超高效液相色谱-串联质谱法测定食品中顺式四氢咔啉和环己基去甲他达拉非

Determination of tetrahydro-β-carboline and N-cyclohexyl nortadalafil in food with ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  环己基去甲他达拉非  顺式四氢咔啉  非法添加  超高效液相色谱-串联质谱法

英文关键词:N-cyclohexyl nortadalafil  tetrahydro-β-carboline  illegally added  ultra performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定食品中非法添加2种新型他达拉非非法添加物含量的分析方法。方法 样品以甲醇为溶剂超声提取, 经Atlantis? T3色谱柱(150 mm×2.1 mm, 3 μm)分离, 以0.1% (V:V)甲酸水溶液-甲醇作为流动相, 进行梯度洗脱。在电喷雾正离子模式下, 采用多反应监测(multiple reaction monitoring, MRM)模式, 基质匹配曲线外标法定量。结果 顺式四氢咔啉、环己基去甲他达拉非在1~50 ng/mL范围内与峰面积均成良好的线性关系, 相关系数r均在0.999以上。顺式四氢咔啉检和环己基去甲他达拉非的检出限均小于3 μg/kg, 定量限均小于10 μg/kg, 在饼干等4种基质中1、2、10 ng/mL 3个水平下加标回收率为66.1%~117.4%, 相对标准偏差均未超过10% (n=6)。结论 该方法准确、可靠, 可满足食品中顺式四氢咔啉、环己基去甲他达拉非的定量分析。

英文摘要:

      Objective To establish a method for the determination of 2 kinds of new illegal tadalafil additives in food by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The compound was extracted by methanol ultrasonic wave method. The extract was separated on an Atlantis? T3 column (150 mm×2.1 mm, 3 μm). After separation, gradient elution was carried out with 0.1% (V:V) formic acid aqueous solution methanol as the mobile phase and the samples were determined with electrospray ionization source under positive ion mode and multiple reaction monitoring (MRM) mode. External standard of the blank matrix-matched calibration curves was used for quantification. Results Tetrahydro-β-carboline and N-cyclohexyl nortadalafil had good linearity with the peak area in the range of 1?50 ng/mL, with the correlative coefficients over 0.999. The limits of detection of tetrahydro-β-carboline and N-cyclohexyl nortadalafil were all less than 3 μg/kg, and the limits of quantitation were all less than 10 μg/kg. In 4 kinds of substrates such as cookies, the recoveries were 66.1%-117.4% at the spiked levels of 1, 2, 10 ng/mL, with the relative standard deviations lower than 10% (n=6). Conclusion This method is accurate and reliable, which is suitable for the determination of tetrahydro-β-carboline and N-cyclohexyl nortadalafil illegally added into food.