HPLC-MS/MS法同时测定保健食品中11种壮阳类非法添加

Determination of 11 Aphrodisiac Drug Illegally Added in Health Food by HPLC-MS/MS Simultaneously

对同时测定保健食品中11种壮阳类药物的高效液相色谱-串联质谱法进行优化,将仪器的检出限优化至0.01 mg/kg。针对保健食品样品的前处理、色谱条件和质谱条件进行优化,采用高效液相色谱-三重四级杆串联质谱(HPLC-MS/MS)法测定保健食品中11种壮阳类药物的含量。样品直接采用乙腈提取,正离子模式下,以0.1%甲酸水-0.1%甲酸乙腈为流动相进行梯度洗脱,以多反应监测模式(MRM)记录11种那非的离子碎片响应进行定性定量分析。结果表明,采用优化后的提取方法,色谱条件及质谱条件,11种那非的线性关系良好,线性范围为1.0~200.0ng/m L,线性相关系数R为0.9991~0.9998,样品添加回收试验的回收率范围为62.5%~120.7%,相对标准偏差范围为4.2%~9.5%(n=10)。该法简单、可靠、重现性好、灵敏度高,适用于保健品基质样品中11种壮阳类药物的同时检测。

Optimize the method for the simultaneous determination of 11 aphrodisiac drug illegally added in health food by HPLC-MS/MS.A method of high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)for the simultaneous detection of 11 aphrodisiac compounds illegally added in health food was described.The samples were extracted with acetonitrile.The samples were analyzed by MRM method in positive mode.Acetonitrile-water added with formic acid was used as mobile phase and ion fragment response was used to quantitative analysis.The results showed that the linear range was from 1.0 ng/mL to 200.0 ng/mL,while the range of the linear correlation was between 0.9991 and 0.9998.The range of recovery for 11 aphrodisiac compound was from 62.5%to 120.7%,and the value of RSD was range from 4.2%to 9.5%.The optimized method was sample,reliable,reproducible and with high sensitivity.The method would be suitable for the simultaneous detection of the 11 aphrodisiac compounds in health food.