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

作　　者：夏金涛 张莉 吴婉琴 朱晓玲 蒋颖 江丰 XIA Jin-Tao;ZHANG Li;WU Wan-Qin;ZHU Xiao-Ling;JIANG Ying;JIANG Feng(Hubei Provincial Institute for Food Supervision and Test,Wuhan 430075,China;Key Laboratory of Detection Technology of Focus Chemical Hazards in Animal-derived Food for State Market Regulation,Wuhan 430075,China;Hubei Shizhen Laboratory,Wuhan 430065,China)

机构地区：[1]湖北省食品质量安全监督检验研究院,武汉430075 [2]国家市场监管重点实验室(动物源性食品中重点化学危害物检测技术),武汉430075 [3]湖北时珍实验室,武汉430065

出　　处：《食品安全质量检测学报》2024年第21期13-21,共9页Journal of Food Safety and Quality

基　　金：国家市场监督管理总局科技计划项目(2022MK085);国家重点研发计划项目(2023YFF1104700);国家市场监督管理总局创新人才计划(青年拔尖人才)项目(QNBJ202330)。

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。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 quantification 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.

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 

分 类 号：O657.63[理学—分析化学] TS218[理学—化学]