基于液相色谱-质谱联用法建立盐酸坦洛新缓释片比格犬体内含量检测方法

A method for detecting the content of tamsulosin hydrochloride sustained-release tablets in Beagle dogs based on liquid chromatography-mass spectrometry

建立了一种基于液相色谱-质谱联用法的市售盐酸坦洛新缓释片的动物体内含量变化检测方法,以比格犬为实验动物绘制药物药动学曲线,并验证方法的可靠性。色谱柱为Zorbax Extend-C18柱(150 mm×4.6 mm,5μm),保护柱为C18柱(4.0 mm×3.0 mm),流动相为甲醇-水-甲酸(V(甲醇):V(水):V(甲酸)=85:14:1),流速为0.6 mL/min,柱温为30℃,进样量为20μL。采用ESI离子源正离子多反应监测(MRM)模式选择离子对409.3→228.2、256.3→167.1进行测定。结果表明,盐酸坦洛新在0.1~10.0 ng/mL浓度范围内呈良好线性相关性,精密度为7.1%,提取回收率为92%,盐酸坦洛新缓释片的体内含量变化被准确描述。该方法灵敏度高、专属性好、精密度高,可用于简单快捷地检测市售盐酸坦洛新缓释片的动物体内含量变化。

In this study,we developed a method based on liquid chromatography-mass spectrometry to detect content changes in animals administered commercially available tamsulosin hydrochloride sustained-release tablets.Beagle dogs were used as the experimental animals to construct drug pharmacokinetic curves as well as to verify the reliability of the method.The column used was the Zorbax Extend-C18 column(150 mm×4.6 mm,5μm).C18(4.0 mm×3.0 mm)was used as the guard column,and the mobile phase was methanol-water-formic acid(V(methanol):V(water):V(formic)=85:14:1).The flow rate was 0.6 mL/min,column temperature was 30℃,and injection volume was 20μL.The ESI ion source positive ion multiple reaction monitoring mode was used to select ion pairs 409.3→228.2 and 256.3→167.1 for determination.The results showed that tamsulosin hydrochloride has a good linear correlation in the concentration range of 0.1~10.0 ng/mL.The precision was 7.1%,and the recovery rate of extraction was 92%.The content changes of tamsulosin hydrochloride sustained-release tablets in Beagle dogs were accurately described.The above method has high sensitivity,good specificity,and high precision and can quickly and easily detect the content changes in animals administered commercially available tamsulosin hydrochloride sustained-release tablets.