Meng Liang, Dai Yong, Chen Chen, Zhang Jun
Department of Forensic Science, Fujian Police College, Fuzhou, China.
Engineering Research Center, Fujian Police College, Fuzhou, China.
Forensic Sci Res. 2020 Dec 7;6(3):273-280. doi: 10.1080/20961790.2020.1838403. eCollection 2021.
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 PointsThe 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.
一种基于高速研磨和固相微萃取(SPME)的新型毛发样本预处理方法已被应用于通过液相色谱-质谱联用(LC-MS)测定毛发样本中的苯丙胺、氯胺酮及其代谢物。取20毫克毛发样本,与2毫升饱和碳酸钠溶液一起,使用高效毛发研磨机在4℃下以70赫兹振荡研磨2分钟。离心后,转移1.5毫升上清液,采用直接浸入式固相微萃取(DI-SPME)进行处理。用纤维萃取的目标分析物经解吸后,采用LC-MS进行分析。在最佳条件下,所有分析物的回收率为90.2%-95.8%。该分析方法对所有分析物在0.2至10纳克/毫克范围内呈线性,相关系数在0.9985至0.9993之间。所有分析物的检测限估计为0.067纳克/毫克。准确度(平均相对误差)在±6.9%以内,精密度(相对标准误差)小于6.8%。毛发高速研磨与SPME相结合具有操作简便、环境友好和检测灵敏度高的优点。该方法为法医目的毛发样本中药物的灵敏检测提供了一种替代分析方法。要点固相微萃取用于结合LC-MS测定毛发中的药物。首次开发了毛发高速研磨与固相微萃取相结合的方法。实现了良好的线性、灵敏度、回收率和精密度。