超高效液相色谱-串联质谱法快速检测塑料制品中22种添加剂

Rapid detection of 22 additives in plastic products by ultra-high performance liquid chromatography-tandem mass spectrometry

建立了超高效液相色谱与三重四级杆串联质谱同时测定塑料制品中22种常见光稳定剂和抗氧化剂的分析方法,采用通用型Waters ACQUITY UPLC BEH C_(18)色谱柱(50 mm×2.1 mm×1.7μm),以甲醇-水(0.1%(w)甲酸)体系为流动相梯度洗脱,优化的前处理条件为:萃取试剂为丙酮,超声萃取时间设置为20 min,萃取试剂体积为2 m L,萃取次数为3次。实验结果表明,22种添加剂在0.05~10 mg/L范围内线性良好,相关系数均大于0.999 0,检出限均在0.01~0.05 mg/L之间,定量限均为0.05 mg/L;三个添加水平下22种添加剂加标平均回收率为80.0%~121.3%,RSD(n=6)均小于10%,满足了实际检测分析的需要,操作简便、响应灵敏、快速准确。

An analysis method for simultaneous determination of 22 additives in plastic products by ultra-high performance liquid chromatography and triple quadrupole mass spectrometry（UPLCMS） was established. General-purpose Waters ACQUITY UPLC BEH C（18） column（50 mm×2.1 mm×1.7 μm） was employed,and gradient elution was performed with a mobile phase of methanolwater（0.1%（w）formic acid）. The optimized pretreatment conditions were the extraction reagent being acetone,ultrasonic extraction time being set to 20 min,the volume of the extraction reagent being 2 m L,and the number of extractions being 3. The experimental results showed that the 22 additives exhibited a good linearity in the range of 0.05-10 mg/L with the correlation coefficients thereof being all greater than 0.999 0,the detection limits thereof being all in the range of 0.01-0.05 mg/L and the quantification limits thereof being all 0.05 mg/L. The spiked average recoveries of the 22 additives at three adding levels were between 80.0%-121.3%,and the relative standard deviations（n=6） were all less than 10%. The requirements of actual detection and analysis can be satisfied,and simple operation,sensitive response,fastness and accuracy can be achieved.