UPLC-MS/MS法同时测定性保健食品中6种PDE5型非法添加物的含量

Simultaneous Determination of Six llegally Added PDE5 Inhibitors in Sexual Health Foods by UPLC-MS/MS

目的采用超高效液相色谱-串联质谱(UPLC-MS/MS),建立性保健食品中非法添加的6种磷酸二酯酶5(PDE5)型化合物的含量测定方法。方法采用Waters ACQUITY UPLC BEH C18色谱柱,流动相为0.02 mol/L乙酸铵溶液(含0.1%乙酸)-甲醇,梯度洗脱,流速为0.25 ml/min,柱温35℃,进样量10μl;MS条件:电喷雾离子源(ESI),正离子模式,离子源电压5500 V,雾化器压力(GS1)、辅助气压力(GS2)分别为45,55 psi,离子源温度500℃,多反应监测模式(MRM)扫描。结果6种非法添加化合物的峰面积与质量浓度均呈良好的线性关系,相关系数均大于0.997,检出浓度0.108~0.906 ng/ml,精密度、稳定性、重复性试验的相对标准偏差(RSD)分别≤4.33%,3.43%,4.25%,平均回收率为90.57%~113.92%,RSD为1.81%~4.92%。结论本方法简便、灵敏、准确,专属性强,适用于性保健食品中6种PDE5型非法添加物的定量检测。

Objective To establish a simultaneous determination method for six illegally added PDE5 inhibitors in sexual health foods by UPLC-MS/MS.Methods The separation was performed on a Waters ACQUITY UPLC BEH C18 column with mobile phase consisted of 0.02 mol/L ammonium acetate water solution(containing 0.1%acetic acid)-mathanol at the flow rate of 0.25 ml/min.The column temperature was set at 35℃,and the injection volumn was 10μl.The MS conditions were set as:electrospray ion source(ESI),positive ion mode,ion source voltage of 5500 V,nebulizer pressure(GS1)of 45 psi and aux gas pressure(GS2)of 55 psi,and ion source temperature of 500℃.The multiple reaction monitoring(MRM)was used.Results The standard curves were obtained with good correlation coefficients(R>0.997)in ranges of 0.108-0.906 ng/ml.RSDs for precision,stability,repeatability tests were not more than 4.33%,3.43%,4.25%,respectively.The recoveries were in the range of 90.57%-113.92%,with RSDs of 1.81%-4.92%.Conclusion The method is simple,sensitive,accurate and specific.It is suitable for the content determination of six illegally added PDE5 inhibitors in sexual health foods.