摘要
目的:建立液相色谱-质谱-质谱(LC-MS-MS)法测定人血清中非洛地平的浓度。方法:血清样品经液-液萃取预处理。色谱柱为Xterra柱(50 mm×2.1 mm,3.5μm),流动相为乙腈-0.02%氨水,采用梯度洗脱,流速为0.3 mL/min。非洛地平和尼莫地平(内标)的多反应监测(MRM)扫描离子对分别为m/z382.1→145和m/z417.2→92,两者的保留时间分别为1.24 min和1.06 min。结果:非洛地平在0.04～20 ng/mL范围内线性关系良好(r=0.999 7),低、中、高浓度(0.08、8.0、16.0 ng/mL)的日内RSD分别为6.60%、7.22%和5.01%(n=6),日间RSD分别为9.42%、8.46%和5.12%(n=14),准确度为98.21%～106.20%(n=6)。结论:本法操作简便,检测准确、灵敏、专一,重复性好,适用于非洛地平血药浓度监测和药动学及生物利用度研究。
Objective： To establish a LC-MS-MS method for determining the concentration of felodipine in human serum. Methods：The serum samples were pretreated by liquid-liquid extraction. The chromatographic column was a Xterra column （50 mm×2.1 mm, 3.5 μm）. The mobile phase consisting of acetonitrile-0.02% ammonia water was eluted at a flow rate of 0.3 mL/min with gradient program. Felodipine and its internal standard nimodipine was monitored in multiple reaction monitoring（MRM） mode. The fragmentation transitions from precursor to production were m/z 382. 1/145 for felodipine and m/z 417.2/92 for nimodipine. The retention time of felodipine and nimodipine was 1.24 and 1.06 min, respectively. Results： For felodipine, the linear range was 0.04-20 ng/mL （r= 0. 999 7）. At low, middle and high concentrations（0.08,8.0,16.0 ng/mL）, the intra-day RSDs were 6. 60%,7. 22% and 5.01% （n=6） ,the inter-day RSDs were 9. 42%,8. 46% and 5. 12%（n= 14） ,and the accuracy rates were 98.2%- 106.20%（ n = 6 ）. Conclusion： This method is simple, accurate, sensitive, specific and reproducible for the determination of felodipine in human serum. It is suitable for therapeutic drug monitoring,pharmacokinetic and bioavailability study of felodipine.
出处
《药学服务与研究》
CAS
CSCD
2007年第4期253-255,共3页
Pharmaceutical Care and Research
关键词
非洛地平
色谱法
高压液相
光谱分析
质量
血药浓度
felodipine
chromatography, high pressure liquid
spectrum analysis, mass
plasma concentration
