详细信息
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
文献类型:期刊文献
中文题名: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
英文题名:Detection of sildenafil illegally added in maca products by liquid chromatography tandem mass spectrometry
作者:李绍辉[1,2];吴寒秋[2];许秀丽[2];章飞芳[1];冯峰[2];张峰[2];梁鑫淼[1,3]
机构:[1]华东理工大学药学院,上海200237;[2]中国检验检疫科学研究院食品安全研究所,北京100176;[3]中国科学院大连化学物理研究所,辽宁大连116023
年份:2016
卷号:37
期号:11
起止页码:310
中文期刊名:食品工业科技
外文期刊名:Science and Technology of Food Industry
收录:CSTPCD;;北大核心:【北大核心2014】;CSCD:【CSCD_E2015_2016】;
基金:国家重大科学仪器设备开发专项项目(2012YQ14000806);质检公益性项目(201310134)
语种:中文
中文关键词:玛咖;西地那非;UPLC-MS/MS
外文关键词:Maca; Sildenafil ;UPLC- MS/MS
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0.2-20μg/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。
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( tO mmol/L ammonium acetate) :water( 10 mmol/L ammonium acetate) (90: 10,v/v)at a flow rate of 0.3 mL/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/z 475.3 〉 282.9 was used as qualifying ion for sildenafiI.The collision energy was 50 and 60 eV, 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.
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