保健食品中O-丙基羟基伐地那非的快速筛查、确证和定量测定

Rapid screening, identification and quantitative determination of O-propyl hydroxyvardenafil in dietary supplement

中文关键词:  快速筛查  结构确证  定量测定  非法添加物  O-丙基羟基伐地那非

英文关键词:rapid screening  structural identification  quantitative determination  illegal additives  O-propyl hydroxyvardenafil

中文摘要:

      目的 利用高分辨质谱仪快速筛查壮阳类保健食品中的磷酸二酯酶5型抑制剂(phosphodiesterase type 5 inhibitors, PDE-5i), 确证其中发现的新型非法添加物并建立定量检测方法。方法 采用超高效液相色谱-四级杆-飞行时间质谱仪(ultra performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry, UPLC-Q-TOF/MS)对20批次保健食品中的非法添加物进行日常非靶向筛查, 在2批次压片糖果中鉴别出一种新型伐地那非类似物。结合化合物的质谱裂解规律及核磁共振波谱(nuclear magnetic resonance spectrometry, NMR)对未知物结构进行确证。采用超高效液相色谱-三重四级杆质谱法(ultra performance liquid chromatography-coupled triple quadrupole mass spectrometry, UPLC-MS/MS)建立了典型食品基质中未知物的定量检测方法。结果 未知物被确证为O-丙基羟基伐地那非。该物质溶剂校准和基质匹配曲线在2~100 ng/mL质量浓度范围内线性关系良好, 相关系数(r2)大于0.995, 检出限为0.05 mg/kg, 定量限为0.10 mg/kg。在固体饮料、压片糖果、果冻基质中3个水平加标回收率为94.45%~104.16%, 相对标准偏差(relative standard deviation, RSD)为0.70%~4.02%。采用该方法测得2批次阳性样品中O-丙基羟基伐地那非的含量分别为22.0 mg/kg、13.8 g/kg。结论 本方法适用于食品中那非类似物的快速筛查, 用于O-丙基羟基伐地那非的定量检测高效、灵敏、准确。本研究为食品基质中非法添加物的系统性确证和定量研究提供了可供借鉴的参考模型。

英文摘要:

      Objective To rapid screen phosphodiesterase type 5 inhibitor (PDE-5i) in aphrodisiac dietary supplement with high-resolution mass spectrometer, identify the novel illegal additives found in those food matrices, and establish a quantitative detection method. Methods A new vardenafil analog was identified in 2 batches of pressed candies during routine non-targeted screening illegal additives in 20 batches of dietary supplement by ultra performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry (UPLC-Q-TOF/MS). The structure of the unknown compound was identified by the combination of the fragmentation law of mass spectrum and nuclear magnetic resonance spectrum (NMR). A quantitative method for the determination of unknown compound in typical food matrices was developed by ultra performance liquid chromatography-coupled triple quadrupole mass spectrometry (UPLC-MS/MS). Results The unknown compound was identified as O-propyl hydroxyvardenafil. Sufficient linearity (range 2–100 ng/mL) in matrix matched and solvent calibrations were obtained with correlation coefficient (r2)>0.995. The limits of detection and quanti?cation for the compounds were 0.05 mg/kg and 0.10 mg/kg, respectively. In solid beverages, pressed candies and jellies, recoveries of this compound were ranged from 94.45 to 104.16% with relative standard deviation (RSD) of 0.70%–4.02% in 3 different spiking levels. The content of O-propyl hydroxyvardenafil in 2 batches of positive real samples was 22 mg/kg and 13.8 g/kg, respectively. Conclusion This method is suitable for the rapid screening of nafil analogs in food matrices and its application to the quantitative determination of O-propyl hydroxyvardenafil is highly effective, sensitive and accurate. This study provides a reference model for the systematic identification and quantitative study of illegal additives in food matrices.