高效液相色谱-四极杆/线性离子阱质谱测定替米沙坦中N-甲基邻苯二胺残留量

建立了高效液相色谱-四极杆/线性离子阱质谱(HPLC-QTRAP-MS/MS)测定替米沙坦中N-甲基邻苯二胺残留量的分析方法。替米沙坦药物以水-乙腈(80∶20,体积比)溶解后,采用Agilent Eclipse XDB-C18色谱柱(3.5μm,2.1 mm×100 mm)进行分离,以0.1%(体积分数)甲酸水和乙腈作为流动相进行梯度洗脱,电喷雾正离子(ESI+)扫描方式下选择离子监测(SRM)模式对样品进行检测。结果表明,N-甲基邻苯二胺在2.0~50μg/L范围内线性关系良好(r0.99),检出限(S/N=3)为0.5μg/L,定量下限(S/N=10)为2.0μg/L。该方法操作简单、灵敏度高、重现性好,可用于替米沙坦中N-甲基邻苯二胺残留量的测定。

Determination of N-Methyl-o-phenylenediamine in Telmisartan by HPLC-QTRAP-MS/MS

A high performance liquid chromatography-quadrupole ion mass spectrometric (HPLC-QTRAP-MS/MS) method was developed for the determination of N-Methyl-o-phenylenediamine residues in telmisartan.After extracted with water-acetonitrile (80 ∶ 20,by volume),the telmisartan samples were separated on an Agilent Eclipse XDB-C18 column(3.5 μm,2.1 mm × 100 mm) with a mobile phase of 0.1％ formic acid solution-acetonitrile.The electrospray was operated in the positive mode and the samples were monitored under the select reaction monitoring (SRM) mode.As a result,the calibration curves of N-Methyl-o-phenylenediamine showed a good linearity (r ＞ 0.99) in the range of 2.0-50 μg/L.The limits of detection (S/N =3) was 0.5 μg/L,and the limits of quantitation(S/N =10) was 2.0 μg/L.The method has the advantages of simple operation,high sensitivity,good reproducibility,and could be used for the detection of N-Methyl-o-phenylenediamine residues in telmisartan.