液相色谱-离子肼质谱联用法快速检测补肾壮阳类保健食品中非法添加的11种化学物质

Rapid detection of illegal added chemicals in kidney strong health products with HPLC-MS

目的建立液相色谱-离子肼质谱联用法检测补肾壮阳类保健食品中11种化学物质。方法样品经甲醇提取,采用液相色谱-电喷雾离子肼质谱联用法测定。色谱条件:Agilent Eclipse Plus C18色谱柱(100 mm×4.6 mm,3.5μm);梯度洗脱:流动相A为含0.1%乙酸的0.02 mol/L乙酸铵溶液,流动相B为乙腈;质谱条件:扫描方式:正离子扫描;雾化气压:240 k Pa;去溶剂气温度:350℃;去溶剂气流量:10 L/min;离子扫描范围:50 m/z^1 000 m/z;通过与对照品质谱图的对比,对样品中非法添加的化学药物进行定性鉴别。结果方法的检出限为2.5μg/ml^7.9μg/ml,最低检出浓度为50μg/g^158μg/g;在20批样品中,检测到有18批样品中含有西地那非。结论该方法简便、快捷,准确性、灵敏度均可满足定性检查的要求。

Objective To establish HPLC-MS method to detect 11 kinds of chemicals in kidney strong health products.Methods Samples were extracted by methanol,and detected using HPLC-MS. The chromatographic conditions were as the following,Agilent Eclipse Plus C18（ 100 mm × 4. 6 mm,3. 5 μm） column; the gradient elution conditions were that the mobile phase A was 0. 02 mol / L ammonium acetate solution containing 0. 1% acetic acid,and mobile phase B was acetonitrile; mass spectrometry conditions were that scanning mode was positive ion scanning; atomizing air pressure： 240 k Pa to solvent temperature： 350 ℃,solvent gas flow： 10 L / min; ion scanning range was among 50 m / z-1 000 m / z; compared with control quality spectra,illegal added chemical samples were determined and identified. Results Out of 20 batches of samples,18 samples contained sildenafil with the detection limit of the method of 2. 5 μg / ml-7. 9 μg / ml,and the minimum detectable concentration of 50 μg / g-158 μg / g. Conclution The method is simple,rapid,accuracy and sensitivity,and can meet the requirements of qualitative check.