二维液质联用技术测定饮料中21种邻苯二甲酸酯

Rapid Determination of 21 Phthalate Esters in Beverage by Twodimensional Chromatography-mass Spectrometry

建立二维色谱-质谱联用技术(2D-LC-MS/MS)快速检测饮料中21种邻苯二甲酸酯类塑化剂的方法。饮料试样经乙腈-叔丁基甲醚(9︰1)提取后,直接进二维液相色谱-质谱联用仪分析。通过二维液相的第一维在线净化富集、第二维分离分析功能实现对21种邻苯二甲酸酯类塑化剂在线全自动的定性、定量分析。结果表明,21种邻苯二甲酸酯类塑化剂在8~1000 ng/mL范围内线性关系良好,相关系数R2均大于0.994,方法检出限范围为20~50μg/kg,在50~1000μg/kg加标水平下的回收率为85%~106%,相对标准偏差rSD(n=6)均小于10%。该方法操作简单、灵敏度高、分析时间短,适用于饮料中多种塑化剂的快速检测分析,可为国家相关标准制定提供参考依据。

Establish a two-dimensional liquid chromatography-mass spectrometry(2 D-LC-MS/MS)method for 21 phthalate esters in beverage.The beverage sample was extracted by acetonitrile-tert-butyl methyl ether(9︰1),then directly analyzed by two-dimensional liquid chromatography and mass spectrometry to realize the online automatic qualitative and quantitative analysis of 21 phthalate esters.Sample was purified and enriched through the first dimension of two-dimensional liquid phase,separated and analyzed through the second dimension.The results showed that the calibrations of 21 phthalate ester plasticizers were linear in the wide range of 8-1000 ng/mL with the correlation coefficients R2≥0.994.The limits of detection(LODs)were 20-50μg/kg.The average recoveries of the 21 phthalate esters in the range of 50-1000μg/kg were ranged from 85%to 106%.RSDs(Relative standard deviation)were less than 10%.This method was easy operated,highly sensitive and timeless,and could be used for the rapid detection and analysis of various plasticizers in beverages,to provide references for establishing relevant national standards.