高效液相色谱-四极杆/线性离子阱质谱仪测定盐酸黄酮哌酯中的1-(2-羟乙基)哌啶残留

Determination of 1-(2-Hydroxyethyl) piperidine in Flavoxate Hydrochloride by HPLC-QTRAP-MS/MS

建立了盐酸黄酮哌酯中1-(2-羟乙基)哌啶的高效液相色谱-四极杆/线性离子阱质谱(HPLC-QTRAP-MS/MS)定量分析方法。盐酸黄酮哌酯药物用0.1%甲酸溶解后,经Agilent ZORBAX SB-Aq C_(18)(2.1 mm×100mm,1.8μm)色谱柱分离,以乙腈-0.1%甲酸水作为流动相进行梯度洗脱,采用电喷雾正离子扫描方式,以选择反应监测(SRM)模式进行检测。结果表明,1-(2-羟乙基)哌啶在10~100μg/L范围内线性关系良好(r=0.999 7),加标回收率为98.9%~106.8%,相对标准偏差(RSD)均不大于3.0%,方法检出限(S/N=3)为6.0mg/L,方法定量下限(S/N=10)为20 mg/L。该方法简单、灵敏、准确,适用于盐酸黄酮哌酯中1-(2-羟乙基)哌啶残留的测定。

A high performance liquid chromatography-quadrupole ion trap tandem mass spectrometric（HPLC-QTRAP-MS/MS） method was developed for the quantification of 1-（2-hydroxyethyl） piperidine residue in flavoxate hydrochloride.After dissolved with 0.1% formic acid,the flavoxate hydrochloride sample was loaded onto an Agilent ZORBAX SB-Aq C18（2.1 mm×100 mm,1.8 μm） column to separate with a mobile phase of 0.1% formic acid-acetonitrile.The electrospray was operated in positive ion mode,and the sample was monitored in the select reaction monitoring（SRM） mode.As a result,the calibration curve of 1-（2-hydroxyethyl）piperidine showed a good linearity（r=0.999 7） in the range of 10-100 μg/L.The recoveries were in the range of 98.9%-106.8%,with relative standard deviations（RSDs） not more than 3.0%.The limit of detection（LOD,S/N=3） for the method was 6.0 mg/L,and the limit of quantitation（LOQ,S/N=10） was 20 mg/L.The method has the advantages of simple operation,high sensitivity and good reproducibility,and could be used for the detection of 1-（2-hydroxyethyl）piperidine in flavoxate hydrochloride.