超高效液相色谱串联质谱法检测玛咖产品中非法添加西地那非
Detection of sildenafil illegally added in maca products by liquid chromatography tandem mass spectrometry
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摘要: 建立了检测玛咖中西地那非的超高效液相色谱-串联质谱(UPLC-MS/MS)法。色谱条件为Agilent SB-C18柱;柱温25℃;流动相为甲醇(10 mmol/L乙酸铵):水(10 mmol/L乙酸铵,m/V)(90∶10,v/v)等度洗脱;流速:0.3 m L/min;进样量:5μL。质谱条件为正离子模式(ESI+),多反应监测模式(MRM);三重四级杆质量分析器;分子离子峰M+H+m/z 475.3,子离子为m/z 282.9,碰撞能50 e V;m/z 58.1碰撞能为60 e V。西地那非在0.220μg/L范围内线性关系良好,相关系数R2为0.9994。建立的方法准确可靠、灵敏度高,可应用于玛咖产品中西地那非的含量测定。Abstract: The purpose was to establish a method for determination of sildenafil in Maca products by UPLC-MS /MS.The samples were separated on Agilent SB-C18 column( 1.8 μm,2.1 mm × 50 mm) and eluted using mobile phase of methanol( 10 mmol/L ammonium acetate) : water( 10 mmol/L ammonium acetate)( 90 ∶ 10,v/v) at a flow rate of 0.3 m L/min,the injection volume was 5 μL.MS condition was positive ion mode,collecting multiple reaction monitoring( MRM) mode.Precursors to product ion transitions of m/z 475.3 > 58.1 was to quantify sildenafil,and m/z475.3 > 282.9 was used as qualifying ion for sildenafil. The collision energy was 50 and 60 e V,respectively. The method was linear in the concerntration range of 0.2 ~ 20 μg/L,and the correlation coefficient was 0.9994. The method was accurate,reliable and highly sensitive,and hence it can be applied in the determination of sildenafil in Maca products.