摘要
建立高效液相色谱-串联质谱法(HPLC-MS/MS)测定人血浆中消旋卡多曲活性代谢物Thiorphan(TP)的含量及S-Methyl-Thiorphan(MTP)的相对含量。采用Kromasil C18色谱柱(25mm×4.6mm,5μm),流动相为V(水)∶V(乙腈)=72∶28,甲酸调pH至2.8。加抗氧化剂的血浆样品经乙腈直接沉淀后进样、MRM模式外标法定量,TP和MTP检测离子对分别为m/z252/218和m/z266/218。TP在6.25~3200μg/L范围内线性关系良好(r=0.9998);方法回收率为97.1%~109.0%,批内批间RSD分别小于3.5%及6.0%。
A high performance liquid chromatography-tandem mass spectrometric (HPLC-MS/MS) method was established for the determination of the racecadotril metabolites, thiorphan (TP) and S-methyl-thiorphan (MTP) in human plasma. Kromasil C18 column (25 mm ×4.6 mm, 5 μm) was used. The mobile phase was water-acetonitrile (72:28, pH 2. 8 with formic acid). The plasma added antioxidant was precipitated with acetonitrile and the content of drug was determined by HPLC-MS/MS using electrospray ionization. TP and MTP were detected on multiple reaction monitoring mode by the transitions from the precursor to the product ion (m/z 252/218 and m/z 266/218). For TP, calibration curve was linear in the range from 6.25 to 3200 μg/L, the limit of quantitation in plasma was 6.25 μg/L, the method recovery was 97.1% - 109.0% , the RSD of inter-and intra-day precision were less than 3.5% and 6.0% , respectively.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2008年第1期91-94,共4页
Chinese Journal of Analytical Chemistry