高效液相色谱-串联质谱法同时测定烟用香精香料中16种邻苯二甲酸酯类化合物

Simultaneous Determination of Sixteen Phthalate Acid Esters in Tobacco Flavor by High Performance Liquid Chromatography-Electrospray Ionization Tandem Mass Spectrometry

采用液相色谱-串联质谱（LC—MS／MS）联用技术建立了烟用香精香料中16种邻苯二甲酸酯类化合物的测定方法。样品经超声萃取、离心后，用DionexACCLAIMC18色谱柱（150×3mm，3μm）分离，以水溶液一甲醇溶液为流动相，采用梯度洗脱方式，以电喷雾离子源正离子多反应监测模式进行分析检测。方法的定量限（S／N-10）为0．28～37．5ng／mL，线性范围为50～1000ng／mL，样品加标回收率在78．9％～119．3％范围，相对标准偏差（RSD）为2．5％～16．6％。方法成功应用于烟用香精香料中邻苯二甲酸酯类化合物的检测。

A high pertormance liquid chromatography-electrospray ionization tandem mass spectrometry （LC-ESI-MS/MS） method was developed for the determination of phthalate acid esters in tobacco flavor. After ultrasound extraction and centrifugation, the sample was injected into the LC-MS/MS. The analysis was performed on a Dionex ACCLAIM C18 column（150 X 3 ram, 3 /lm）using a gradient elution with the mobile phases of 0.1% water and methanol, and determined by tandem mass spectrometry in positive ESI mode under multiple reaction monitoring mode. The limits of quantification（S/N= 10） were O. 28-37.5 ng/mL,with a linear calibration range spanning 50-1 000 ng/mL. The recoveries ranged from 78.9% to 119.3% at three spiked levels,and the relative standard deviations（RSDs） ranged from 2.5 to 16.6%. The method has been applied to the determination of phthalate acid esters in tobacco flavor.