食品科学

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高效液相色谱-串联质谱检测保健酒中非法添加物艾地那非

张丽媛,颜琳琦,周明昊,吴鸳鸯   

  1. 浙江省食品药品检验研究院,浙江 杭州 310000
  • 出版日期:2016-07-25 发布日期:2016-07-26

Determination of Aildenafil Illegally Added in Health Wine by High Performance Liquid Chromatography-Tandem Mass Spectrometry

ZHANG Liyuan, YAN Linqi, ZHOU Minghao, WU Yuanyang   

  1. Zhejiang Institute for Food and Drug Control, Hangzhou 310000, China
  • Online:2016-07-25 Published:2016-07-26

摘要:

目的:采用高效液相色谱-串联质谱(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)法,建立保健酒中非法添加物艾地那非的检测方法。方法:使用Agilent RRDH Eclipse-plus C18色谱柱(2.1 mm×100 mm,1.8 μm),以0.1%甲酸-乙腈溶液为流动相A、0.1%乙酸-20 mmol/L乙酸铵溶液为流动相B进行梯度洗脱。通过HPLC-MS/MS系统中全扫描模式对艾地那非进行定性分析,多反应监测模式对艾地那非进行定量分析。结果:该方法线性r2大于0.99,精密度相对标准偏差小于3%,不同质量浓度样品平均回收率为97.31%~100.66%,检出限为0.6 ng/mL,定量限为1.6 ng/mL。结论:此方法测定准确、灵敏度高、分离度高,可用于保健酒中非法添加物艾地那非的筛选和检测。

关键词: 艾地那非, 高效液相色谱-串联质谱法, 保健酒, 检测方法, 非法添加

Abstract:

Objective: To develop a detection method for aildenafil adulterated in health wine using high performance liquid
chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods: The chromatography was performed using an
Agilent RRDH Eclipse plus C18 column (2.1 mm × 100 mm, 1.8 μm), with a mobile phase consisting of acetonitrile-0.1%
formic acid (phase A) and 0.1% acetic acid -20 mmol/L ammonium acetate (phase B) by gradient elution. Qualitative
analysis of aildenafil was conducted under full-scan model, and quantitative analysis in the multiple reaction monitoring
(MRM) model. Results: The method was linear with a correlation coefficient (r2) > 0.99, and its precision, expressed as
RSD, was < 3%. The recoveries of aildenafil at different spiked concentrations ranged from 97.31% to 100.66%. The limit
of detection (LOD) was 0.6 ng/mL and the limit of quantitation (LOQ) was 1.6 ng/mL. Conclusion: This method is fast and
accurate with a high sensitivity and a high degree of separation. It can be used for the screening and detection of aildenafil
illegally added in health wine.

Key words: aildenafil, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), health wine, detection method, illegally added

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