食品中新型那非衍生物丙氧苯基羟基伐地那非的筛查和定量测定

Screening and quantitative determination of novel nafil derivative propoxyphenyl hydroxyvardenafil in foods

中文关键词:  非法添加  丙氧苯基羟基伐地那非  高效液相色谱-串联三重四极杆质谱法  超高效液相色谱-四极杆-静电场轨道阱质谱法  伐地那非结构类似物

英文关键词:illegal addition  propoxyphenyl hydroxyvardenafil  high performance liquid chromatography- tandem triple quadrupole mass spectrometry  ultra performance liquid chromatography-quadrupole-exactive orbitrap-high resolution mass spectrometry  vardenafil structural analogues

中文摘要:

      目的 对在食品中发现的一种新型伐地那非衍生物进行筛查, 并建立定量测定方法。方法 采用超高效液相色谱-四极杆-静电场轨道阱高分辨质谱法在食品中发现一种与伐地那非结构类似的化合物。通过高分辨质谱碎片离子推测该伐地那非结构类似物的分子结构及裂解规律, 与定制合成的对照品比较, 确定物质名称。采用高效液相色谱-串联三重四极杆质谱法的多反应监测模式进行扫描, 外标法定量测定。结果 在食品中筛查出新型那非衍生物丙氧苯基羟基伐地那非, 丙氧苯基羟基伐地那非在2~50 ng/mL质量浓度范围内线性关系良好, 检出限为0.03 mg/kg, 定量限为0.10 mg/kg, 在咖啡、压片糖果、果冻及植物饮料基质中3个加标水平下的平均回收率为87.6%~102.6%, 相对标准偏差(relative standard deviation, RSD)为0.5%~6.3%, 方法重现性和稳定性良好, RSD<5%。采用该方法对实际样品进行测定, 发现34个阳性样品, 含量范围为1.60×103~2.62×104 mg/kg。结论 该方法具有快速、准确、灵敏度高等优点, 可用于食品中那非衍生物丙氧苯基羟基伐地那非的筛查和定量测定, 为打击非法添加伐地那非衍生物的监管提供技术支持。

英文摘要:

      Objective To study and screen the novel vardenafil derivative in food, and establish a quantitative method. Methods A compound with similar structure to vardenafil was detected in food by ultra performance liquid chromatography-quadrupole-exactive orbitrap-high resolution mass spectrometry. The molecular structure and fragmentation law of the vardenafil structure analogue were inferred from the fragment ions of high-resolution mass spectrometry. The compound name was clarity compared with the custom-synthesized reference substance. Quantitative analysis was carried out in a multiple reaction monitoring by high performance liquid chromatography-tandem triple quadrupole mass spectrometry with the external standard method. Results The novel vardenafil derivative in food was identified as propoxyphenyl hydroxy-vardenafil. The results showed that good linearity was observed for propoxyphenyl hydroxyvardenafil within the concentration range of 2–50 ng/mL. The limit of detection was 0.03 mg/kg, and the limit of quantitation was 0.10 mg/kg. The average recoveries and relative standard deviations (RSD) of coffee, confectionery, jelly and plant-based drinks were 87.6%–102.6% and 0.5%–6.3% respectively. The reproducibility and stability of the method were good (RSD<5%). The method was applied to measure the real samples, and 34 batches of positive samples were found with the content range of 1.60×103–2.62×104 mg/kg. Conclusion This method is fast, accurate and high sensitivity, can be used for screening and quantitative determination of the derivative propoxyphenyl hydroxyvardenafil in food, and can provide technical support for the supervision of the illegal addition of vardenafil derivatives.