Validation of a method for simultaneous analysis of cocaine, benzoylecognine and cocaethylene in urine using gas chromatography-mass spectrometry

Abstract The present study describes a method for simultaneous analysis of cocaine, benzoylecgonine and cocaethylene in urine samples. After solid phase extraction, Gas Chromatography-Mass Spectrometry was used for identification and quantification. The calibration curves were linear at 20 - 3000 ng/mL, r2 0.9997 for benzoylecgonine, 15 - 2000 ng/mL, r2 0.9985 and r2 0.9993 for cocaine and cocaethylene, respectively. Accuracy values: cocaine: 93,5 - 102,1%; benzoylecgonine: 97,5 - 104,8%; cocaethylene: 90,6 - 101,5%. Precision values: cocaine: C.V 5,4 - 14,6%; benzoylecgonine: C.V 7,8 - 12,3%; cocaethylene: C.V 5,9 - 12,3%. Detection and quantification limit values: cocaine and cocaethylene:10 ng/mL and 15 ng/mL, respectivalty; benzoylecgonine:15 ng/mL and 20 ng/mL, respectivaley. Recovery values: cocaine: 78,0 - 85,8%; benzoylecgonine: 74,0 - 79,8%; cocaethylene: 83,0 - 91,5%. The method described is advantageous compared to others, as it simultaneously detects the major analytes found in urine samples due to cocaine use and has been successfully validated.

摘要
本研究报道了一种可同时分析尿液样本中可卡因（cocaine）、苯甲酰爱康宁（benzoylecgonine）及可乐乙酯（cocaethylene）的检测方法。样本经固相萃取（solid phase extraction）处理后，采用气相色谱-质谱联用法（Gas Chromatography-Mass Spectrometry）完成定性与定量分析。
校准曲线的线性范围及对应决定系数如下：苯甲酰爱康宁为20~3000 ng/mL，r²=0.9997；可卡因与可乐乙酯的线性范围均为15~2000 ng/mL，二者r²分别为0.9985与0.9993。
准确度性能指标：可卡因为93.5%~102.1%；苯甲酰爱康宁为97.5%~104.8%；可乐乙酯为90.6%~101.5%。
精密度性能指标：可卡因的变异系数（C.V）为5.4%~14.6%；苯甲酰爱康宁的变异系数为7.8%~12.3%；可乐乙酯的变异系数为5.9%~12.3%。
检测限与定量限：可卡因与可乐乙酯分别为10 ng/mL、15 ng/mL；苯甲酰爱康宁的检测限与定量限分别为15 ng/mL、20 ng/mL。
回收率性能指标：可卡因为78.0%~85.8%；苯甲酰爱康宁为74.0%~79.8%；可乐乙酯为83.0%~91.5%。
相较于其他同类检测方法，本方法可同时检出可卡因滥用后尿液样本中的主要相关分析物，且已完成成功验证，具备显著应用优势。