液相色谱-串联质谱法快速筛查减肥类中药及保健品中非法添加30种化学药

建立了中药及保健品中30种减肥类化学药的高效液相色谱-串联质谱(LC-MS/MS)快速筛查方法。实验优化了前处理方法、色谱分离条件和质谱参数。样品采用甲醇超声萃取,Agilent poroshell 120 ECC18(4.6 mm×100 mm,2.7μm)色谱柱分离,流动相为乙腈-水溶液(含10 mmol/L甲酸铵,0.1%甲酸,10%甲醇),梯度洗脱,流速0.25 m L/min,采用正负离子切换模式的电喷雾质谱检测,多反应选择离子监测(MRM)。该方法能同时筛查30种化学药,覆盖面广,简便、快速、准确可靠,已用于减肥类中药及保健品中非法添加化学药的筛查及检测。

Simultaneous Determination of Thirty Chemical Drugs Illegally Added in Anti-obesity Traditional Chinese Medicine and Health Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry

A high-performance liquid chromatograph-mass spectrometric (LC-MS/MS) method was proposed for the determination of thirty chemical compositions,which were illegally mixed into the antiobesity traditional Chinese medicine and health products.The conditions of extraction and mass parameters were optimized.The drugs were extracted with methonal in ultrasonic condition,separated on a C18 chromatographic column using a mixture of acetonitrile and water(containing 10 mmol/L ammonium formate,0.1％ formic acid,10％ methanol) as mobile phase.The detection of analytes was performed by positive-ion and negative-ion electrospray ionization mass spectrometry(ESI -MS) under multiple reaction monitoring(MRM) mode.The method was proved to be able of covering large area,simple,rapid,accurate and reliable.It was used in screening and examination of illegally added chemicals in Chinese traditional medicine and health food.