牙膏中4种水杨酸酯同时测定的气相色谱-质谱法

Simultaneous determination of 4 kinds of salicylic acid esters in toothpaste by gas chromatography-mass spectrometry

目的建立了气象色谱-质谱法同时测定牙膏中4种水杨酸酯的方法。方法样品用海砂研磨均匀,乙醇提取,涡旋2 min及超声10 min,5 000 r/min离心10 min,提取液经VF-wax MS色谱柱(30 m×0.32 mm×0.25μm)分离后,进行气相色谱-质谱法测定,外标法定量。结果在优化的实验条件下,水杨酸酯在0.05~10μg/ml的浓度范围内线性关系良好,线性系数均r>0.998 7,方法检出限均为0.02μg/ml,平均回收率在92.0%~97.0%之间,RSD在1.30%~4.34%之间。结论该方法简便、快速,重现性好,适用于牙膏中4种水杨酸酯的同时测定。

[Objective]To establish a gas chromatography-mass spectrometry method for the simultaneous determination of 4 kinds of salicylic acid esters in toothpaste.[Methods] The samples were lapped with sand,extracted with ethanol,then treated by vortex for 2 minutes and ultrasonic for 10 minutes,and centrifuged at 5 000 r/min for 10 minutes.The extraction was separated with VF-wax MS column（30 m×0.32 mm×0.25 m） and determined by gas chromatography-mass spectrometry,and the quantitative analysis was performed by external standard method.[Results] Under the optimized conditions,the calibration curve showed good linearity in the range of 0.05-10 μg/ml of salicylic acid esters,the linear coefficients（r） were higher than 0.998 7.The detection limits of the method were 0.02 μg/ml.The recovery and the relative standard deviation（RSD） were 92.0%-97.0% and 1.30%-4.34%,respectively.[Conclusion] This method is simple and rapid with good repeatability.It is suitable for simultaneous determination of 4 kinds of salicylic acid esters in toothpaste.