超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法快速筛查配制酒中的11种那非类药物

Ultra high performance liquid chromatography-quadrupole/Orbitrap mass spectrometry for the rapid screening and confirmation of eleven kinds of sildenafil drug illegally added in compound wine

目的建立超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法快速筛查配制酒中的11种那非类药物的分析方法。方法样品稀释、过滤后经Hypersil GOLD C18(150 mm×2. 1 mm,1. 9μm)分离,超高效液相色谱-四极杆/静电场轨道阱质谱分离检测,电离模式为电喷雾正离子模式,数据采集使用一级母离子全扫描和数据依赖的二级子离子扫描(Full MS/dd-MS2)模式。结果在11 min内,11种那非类化合物能得到较好分离;在3μg/L^100μg/L内线性关系良好,检出限为1μg/L^2μg/L,定量限为3μg/L^5μg/L,回收率为86. 4%~107. 9%,RSD为0. 5%~6. 7%(n=3)。705批配制酒中,检出西地那非和伐地那非4批次,阳性率为0. 6%。结论该方法简单快捷,定性准确,可用于配制酒中11种那非类药物的快速筛查及确证。

Objective To establish an ultra high performance liquid chromatography-quadrupole/orbitrap mass spectrometry method for the screening and confirmation of eleven kinds of sildenafil drug illegally added in compound wine. Methods The samples were diluted and filtrated before analysis,separated by a Hypersil GOLD C18( 150 mm × 2. 1 mm,1. 9 μm),and determined via UHPLC-Q/Orbitrap HRMS. The electro spray ion source in the positive mode was used,and the data was collected using full mass and full MS/dd-MS2( Full MS/dd-MS2). Results Within 11 minutes,11 kinds of sildenafil compounds can be well separated;the linear relationship is good within 3 μg/L-100 μg/L,the detection limit is within1 μg/L ~ 2 μg/L,and the limit of quantification is within 3 μg/L-5 μg/L,the recovery is within 86. 4%-107. 9%,and the RSD was within 0. 5%-6. 7%( n = 3). Out of 705 batches of wine,4 batches of sildenafil and vardenafil were detected,with a positive rate of 0. 6%. Conclusion The method is simple,fast,and accurate,and it provides a novel powerful tool for the high-throughput rapid screening and confirmation of 11 kinds of sildenafil drug in compound wine.