保健食品中13种那非类物质快速检测及确证

Rapid Detection and Confirmation of 13 Kinds of Nafil Drug in Health Food

建立一种高效液相色谱同时测定保健食品中13种那非类非法添加物质的定性及定量分析方法,采用超高液相色谱串联质谱对阳性样品进行快速确证。样品中的那非物质经乙腈提取后,采用Waters Symmetry Shield C18(250 mm×4.6 mm,5μm)色谱柱,以乙腈-20 mmol/L乙酸铵水溶液(含0.1%乙酸)进行梯度洗脱,液相色谱紫外检测器进行检测,超高液相色谱串联质谱进行确证。结果表明,13种那非类物质在50 min内有良好的分离度,在0.3~50μg/mL范围内线性关系良好,相关系数(R2)≥0.998,检出限(LOD)为28.52~39.71 mg/kg,定量限(LOQ)为62.60~143.50 mg/kg,低(1倍定量限)、中(5倍定量限)、高(10倍定量限)3个水平的平均回收率为92.64%~109.17%。该方法简便、快捷、准确度高,适合保健食品中非法添加物质的快速检测和准确定量。

A qualitative and quantitative analysis method for simultaneous determination of 13 kinds of nafil drug illegally added substances in health products by high performance liquid chromatography was established,and the positive samples were identified by ultra-high performance liquid chromatography-tandem mass spectrometry.The sample was extracted by acetonitrile,then gradient elution was carried out on Waters Symmetry Shield C18(250 mm×4.6 mm,5μm)column with acetonitrile-20 mmol/L ammonium acetate aqueous solution(containing 0.1%acetic acid).The nafil drug was detected by liquid chromatography ultraviolet detector and confirmed by ultra-high performance liquid chromatography tandem mass spectrometry.The results showed that the 13 kinds of nafil drug were well separated within 50 min,and had a good linear relationship in the range of 0.3-50μg/mL.The correlation coefficient(R2)was more than 0.998;The detection limit(LOD)was between 28.52 and 39.71μg/g;The quantitative limit(LOQ)was between 62.60 and 143.50 mg/kg;The average recovery of low,medium and high levels ranged from 92.64%to 109.17%.The method was simple,fast,accurate and suitable for rapid detection and accurate quantification of illegally added substances in health food.