超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速测定羊乳中11种磷酸二酯酶-5抑制剂

Rapid determination of eleven PDEs-5 in goat’s milk by high performance liquid chromatography quadrupole/electrostatic field orbitrap high resolution mass spectrometry

建立了超高效液相-四极杆/静电场轨道阱系统(UPLC-Q-Exctive-MS/MS)快速检测羊乳中磷酸二酯酶-5抑制剂(豪莫西地那非、伐地那非、氨基他达拉非、那红地那非、红地那非、伪伐地那非、那莫西地那非、硫代艾地那非、他达拉非、西地那非及羟基豪莫西地那非)的方法。样品经乙腈提取,PRiME HLB净化后,以0.1%甲酸水-乙腈为流动相,采用ACQUITY UPLC HSS T3(2.1×100 mm,1.8 mm)色谱柱分离。在电喷雾正离子模式下(ESI+)下优化影响全扫分辨率,结合二级质谱提高准确度。结果表明,在0~100 mg/L浓度范围,目标化合物线性关系良好,方法检出限为2.5~5.0 mg/kg,本方法在3个水平下的加标回收率为75.4%~97.8%,RSD为1.6%~6.2%。本方法成功应用于羊乳中11种磷酸二酯酶-5抑制剂的快速检测。

A high performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass method was developed for the determination of 11 PDEs in goat’s milk.The goat’s milk sample was extracted by acetonitrile and cleaned up with PRiME HLB.Then,separation of the 11 PDEs-5 was performed on an ACQUITY UPLC HSS T3(2.1×100 mm,1.8 mm)column by using 0.1%formic acid-acetonitrile as the mobile phase.The mass resolution was optimized under the electrospray positive ion mode(ESI+)and the accuracy of qualitative analysis was further improved by combining with two stage threshold-triggered full mass scan mode.The linear range of eleven PDEs-5 was 0-100 mg/L and the limit of detection was between 2.5 mg/kg and5.0 mg/kg,the recoveries were in the range of 75.4%-97.8%,with the relative standard deviation in the range of 1.6%-6.2%.The method was successfully used for the determinatiun of eleven PDEs-5 in goat’s milk.