超高效液相色谱-串联质谱法同时测定食品中4种减肥类非法添加药物

Simultaneous determination of 4 compounds illegally added in foods and losing weight health foods by HPLC-MS/MS

建立了固相萃取-超高效液相色谱-串联质谱法同时测定食品中双醋酚汀、比沙可啶、酚酞和脱乙酰比沙可啶4种非法添加化学药物的分析方法。样品用乙腈超声提取后,采用C 18固相萃柱净化,经Waters ACQUITYUPLC BEH C18色谱柱(50 mm×2.1 mm,1.7μm)分离,以乙腈和20 mmol/L甲酸铵溶液为流动相进行梯度洗脱,采用电喷雾-正离子多反应监测模式,外标法定量。结果表明,在1.0~500.0 ng/mL的质量浓度范围内,4种化学药物的线性相关系数均大于0.99,方法的检出限在0.05~0.1μg/kg之间。在不同类型基质中进行3个水平添加实验(n=6),4种化学药物的回收率为79.2%~111.8%,相对标准偏差为0.21%~13.3%。本方法简单快速、准确度好、精密度高,适合于食品和减肥类保健食品中4种非法添加化学药物的同时检测。

After ultrasonic extraction with acetonitrile,the samples were purified by C 18 SPE columns.The separation was performed on Waters C 18 column(50 mm×2.1 mm,1.7μm)by gradient elution with acetonitrile and 20 mmol/L ammonium formate solution as the mobile phases.The electrospray ionization mass spectrometry was operated in positive mode using multiple reaction monitoring(MRM).The target compounds,oxyphenisatin diacetate,bisacodyl,phenolphthalein,deacetylbisacodyl,were quantified by external standard method.Under the optimal conditions,the calibration curves of all the analytes were linear in the concentration range of 1.0-500.0 ng/mL,with correlation coefficients greater than 0.99.The limits of quantitation(LOQs)ranged from 0.05μg/kg to 0.1μg/kg.The average recoveries for different matrixes at three spiked levels ranged from 79.2% to 111.8%,with relative standard deviations(RSDs)of 0.21%-13.3%.The method was simple,rapid,accurate and precise.