高效液相色谱-串联质谱法测定食品、保健食品中一种新型他达拉非衍生物

Determination of a novel tadalafil derivatives added illegally into food and health products by high performance liquid chromatography-tandem mass spectrometry

目的建立高效液相色谱-串联质谱法测定食品、保健食品中一种新型的非法添加物3-羟基丙基去甲他达拉非的分析方法。方法样品采用甲醇超声提取,以Agilent Eclipse Plus C18(2.1 mm×100 mm,1.8μm)色谱柱分离待测物,以0.1%甲酸溶液-甲醇为流动相,梯度洗脱,流速为0.4mL/min;在电喷雾正离子化模式下,采用多反应监测(multiple reaction monitoring,MRM)模式检测,标准曲线进行外标法定量。结果3-羟基丙基去甲他达拉非在2~50μg/mL范围内线性良好,相关系数r2≥0.999,方法检出限和定量限分别为50μg/kg和100μg/kg,回收率为74.58%~117.97%,RSD≤5.0%。结论该方法简单、准确、高效、专属性强,适用于食品和保健食品中非法添加3-羟基丙基去甲他达拉非的定性和定量检测。

Objective To establish a method for the determination of 3-hydroxypropyl decatadafil——a new illegal additive in food and health food by high performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted by ultrasonic method using methanol, and the extracts were carried out on an Agilent Eclipse Plμs C18 column(2.1 mm×100 mm, 1.8 μm) with gradient elution of 0.1% aqueous formic acid solution and methanol. The flow rate was 0.4 mL/min. Determination was performed by multiple reaction monitoring mode using electrospray ionization in positive ion mode. The external standard method of peak area was employed for quantitative analysis. Results Good linearity was obtained in the range of 2-50 μg/mL for 3-hyd rox ypropyl-nortadalafil, and correlation coefficients(r2) were above 0.999. The limits of detection(LODs) and quantification(LOQs) were 50 μg/kg and 100 μg/kg, respectively. The average recoveries were in the range of 74.58%-117.97%. The relative standard deviations were lower than 5.0%. Conclusion This method is easy, acc urate, effective and sensitive, and it is suitable for qualitative and quantitative detection of 3-hydrox yprop yl-nortadalafilillegally added into food and health products.