食品中一种新型非法添加物O-丙基伐地那非的快速筛查和定量测定

Rapid screening and quantitative determination of a new illegally added compound O-propyl vardenafil in foods

中文关键词:  超高效液相色谱-四级杆-静电场轨道阱质谱  超高效液相色谱-三重四极杆质谱  非法添加  O-丙基伐地那非  伐地那非衍生物

英文关键词:ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry  ultra performance liquid chromatography-coupled triple quadrupole mass spectrometry  illegal addition  O-propyl vardenafil  vardenafil analogue

中文摘要:

      目的 对在食品中发现的一种非法添加的新型磷酸二酯酶5型(phosphodiesterase type 5, PDE-5)抑制剂O-丙基伐地那非进行结构解析并建立定量测定方法。方法 采用高效液相色谱-二极管阵列检测器法(high performance liquid chromatography-diode array detector, HPLC-DAD)发现了一种未知的新型伐地那非类似物, 采用超高效液相色谱-四极杆-静电场轨道阱高分辨质谱法(ultra performance liquid chromatography- quadrupole/electrostatic field orbitrap high resolution mass spectrometry, UPLC-Q-Orbitrap HRMS)对其结构进行质谱解析, 并依据解析的化学结构购买对照品, 确定该物质为O-丙基伐地那非。采用超高效液相色谱-三重四极杆质谱法(ultra performance liquid chromatography-coupled triple quadrupole mass spectrometry, UPLC-MS/MS)建立典型食品中O-丙基伐地那非的定量测定方法。结果 O-丙基伐地那非在0.50~50.25 ng/mL质量浓度范围内线性关系良好, 相关系数(r)为0.9998, 方法检出限(S/N=3)为0.02 mg/kg, 方法的定量限(S/N=10)为0.05 mg/kg, 在咖啡、压片糖果、保健酒基质中3个水平加样回收率分别为91.8%~93.9%、84.9%~87.3%和95.6%~103.0%, 相对标准偏差均不大于4.6%。采用该方法对市场监管部门送检的93批样品进行测定, 结果其中17批检出O-丙基伐地那非, 其含量为28~359 mg/kg。结论 所建立的方法快速、灵敏、准确, 可用于O-丙基伐地那非的筛查和定量。本研究思路可给其他非法添加未知物的鉴定提供参考。

英文摘要:

      Objective To study the structure of O-propyl vardenafil, a new illegally added phosphodiesterase type 5 (PDE-5) inhibitor found in food, and establish a quantitative determination method. Methods An unknown analogue of vardenafil was found by high performance liquid chromatography-diode array detector (HPLC-DAD). The structure was analyzed by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry (UPLC-Q-Orbitrap HRMS). According to the analytical structure, the reference substance was purchased and the substance was identified as O-propyl vardenafil. The quantitative determination method of O-propyl vardenafil in typical food was established by ultra performance liquid chromatography coupled triple quadrupole mass spectrometry (UPLC-MS/MS). Results O-propyl vardenafil showed good linearity in the mass concentration range of 0.50?50.25 ng/mL, and the correlation coefficient (r) was 0.9998. The limit of detection (S/N=3) was 0.02 mg/kg, and the limit of quantitation (S/N=10) was 0.05 mg/kg. In coffee, pressed candy and healthcare liquor, the recoveries at 3 levels were 91.8%?93.9%、84.9%?87.3%和95.6%?103.0%, 92.5%, 86.3% and 98.6%, respectively, the relative standard deviation was less than 4.6%. The method was used to determine 93 batches of samples sent by the market regulatory department. The results showed that O-propyl vardenafil were detected in 17 batches, and the content were from 28 to 359 mg/kg. Conclusion The established method is fast, sensitive and accurate, and can be used for the screening and quantification of O-propyl vardenafil. The research ideas can provide reference for the identification of other illegally added compounds in foods.