论文部分内容阅读
目的采用LC-MS/MS法同时测定人血浆中咖啡因和氯苯那敏的浓度。方法人血浆样本经液液萃取后,选用InertsilODS-SP色谱柱(75 mm×2.1 mm,3μm),流动相为甲醇-5 mmol.L-1乙酸铵(含0.5%甲酸)(55∶45),流速0.3 mL.min-1,选用API3200型三重四极杆串联质谱仪的多重反应监测(MRM)扫描方式进行监测,电喷雾离子化源,正离子方式,选择监测离子反应分别为m/z 195.3→110.2(咖啡因)、m/z 275.2→230.2(氯苯那敏)和m/z 256.2→167.3(苯海拉明内标)。结果血浆中咖啡因和氯苯那敏的线性范围分别为4.0～1.2×103、0.05～15.0μg.L-1(r>0.999);批内、批间RSD均小于13%;相对误差(RE)均在±5%的范围内;平均提取回收率分别为67.6%±1.3%、69.1%±3.4%。结论所用方法快速、灵敏、专属性强、重复性好,适用于人血浆中咖啡因和氯苯那敏的测定,并可用于小儿氨酚烷胺泡腾片的人体生物等效性研究。
Objective To determine the concentration of caffeine and chlorpheniramine in human plasma simultaneously by LC-MS / MS. Methods Human plasma samples were separated by liquid-liquid extraction using Inertsil ODS-SP column (75 mm × 2.1 mm, 3 μm) with methanol-5 mmol·L-1 ammonium acetate (0.5% formic acid) , The flow rate was 0.3 mL · min-1. Multiple-reaction monitoring (MRM) scanning was performed with the API3200 triple quadrupole mass spectrometer. The electrospray ionization source and the positive ion mode were used to monitor the ion reaction in m / z 195.3 → 110.2 (caffeine), m / z 275.2 → 230.2 (chlorpheniramine) and m / z 256.2 → 167.3 (diphenhydramine internal standard). Results The linear ranges of caffeine and chlorpheniramine in plasma were 4.0 ~ 1.2 × 103 and 0.05 ~ 15.0 μg.L-1, respectively (r> 0.999). The intra-assay and inter-assay RSD were less than 13% ) Were within ± 5%. The average recovery was 67.6% ± 1.3% and 69.1% ± 3.4%, respectively. Conclusion The method is rapid, sensitive, specific and reproducible. It is suitable for the determination of caffeine and chlorpheniramine in human plasma and can be used to study the bioequivalence of paracetamol effervescent tablets in children.