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目的:建立测定小鼠脑组织中枸橼酸芬太尼的液相色谱-质谱联用法。方法:色谱柱为Agilent Zorbax SB-C18(2.1mm×150mm,3μm);流动相为乙腈-0.05%甲酸(38∶62),流速0.3mL·min-1;柱温35℃;质谱条件为电喷雾电离源(ESI),以选择性正离子方式检测,枸橼酸芬太尼和内标盐酸美金刚的选择检测离子分别为m/z337.30([M+H]+)、m/z180.20([M+H]+)。小鼠尾静脉注射给予枸橼酸芬太尼(0.1mg·kg-1)30min后,测定12只小鼠脑组织内芬太尼的浓度。结果:小鼠脑组织内枸橼酸芬太尼的质量浓度为(18.4±6.4)μg·L-1,线性范围为1～50μg·L-1,检测限为0.25μg·L-1,方法回收率均大于95%。结论:本方法专属性强,灵敏度高,线性关系良好,操作简便,适用于小鼠脑组织内枸酸橼芬太尼浓度的测定。同时也可以为其他生物组织样本中芬太尼浓度测定提供参考。
Objective: To establish a liquid chromatography-mass spectrometry method for the determination of fentanyl in mouse brain. METHODS: The column was Agilent Zorbax SB-C18 (2.1 mm × 150 mm, 3 μm). The mobile phase was acetonitrile-0.05% formic acid (38:62), the flow rate was 0.3 mL · min- Spray ionization source (ESI) was detected by selective positive ion method. The detected ions of fentanyl citrate and internal standard memantine hydrochloride were m / z 337.30 ([M + H] +), m / z 180 .20 ([M + H] +). After intravenous injection of fentanyl (0.1 mg · kg-1) into the tail vein of mice for 30 min, the concentration of fentanyl in the brains of 12 mice was measured. Results: The concentration of fentanyl in mouse brain tissue was (18.4 ± 6.4) μg · L-1, the linear range was 1 ~ 50μg · L-1, the detection limit was 0.25μg · L-1. Recovery rates were greater than 95%. Conclusion: This method is specific, sensitive, linear, and easy to operate. It is suitable for the determination of citrate fentanyl concentration in mouse brain. It also can provide a reference for the determination of fentanyl concentration in other biological samples.