液相色谱-串联质谱法测定抗疲劳类保健食品中非法添加的西地那非含量的不确定度评定

Uncertainty evaluation for the determination of sildenafil illegally added in anti-fatigue health food by liquid chromatography-tandem mass spectrometry

目的对液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)测定抗疲劳类保健食品中非法添加的西地那非含量的不确定度进行评定。方法根据JJF1059.1—2012《测量不确定度评定与表示》、JJF 1135—2005《化学分析测量不确定度评定》,采用液相色谱-串联质谱法测定抗疲劳类保健食品中西地那非残留量,对测定方法中的关键环节进行分析,对各不确定度分量进行识别和量化,计算出合成不确定度和扩展不确定度。结果当西地那非含量为0.927μg/g, k=2(置信水平95%)时,扩展不确定度为0.06μg/g,测试结果表示为(0.927±0.06)μg/g。结论本方法为液相色谱-串联质谱法测定抗疲劳类保健食品中非法添加的西地那非含量的不确定度提供了参考依据。

Objective To evaluate the uncertainty for the determination of sildenafil illegally added in anti-fatigue health food by liquid chromatography-tandem mass spectrometry(LC-MS/MS). Methods According to JJF 1059.1—2012 Measurement uncertainty evaluation and presentation and JJF 1135—2005 Evaluation of measurement uncertainty in chemical analysis, the sildenafil residues in anti-fatigue health food was measured by liquid chromatography-tandem mass spectrometry. Through the analysis of key links in the determination method, each component of uncertainty was identified and quantified, then, the combined uncertainty and expanded uncertainty were calculated. Results The sildenafil content was 0.927 μg/g, k=2(confidence level was 95%), and the expanded uncertainty was 0.06 μg/g. The assay result of the sample was(0.927±0.06) μg/g. Conclusion The established method provides important reference for the uncertainty evaluation of determination of sildenafil illegally added in dietary supplement of aphrodisiacs by LC-MS/MS.