生物检材中复方芬太尼的气相色谱和气相色谱/质谱检测

目的：建立生物检材中复方芬太尼的气相色谱（GC）和气相色谱/质谱检测方法（GC/MS法）。方法：检材经10%氢氧化钠调pH=10,乙醚萃取,气/质联用法定性,气相色谱内标法定量检测生物检材中复方芬太尼。结果：GC/MS法分析芬太尼的选择离子m/z为245,146;异丙嗪的选择离子m/z为284,72。GC检测的回归方程、线性检测范围、相关系数、回收率、最低检出浓度分别为：心血中芬太尼为Y=23.376X＋0.516 8（μg/mL）,（0.1~220）μg/mL,0.985,（98.5±3.5）%,0.1μg/mL,异丙嗪为Y=16.537X＋0.158 4（μg/mL）,（0.12~200）μg/mL,0.974,（97.50±2.0）%,0.12μg/mL;肝组织中芬太尼为Y=82.236X＋0.413 4（μg/mL）,（0.1~220）μg/g,0.975,（95.6±0.75）%,0.1μg/g,异丙嗪为Y=40.437X＋0.134 2（μg/mL）,（0.12~200）μg/g,0.964,（94.8±0.15）%,0.12μg/g。染毒家兔心血及心、肝、脾、肺、肾和脑中芬太尼的含量依次为：（24.39±6.43）μg/mL及（84.96±1.03）,（73.82±1.73）,（55.74±2.07）,（42.64±1.38）,（35.94±2.87）,（10.15±7.05）μg/g,异丙嗪的含量依次为：（146.69±2.43）μg/mL及（204.96±13.03）,（213.32±1.73）,（115.74±3.07）,（95.64±5.38）,（195.34±2.87）,（170.15±1.05）μg/g。结论：生物检材中GC/MS法选择性好,定性准确,GC检测简便,快速,灵敏,定量结果准确,可用于芬太尼麻醉意外中毒的临床快速检验诊断和芬太尼滥用中毒死亡案件的法医学鉴定。

The analysis of compound-fentanyl in biomaterial by gas chromatography and gas chromatography-mass spectrography

Objective：To establish the method for detecting the compound-Fentanyl in biomaterial by gas chromatography（GC） and gas chromatography-mass spectrography（GC/MS）.Methods：The specimen was alkalified to pH10,and then extracted with ether.The extraction was analyzed qualitatively and quantitatively by GC/MS and GC respectively.Results：The m/z of selected ion of Fentanyl was 245,146 and the m/z of selected ion of promethazine was 284,72 by GC/MS.The regression equation,linear range,correlation coefficient,recovery rate,limit of detection of fentanyl and promethazine in heart blood was Y=23.376X＋0.5168（μg/g）,0.1~220 μg/mL,0.985,（98.5±3.5）%,0.1 μg/mL and Y=16.537X＋0.158 4（μg/g）,0.12~200 μg/mL,0.974,（97.50±2.0）%,0.12 μg/mL respectively;those of Fentanyl and Promethazine in liver was Y=82.236X＋0.413 4（μg/g）,0.1~220 μg/g,0.975,（95.6±0.75）%,0.1 μg/g and Y=40.437X＋0.134 2（μg/g）,0.12~200 μg/g,0.964,（94.8±0.15）%,0.12 μg/g respectively.The concentrations of fentanyl and promethazine after administration in heart-blood,heart,liver,spleen,lung,kidney and brain were（24.39±6.43） μg/mL,（84.96±1.03）,（73.82±1.73）,（55.74±2.07）,（42.64±1.38）,（35.94±2.87）,（10.5±7.05） μg/g and（146.69±2.43） μg/mL,（204.96±13.03）,（213.32±1.73）,（115.74±3.07）,（95.64±5.38）,（195.34±2.87）,（170.15±1.05） μg/g（n=6,μg/mL or μg/g） respectively.Conclusion：This method is more selective,more sensitive,simpler,more accurate,and can be applied not only to clinical diagnosis of fentanyl poisoning,but also to forensic identify of fentanyl poisoning death.