Semi‐quantitative analysis of tramadol, dextromethorphan, and metabolites in decomposed skeletal tissues by ultra performance liquid chromatography quadrupole time of flight mass spectrometry,Drug Testing and Analysis

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Semi‐quantitative analysis of tramadol, dextromethorphan, and metabolites in decomposed skeletal tissues by ultra performance liquid chromatography quadrupole time of flight mass spectrometry
Drug Testing and Analysis ( IF 2.6 ) Pub Date : 2017-12-18 , DOI: 10.1002/dta.2327
H. M. Cornthwaite ₁ , L. Labine ₂ , J. H. Watterson _{1,

2}

Affiliation

The use of filtration/pass‐through extraction (FPTE) and ultra‐performance liquid chromatography quadrupole time‐of‐flight mass spectrometry (UPLC–qTOF–MS) to detect tramadol (TRAM), dextromethorphan (DXM), and metabolites from skeletal remains is described. Rats (n=5) received 50 mg/kg tramadol and were euthanized by CO₂ asphyxiation approximately 30 minutes post‐dose. Rats (n=4) received 75 mg/kg dextromethorphan and were euthanized by CO₂ asphyxiation approximately 45 minutes post‐dose. Remains decomposed to skeleton outdoors and vertebral bones were collected. Bones were cleaned, dried, and pulverized to a fine powder. Bones underwent dynamic methanolic extraction followed by FPTE before analysis using UPLC–qTOF–MS. Recovery was at least 90% of maximal value within the first 10 minutes of methanolic extraction for all samples assayed. Analytical response was measured over the concentration range of 1–500 ng/mL, with precision and bias <20% in triplicate analyses of all calibrators, and a limit of detection of 1 ng/mL for TRAM, DXM, and all metabolites. The vertebral bone analyzed using this method detected TRAM, DXM, and their respective metabolites in all samples analyzed.

中文翻译：

超高效液相色谱四极杆飞行时间质谱法对分解的骨骼组织中的曲马多，右美沙芬和代谢物进行半定量分析

使用过滤/通过萃取（FPTE）和超高效液相色谱四极杆飞行时间质谱（UPLC–qTOF–MS）检测曲马多（TRAM），右美沙芬（DXM）和骨骼残留物中的代谢物描述。大鼠（n = 5）接受50 mg / kg曲马多，并在给药后约30分钟通过CO ₂窒息安乐死。大鼠（n = 4）接受75 mg / kg右美沙芬，并通过CO ₂安乐死给药后约45分钟窒息。残骸在户外分解为骨骼，并收集了椎骨。将骨头清洗，干燥并粉碎成细粉。使用UPLC–qTOF–MS进行分析之前，先对骨骼进行动态甲醇萃取，然后进行FPTE。对于所有测定的样品，在甲醇提取的前10分钟内，回收率至少是最大值的90％。在1–500 ng / mL的浓度范围内测量分析响应，对所有校准物进行三次重复分析时，精密度和偏倚<20％，并且对TRAM，DXM和所有代谢物的检出限为1 ng / mL。使用此方法分析的椎骨在所有分析的样品中检测到TRAM，DXM及其各自的代谢产物。

更新日期：2017-12-18

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