摘要
目的 建立测定人尿液中伪麻黄碱药物浓度的方法。方法 采用LC-MS/MS进行测定。色谱柱：美国Agilent Eclipseplus C18（4.6 mm×100 mm,3.5μm）;流动相：甲醇-水（3︰1,含0.005 mol.L 1甲酸铵和0.1%甲酸）;流速：0.5 mL.min 1;柱温：40℃。质谱条件：电喷雾电离源（ESI）,正离子化,扫描方式为选择性离子监测,伪麻黄碱m/z 166.2→148.1,内标对乙酰氨基酚m/z 152.1→110.1。结果 尿液中伪麻黄碱浓度在500~300 000μg.L 1（r2=0.998）内呈良好的线性关系,其批内、批间精密度RSD分别≤4.41%与≤10.04%;伪麻黄碱和内标的提取回收率均〉90%;尿液中伪麻黄碱的平均累积排泄率为44.57%。结论 本研究建立的LC-MS/MS测定人尿液中伪麻黄碱的方法准确、简便、灵敏、重复性好,可用于临床研究中伪麻黄碱的尿药含量测定。
OBJECTIVE To establish a method for determination of pseudoephedrine in urine samples of healthy volunteers. METHODS The pseudoephedrine was determined by LC-MS/MS. The separation was carried on an Agilent Eclipse plus C18（4.6 mm×100 mm, 3.5 μm） colume with a mobile phase of methanol-0.005 mol·L？1 ammonium formate apueous solution with 0.1% formic acid（3∶1） at the flow rate of 0.5 m L·min？1, The column formate temperature was set at 40 ℃. ESI source was applied and operated in positive ion mode. Quantitative determination was performed by using selective reaction monitoring（SRM） of m/z 166.2→148.1 for pseudoephedrine and m/z 152.1→110.1 for paracetamol used as internal standard. RESULTS Pseudoephedrine in urine samples showed good linearity in the range of 500？300 000 μg·L？1（r2=0.998）. The intra-batch and inter-batch precisions（RSD） were ≤4.41% and ≤10.04%, respectively. The extraction recoveries of pseudoephedrine and internal standard were more than 90%. The average cumulative excretion of pseudoephedrine in urine was 44.57%. CONCLUSION The method that using LC-MS/MS to determine pseudoephedrine in urine is accurate, simple and sentitive, and it has a good reproducibility. This method can be applied to the clinical pharmacokinetic study and therapeutic drug monitoring of pseudoephedrine.
出处
《中国现代应用药学》
CAS
CSCD
2015年第4期467-471,共5页
Chinese Journal of Modern Applied Pharmacy
基金
广东省自然科学基金(8151037001000001)
