液相色谱-质谱联用测定不同软膏中的莫匹罗星

Determination of mupirocin in different ointments by HPLC-MS

建立了一种液相色谱-质谱联用测定不同软膏中莫匹罗星含量的方法。色谱柱为AgilentXDB-C18(2.1mm×50mm,1.8μm);水相为0.1%甲酸-水,有机相为乙腈,梯度洗脱,流速为0.3mL·min^-1,柱温30℃。采用ESI离子源正离子模式,多反应离子监测模式下选择离子对501.3→326.7、501.3→308.9和501.3→291.0进行测定。结果表明,莫匹罗星检测质量浓度线性范围为10~500ng·mL^-1(r=0.9995);检出限和定量限分别为4、10ng·mL^-1,精密度实验的相对标准偏差(n=6)为0.8%;低、中、高浓度的加标回收率(n=3)分别为99.8%、109.2%和105.0%,相对标准偏差(n=3)分别为3.5%、1.6%和1.4%。该方法灵敏度高、专属性好、精密度高、简便、快速,可用于不同软膏中莫匹罗星的检测。

A method for the determination of mupirocin in different ointments by the high performance liquid chromatography-mass spectrometry (HPLC-MS) was established. The analytical column was Agilent XDB-C 18 (2.1 mm × 50 mm,1.8 μm), the mobile phase was 0.1% formic acid solution and acetonitrile with gradient elution, and the flow rate was 0.3 mL·min ^-1 . The column temperature was set at 30℃.The detection was achieved in ESI positive ion mode with 501.3→326.7, 501.3→308.9 and 501.3 →291.0. Results showed that the calibration curve was in a linearity over the range of 10~500 ng·mL^-1( r=0.999 5). The limit of detection and quantification was 4 ng·mL^-1 and 10 ng·mL^-1 , respectively. Precision was fine, with RSD(n=6)of 0.8%. The recoveries( n =3)of low, middle and high adding concentrations were 99.8%, 109.2% and 105.0%,and the RSD(n=3) were 3.5%, 1.6% and 1.4%, respectively. The established method is sensitive, specific, accurate, simple and rapid, which is applicable for the determination of mupirocin in different ointments.)