title: A high-throughput method based on microwave-assisted extraction and liquid chromatography-tandem mass spectrometry for simultaneous analysis of amphetamines, ketamine, opiates, and their metabolites in hair.
abstract: A total sample-preparation and analysis time of 50 min is required for the high-throughput method of hair analysis proposed in this paper. The method is applicable to analysis of drugs commonly used in Asia, and their metabolites--methamphetamine (MA), amphetamine (AMP), methylenedioxymethamphetamine (MDMA), methylenedioxyamphetamine (MDA), ketamine (K), norketamine (NK), dehydronorketamine (DHNK), 6-acetylmorphine (6-AM), morphine (MOR), and codeine (COD). Cut and weighed hair (10 mg) was incubated for 3 min with methanol-trifluoroacetic acid (TFA) during microwave-assisted extraction (MAE) at 700 W. The incubation solution was evaporated, the residue was reconstituted in deionized water-methanol, 99:1 (v/v), and 20 μL was injected on to a core-shell column (50 × 4.6 mm, 2.6 μm particle size) for liquid chromatographic-tandem mass spectrometric (LC-MS-MS) analysis. Gradient elution separation was performed in 8 min at a flow rate of 1 mL min(-1). No signal interfering with any of the analytes was found in fourteen blank hair samples from different sources. The limits of detection and quantification were 0.5 pg mg(-1) and 2.0 pg mg(-1), respectively, for MA, AMP, MDMA, MDA, K, NK, and DHNK, and 2.0 pg mg(-1) and 5.0 pg mg(-1), respectively, for 6-AM, MOR and COD. The linear range was between the LOQ and 1000 pg mg(-1), and the correlation coefficients were all greater than 0.999. Investigation of matrix effects revealed that all the analytes were suppressed by less than 20% and the standard deviation (SD) was always less than 7%. Recovery was always greater than 90% and the SD for each compound was less than 6%. Precision and accuracy for each analyte were within 15%. Eight authentic hair specimens from known drug abusers were successfully analyzed. Compared with traditional overnight incubation methods, the rapid 3-min extraction time achieved similar or greater extraction yields. Sample preparation by MAE was a reliable procedure for extraction of the analytes from hair but substantially simpler and faster than other methods.
authors.affiliation: Institute of Medicine, Chung Shan Medical University, Taichung, 40201, Taiwan.
authors.forename: Yuan-Jhe
authors.initials: YJ
authors.lastname: Chang
authors.forename: Mu-Rong
authors.initials: MR
authors.lastname: Chao
authors.forename: Su-Chin
authors.initials: SC
authors.lastname: Chen
authors.forename: Chih-Hong
authors.initials: CH
authors.lastname: Chen
authors.forename: Yan-Zin
authors.initials: YZ
authors.lastname: Chang
mesh_terms: D000662:Amphetamines / Q000032:analysis* / Q000302:isolation & purification / Q000378:metabolism; D000701:Analgesics, Opioid / Q000032:analysis* / Q000302:isolation & purification / Q000378:metabolism; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D006197:Hair / Q000737:chemistry*; D057166:High-Throughput Screening Assays / Q000379:methods*; D006801:Humans; D013287:Illicit Drugs / Q000032:analysis* / Q000302:isolation & purification / Q000378:metabolism; D007649:Ketamine / Q000032:analysis* / Q000302:isolation & purification / Q000378:metabolism; D008872:Microwaves; D015813:Substance Abuse Detection / Q000379:methods; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D000662:Amphetamines; D000701:Analgesics, Opioid; D013287:Illicit Drugs; D007649:Ketamine