWord:microwave-assisted extraction(MAE)  liquid chromatography-tandem mass spectrometry(LC-MS/MS)  nails  antipsychotic and sedative substances

Abstract:

      A method based on microwave-assisted extraction combined with liquid chromatography-tandem mass spectrometry(MAE/LC-MS/MS) was established for the simultaneous determination of 14 antipsychotic and sedative substances in human nails.About 20 mg of decontaminated and pulverized nail samples was microwave-assistedly extracted for twice in the presence of clozapine-d4 used as the internal standard, and the supernatant was determined by LC-MS/MS using the Allure PFPP column with a mobile phase of methanol(containing 20mmol/L ammonium acetate)-20mmol/L ammonium acetate buffer. Multiple reaction monitoring(MRM) mode was used to analyze 14 antipsychotic and sedative substances. Good linearities(r2¡Ý0.990) over the corresponding range were obtained for all the analytes.The limits of detection(LOD) were in the range of 0.1-50pg/mg and the limits of quantitation(LOQ) were 100pg/mg for most of the analytes.The deviations of intra- and inter-RSD were not more than 7.8%.Accuracies were within ¡À10.16%.Positive results were obtained from 7 authentic nail samples,which were in good accordance with the drug administration of the corresponding antipsychotic and sedative substances.The developed method presents a simplified,efficient and rapid procedure for sample preparation,and shows high sensitivity and selectivity,which is suitable for the simultaneous analysis of 14 antipsychotic and sedative substances at pg/mg levels in nail samples.