Determination of amphetamines, ketamine and their metabolites in hair with high-speed grinding and solid-phase microextraction followed by LC-MS

A novel hair sample pre-treatment method based on high-speed grinding and solid-phase microextraction (SPME) had been applied for the determination of amphetamines, ketamine and their metabolites in hair samples by liquid chromatography-mass spectrometry (LC-MS). A 20 mg sample of hair was ground with 2 mL of saturated sodium carbonate solution using a high-efficiency hair grinder with 70 Hz oscillation for 2 min at 4 °C. After centrifuging, 1.5 mL of the supernatant was transferred and treated with SPME by direct immersion (DI-SPME). The target analytes extracted by fibre were desorbed and analysed using LC-MS. Under the optimum conditions, a recovery of 90.2%–95.8% was obtained for all analytes. The analytical method was linear for all analytes in the range from 0.2 to 10 ng/mg with the correlation coefficient ranging from 0.9985 to 0.9993. The detection limits for all analytes were estimated to be 0.067 ng/mg. The accuracy (mean relative error) was within ±6.9% and the precision (relative standard error) was less than 6.8%. The combination of high-speed grinding of hair and SPME had the advantages of being easy to perform, environment-friendly and high in detection sensitivity. The proposed method offered an alternative analytical approach for the sensitive detection of drugs in hair samples for forensic purposes. KEY POINTS: The SPME was involved for the determination of drugs in hair with LC-MS. The hair high-speed grinding combined with SPME was firstly developed. Good linearity, sensitivity, recovery and precision were achieved.