Fraser Candice D, Cornthwaite Heather M, Watterson James H
Department of Forensic Science, Laurentian University, 935 Ramsey Lake Rd, Sudbury, Ontario, P3L 1C6, Canada.
Department of Chemistry & Biochemistry, Laurentian University, 935 Ramsey Lake Rd, Sudbury, Ontario, P3L 1C6, Canada.
Drug Test Anal. 2015 Aug;7(8):708-13. doi: 10.1002/dta.1754. Epub 2014 Dec 8.
Analysis of decomposed skeletal tissues for dextromethorphan (DXM) and dextrorphan (DXT) using microwave assisted extraction (MAE), microplate solid-phase extraction (MPSPE) and gas chromatography-mass spectrometry (GC-MS) is described. Rats (n = 3) received 100 mg/kg DXM (i.p.) and were euthanized by CO2 asphyxiation roughly 20 min post-dose. Remains decomposed to skeleton outdoors and vertebral bones were recovered, cleaned, and pulverized. Pulverized bone underwent MAE using methanol as an extraction solvent in a closed microwave system, followed by MPSPE and GC-MS. Analyte stability under MAE conditions was assessed and found to be stable for at least 60 min irradiation time. The majority (>90%) of each analyte was recovered after 15 min. The MPSPE-GCMS method was fit to a quadratic response (R(2) > 0.99), over the concentration range 10-10 000 ng⋅mL(-1) , with coefficients of variation <20% in triplicate analysis. The MPSPE-GCMS method displayed a limit of detection of 10 ng⋅mL(-1) for both analytes. Following MAE for 60 min (80 °C, 1200 W), MPSPE-GCMS analysis of vertebral bone of DXM-exposed rats detected both analytes in all samples (DXM: 0.9-1.5 µg⋅g(-1) ; DXT: 0.5-1.8 µg⋅g(-1) ).
描述了使用微波辅助萃取（MAE）、微孔板固相萃取（MPSPE）和气相色谱-质谱联用（GC-MS）对分解的骨骼组织中的右美沙芬（DXM）和右啡烷（DXT）进行分析的方法。大鼠（n = 3）接受100 mg/kg的右美沙芬（腹腔注射），给药后约20分钟通过二氧化碳窒息法安乐死。尸体在户外分解为骨骼，回收椎骨，清洗并粉碎。粉碎后的骨骼在封闭的微波系统中使用甲醇作为萃取溶剂进行微波辅助萃取，随后进行微孔板固相萃取和气相色谱-质谱联用分析。评估了分析物在微波辅助萃取条件下的稳定性，发现其在至少60分钟的辐照时间内稳定。15分钟后，每种分析物的回收率大部分（>90%）。在10-10000 ng·mL-1的浓度范围内，微孔板固相萃取-气相色谱-质谱联用方法符合二次响应（R(2) > 0.99），三次重复分析的变异系数<20%。微孔板固相萃取-气相色谱-质谱联用方法对两种分析物的检测限均为10 ng·mL-1。在80°C、1200 W条件下微波辅助萃取60分钟后，对暴露于右美沙芬的大鼠椎骨进行微孔板固相萃取-气相色谱-质谱联用分析，在所有样品中均检测到两种分析物（右美沙芬：0.9-1.5 μg·g-1；右啡烷：0.5-1.8 μg·g-1）。
