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目的建立灵敏、快速的液相色谱-串联质谱法测定兔血清及组织中氟尿嘧啶的浓度。方法血清及组织样本经乙酸乙酯一步提取后,以乙腈-水(70:30,V/V)为流动相,Hypercarb C_(18)柱分离,采用电喷雾电离源,以多反应离子检测(MRM)方式进行负离子检测。用于定量分析的离子反应分别为m/z128.9→m/z41.9(氟尿嘧啶)和m/z188.7→m/z41.9(内标,溴尿嘧啶)。结果测定血清中氟尿嘧啶的线性范围为0.25～50μg·L~(-1),定量下限为0.25μg·L~(-1)。日内、日间精密度(RSD)均小于11%。食管组织中氟尿嘧啶的线性范围为0.5～100μg·L~(-1),定量下限为0.50μg·L~(-1)。日内、日间精密度(RSD)均小于10%。结论该法选择性强、灵敏度很高、操作简便、分析时间短,且可同时测定血清及组织中药物浓度,适用于极低浓度氟尿嘧啶生物样本的大批量检测。
Objective To establish a sensitive and rapid method for the determination of fluorouracil in rabbit serum and tissues by liquid chromatography-tandem mass spectrometry. Methods The serum and tissue samples were separated by Hypercarb C_ (18) column with acetonitrile-water (70:30, V / V) after one step extraction with ethyl acetate and electrospray ionization. MRM) for negative ion detection. The ion reactions used for the quantitative analysis were m / z 128.9 → m / z 41.9 (fluorouracil) and m / z 188.7 → m / z 41.9 (internal standard, bromouracil), respectively. Results The linear range of fluorouracil in serum was 0.25-50 μg · L -1 and the lower limit of quantitation was 0.25 μg · L -1. Day, day precision (RSD) were less than 11%. The linear range of fluorouracil in esophageal tissue was 0.5-100 μg · L -1, and the lower limit of quantitation was 0.50 μg · L -1. Day, day precision (RSD) are less than 10%. Conclusion The method is selective, sensitive, easy to operate, and has short analysis time. It can simultaneously measure the concentration of drugs in serum and tissue and is suitable for the mass detection of very low concentration of fluorouracil in biological samples.