摘要
目的：建立补肾壮阳类中药中11个磷酸二酯酶5型（PDE5型）抑制剂类药物的超高效液相色谱-四极杆飞行时间质谱（UPLC-Q-TOF-MS）快速检测方法。方法：样品经乙腈超声提取后,应用Agilent Extend-C18（1.8μm,2.1 mm×50 mm）色谱柱,以乙腈（A）-含0.1%醋酸的5 mmol·L-1醋酸铵水溶液（B）为流动相,梯度洗脱（0～3.5 min,27%A;3.5～12 min,27%A→69%A;12～14 min,69%A;14～20 min,27%A）,流速0.20 mL·min-1,采用四极杆飞行时间质谱（Q-TOF-MS）检测器,电喷雾离子源（ESI）,毛细管电压（capillary voltage）为4.0 kV,碎裂电压（Fragmentor）为180 V,正离子全扫描检测,扫描范围为m/z 100～1500。结果：那红地那非、红地那非、伐地那非、羟基豪莫西地那非、西地那非、豪莫西地那非、氨基他达拉非、他达拉非、硫代艾地那非、伪伐地那非、那莫西地那非11个化合物14 min内即可完成检测,在50～10000μg·L-1范围内线性相关系数均大于0.999;10倍定量限（LOQ）添加水平的加样回收率在93.8%～102.1%之间,RSD在2.6%～4.8%之间。结论：该方法操作简便、快速,经方法学验证可用于中成药中非法添加PDE5型抑制剂的快速检测。
Objective： To develop an ultra-performance liquid chromatography-quadrupole-time-of-flight mass spectrometric（ UPLC-Q-TOF-MS） method for the determination of 11 phosphodiesterase-5 inhibitors in Chinese medicine preparations for invigorants. Methods： Samples were extracted by ultrasonic method with acetonitrile,and then analyzed by UPLC-Q-TOF-MS. The Agilent Extend-C18column（ 1. 8 μm,2. 1 mm × 50 mm） was adopted with the mobile phase consisting of acetonitrile（ A）-5 mmol·L-1ammonium acetate water solution containing 0. 1% acetic acid（ B） with gradient elution（ 0-3. 5 min,27% A; 3. 5-12 min,27% A→69% A; 12-14 min,69% A; 14-20 min,27% A） at a flow rate of 0. 20 mL·min-1. The Q-TOF-MS was equipped with ESI source. The capillary voltage was 4 kV,and the fragmentor was 180 V,respectively. The detector was operated in positive ion mode by full scan range of m / z 100-1500. Results： Eleven PDE5 inhibitors were determined within 14 minutes, such as noracetildenafil,acetildenafil,vardenafil,hydroxyhomosildenafil,sildenafil,homosildenafil,aminotadalafil,tadalafil,thioaildenafil,pseudovardenafil,norneosildenafil. The correlation coefficients were all more than 0. 999 with linear range of 50-10000 μg·L-1. The average recovery of 11 PDE5 inhibitors at the spiked level of 10-fold LOQ was between 93. 8% and 102. 1% with the relative standard deviation between 2. 6% and 4. 8%. Conclusion： The method is simple and rapid,which can be applied to the detection of PDE5 inhibitors in Chinese medicine preparations according to methodology validation.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2014年第5期879-884,共6页
Chinese Journal of Pharmaceutical Analysis
