抗疲劳保健品中非法添加那非类物质液质筛查方法建立

Research a Liquid Mass Screening Method of the Illegally Added PDE-5 in Health Food

建立那红地那非、伪伐地那非、那莫西地那非、红地那非、西地那非、豪莫西地那非、爱地那非、硫代爱地那非、羟基豪莫西地那非等9种那非类化合物的液相色谱-四级杆飞行时间高分辨质谱联用仪快速筛查和确证检验方法。对照品及样品经过甲醇超声提取,以C_(18)色谱柱(3.0×100 mm,1.8μm)分离,流动相A为0.1%甲酸-5 mmol·mL^(-1)乙酸铵,流动相B为乙腈,梯度洗脱;确定了这9种物质的精确分子质量数,建立多级质谱碎片离子数据库。运用建立的方法对22种保健品进行检测,采用精确质量数匹配和自建多级质谱碎片离子数据库进行检索,实现快速筛查;确定这22种保健品中的非法添加情况。

We established a method for the illegally added Sildenafil,Hongdenafil,Pseudovardenafil of health food by quadrupole time of flight tandem mass spectrometry. We Built an exact molecular mass number and multistage mass spectrometry fragment ions’ data base.The samples were extracted by methanol,and separated setting gradient elution method by C18 column(3.0×100 mm,1.8 μm),with 5 mmol ammonium acetate(0.1% formic acid)-acetonitrile as the mobile phase. Matching by exact molecular mass number and searching by multistage mass spectrometry fragment ion’s data base,we set up a method for Rapid Detecting PDE-5. We corroborated the samples by retention time,isotopic abundance and multistage characteristic fragment ions.We found 20 kinds of health food which has Sildenafil. This method is simple,fast,accurate,high sensitivity which can be used to qualitatively screen the illegally added PDE-5 of health food,to provide the basis for the science of the court.