固相萃取-液相串联质谱测定人血浆中安妥沙星的药物浓度

Determination of Antofloxacin in Human Plasma by Solid Phase Extraction-Liquid Chromatography-Mass Spectrometry

建立了专属性更高的固相萃取(SPE)-高效液相三重四级杆质谱(LC-MS/MS)测定人血浆中安妥沙星的方法。血浆样品经弱阴离子固相萃取柱净化后,洗脱吹干,复溶后进行检测。采用Agilent Eclipse plusC8色谱柱,流动相为10mmol/L乙酸铵(pH 3.5)-甲醇(35∶65,V/V),流速为0.35mL/min,选择离子检测,线性范围为7.0～5080μg/L,R>0.996,检出限0.5μg/L,绝对回收率>77.6%,日间相对标准偏差<7.9%。将本方法用于受试者给药后的血药浓度测定,结果满意。

A new and specific method has been developed for the determination of antofloxacin in human plasma by solid phase extraction-liquid chromatography coupled with tandem spectrometry.The samples were extracted and purified by wean anion solid phase extraction.The eluent was dried and reconstituted before analysis.The separation was performed on an Agilent Eclipse plus C8 column,with a mobile phase consisting of 10 mmol/L ammonium acetate（pH 3.5）-methanol（35∶65,V/V） at a flow of 0.35 mL/min.Identification and quantification were achieved by LC-MS/MS in a positive mode and multiple reactions monitoring（MRM）.Good linearity was observed in a range of 7.0-5080 μg/L with a correlation coefficient of more than 0.996.The detection limit was 0.5 μg/L.Sample recovery was 77.6%,and inter-day coefficient of variation was less than 7.9%.The proposed method has been applied to the determination of antofloxacin in plasma after subjects were orally given 400 mg of antofloxacin tablets.