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目的建立HPLC-MS/MS法同时测定人尿液中对氟马尿酸和对氟苯甲酸浓度的方法。方法以双氯芬酸钠为内标,尿液样品经甲基叔丁基醚萃取后,氮气吹干,流动相复融,用CAPCELL PAK C18MGⅡ色谱柱进行分离,流动相为0.05%甲酸甲醇-水(90∶10),流量为4 mL.min-1,柱温为18℃;大气压电喷雾离子源(ESI),多重反应选择离子监测(MRM),负离子模式检测。结果对氟马尿酸和对氟苯甲酸线性范围为20～4000 g.mL-1(r>0.99)。高、中、低质控样品的日内RSD<6%,日间RSD<7%,绝对回收率均>75%。结论本方法简便、快速、灵敏、重现性好,能够有效地检测人尿液中2种代谢物的含量。
OBJECTIVE To establish a HPLC-MS / MS method for the simultaneous determination of fluoroquinolones and p-fluorobenzoic acid in human urine. Methods Diclofenac sodium was used as an internal standard. The urine samples were extracted with methyl tert-butyl ether (TBS). The urine samples were dried under a nitrogen atmosphere and the mobile phase was reconstituted. The mobile phase consisted of 0.05% formic acid in methanol and water : 10) at a flow rate of 4 mL.min-1 with a column temperature of 18 ° C. Electrospray ionization (ESI), multiple reaction selective ion monitoring (MRM) and negative ion mode were used. Results The linear range of fluomacetin and p-fluorobenzoic acid was 20 ~ 4000 g · mL-1 (r> 0.99). High, medium and low quality control samples within the day RSD <6%, daytime RSD <7%, the absolute recovery rate was> 75%. Conclusion The method is simple, rapid, sensitive and reproducible. It can effectively detect the content of two metabolites in human urine.