固相萃取-三重串联四极杆气相色谱/质谱联用测定食用油中16种邻苯二甲酸酯类化合物  

Determination of 16 phthalates esters in edible oil by solid phase extraction and gas chromatography coupled with triple quadrupole mass spectrometry

作　　者：李俊玲[1] 王冬梅[1] 王余萍[1] 

机构地区：[1]安阳市疾病预防控制中心,河南安阳455000

出　　处：《中国卫生检验杂志》2014年第6期782-785,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立固相萃取-三重串联四极杆气相色谱/质谱联用(GC-MS/MS)同时测定16种邻苯二甲酸酯类化合物的分析方法。方法样品加乙腈涡旋、超声提取、离心分离后经固相萃取仪净化,采用三重串联四极杆气相色谱/质谱联用在多反应监测模式(MRM)下进行测定。结果在MRM模式下用两对离子对16种邻苯二甲酸酯类进行分析,基线漂移少,且在5 V^40 V能量范围内,对母离子进行了碰撞能量优化;16种邻苯二甲酸酯类线性范围为6.0μg/L^5000μg/L,线性相关系数在0.9900~0.9994之间,检出限为0.01 mg/kg^0.04 mg/kg,定量限为0.03 mg/kg^0.1 mg/kg,平均加标回收率为70.1%~119.8%,相对标准偏差(RSD)均<10%。结论该方法适合食用油中邻苯二甲酸酯类的测定,具有良好的回收率及稳定性。Objective A new analytical method was developed for simultaneous determination of 16 phthalate esters in edible oil by solid phase extraction and gas chromatography coupled with triple quadrupole mass spectrometry （GC/MS/MS）. Meth- ods The samples were treated with acetonitrile by swirl for supersonic extraction, then purified by solid phase extractior follow- ing centrifugal separation. The extract was analyzed by gas chromatography coupled with triple quadrupole mass spectrometry u- sing multiple reaction monitoring（MRM）. Results Analysis of the 16 kinds of phthalate esters in the MRM mode using two pairs of ions showed less baseline drift, and the collision energy of the parent ion was optimized in range of 5 V N 40 V. The lin- ear range of the 16 phthalate esters were between 6.0 μg/L and 5000 μg/L, the linear correlation coefficients were between 0. 9900 N 0. 9994, the limits of detection were from 0.01 mg/kg to 0.04 mg/kg, the limits of quantication were 0.03 mg/kg - 0.1 mg/kg. The average recovery rates were in the range of70.1% -119.8 % and relative standard deviations （RSDs） were less than 10 %. Conclusion The method can be applied to the routine analysis of phthalate esters in edible oil samples, with better recovery and stability.

关 键 词：三重串联四极杆气相色谱 质谱联用 固相萃取 邻苯二甲酸酯 

分 类 号：O657.63[理学—分析化学]