摘要
目的建立测定人血浆中苯磺酸氨氯地平含量的LC-MS方法。方法以Agilent1200型系列高效液相色谱仪进行测定。色谱条件:流动相;色谱柱:Agilent Eclipse Plus C183.5μm,3.0×150mm,柱温为30℃,流速为0.3ml/min;质谱条件:离子源为API-ES源,正离子方式检测,扫描方式为选择反应监测(SIM),用于定量的离子反应为氨氯地平母离子m/z409→子离子m/z238,碰撞诱导解离120;干燥气:氮气,流速10L/min,温度300℃,压力为40psi,毛细管电压3000V。结果线性范围为0.5～20.0ng/ml,相关系数r2=0.999,y=5950x+1191。方法的回收率均在98.57%～104.54%之内,日内、日间RSD均小于10%。结论 LC-MS法测定苯磺酸氨氯地平浓度结果稳定,重现性好,可用于苯磺酸氨氯地平人体药代动力学研究。
Objective To establish the LC-MS method for detecting the concentration of amlodipine besylate in human plasma.Methods The Agilent 1200 Series high-performance liquid chro- matography was used for detection. Chromatographic conditions： mobile phase; chromatogram column： Agilent Eclipse Plus C18, 3.5μm, 3.0 × 150 mm, temperature of 30 ℃ and flow rate of 0.3 ml/min; MS conditions： the API-ES source, the positive ion mode detection, the scan mode of reaction monitoring （SIM） for the quantitative ion reactions amlodipine mother ion rn/z 409→ ion rn/z 238 coUisioninduced dissociation 120; Dry air： nitrogen, flow rate of 10 L/min, temperature of 300 ℃, pressure of 40 psi, capillary voltage of 3 000 V. Results Linear range was 0.5 to 20.0 ng/ml, the correlation coefficient： r2 = 0.999, y = 5950x ＋ 1191. The recovery in the method was 98.57% to 104.54%; both intra-day RSD and inter-day RSD were less than 10%. Conclusions LC-MS has a good stability and reproducibility for pharmacokinetic studies of amlodipine besylate content in human plasma.
出处
《临床医学工程》
2012年第5期708-709,共2页
Clinical Medicine & Engineering
