Detecting method for high performance liquid chromatography-tandem mass spectrometry of PDE5 type inhibitors in drugs, healthcare products and food

药品、保健食品和食品中PDE<sub>5</sub>型抑制剂的高效液相色谱-串联质谱联用检测方法

Abstract

The invention discloses a detecting method for high performance liquid chromatography-tandem mass spectrometry of PDE5 type inhibitors in drugs, healthcare products and food. Acetonitrile is used as extractant. 50 percent of acetonitrile is used as diluent. A formic acid-ammonium acetate solution-methanol-acetonitrile system is used as a flowing phase. With a flowing speed of 0.2-0.4 ml/min and a column temperature of 20-50 DEG C, liquid chromatographic column performs separation, then electrospray ionization (ESI) ion source is adopted for ionization, a positive ion mode is adopted for fully scanning a primary and a secondary mass spectrum, and whether the PDE5 type inhibitors is added in a sample can be qualitatively judged according to the secondary mass spectrum. The detecting method has simple sample pretreatment, high accuracy, good specificity, high detection flexibility and short analysis period, can accomplish qualitative analysis of 11 PDE5 type inhibitors through one experiment, is suitable for microscale analysis of the PDE5 type inhibitors and can be used as a verification and arbitration method for supervision inspection.
本发明公开了一种药品、保健食品和食品中PDE<sub>5</sub>型抑制剂的高效液相色谱-串联质谱联用检测方法,以乙腈为提取剂、50%乙腈为稀释剂、甲酸-乙酸铵溶液-甲醇-乙腈体系为流动相,在流速为0.2~0.4ml/min、柱温20~50℃条件下经液相色谱柱分离后,采用电喷雾(ESI)离子源离子化,正离子模式全扫描一、二级质谱,根据二级质谱定性判别样品是否添加PDE<sub>5</sub>型抑制剂。本方法的样品前处理简单,准确度高、专属性好、检测灵敏度高、分析周期短,一次实验就能完成十一种PDE<sub>5</sub>型抑制剂的定性分析,适合PDE<sub>5</sub>型抑制剂的微量分析,也可作为监督检验的确证和仲裁方法。

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    CN-105572242-AMay 11, 2016广东出入境检验检疫局检验检疫技术中心一种保健食品中pde-5抑制剂类违禁药的非目标物快速筛查检测方法