摘要
利用气相色谱-四极杆-飞行时间质谱(GC-QTOF MS)技术建立了油脂食品中23种邻苯二甲酸酯类快速检测方法。样品采用乙腈-甲基叔丁基醚(9∶1,v/v)提取,PSA分散剂净化,经GC-QTOF MS测定,采用外标法定量。在全扫描采集模式下,以特征离子峰的峰面积定量,以化合物的保留时间、精确质量数及谱库检索定准确性。23种化合物在线性范围内均呈现良好的线性关系,相关系数均大于0.99,23种化合物的定量限(S/N=10)为0.05~0.1mg/kg,在0.1~5.0mg/kg 3个添加水平下的平均回收率为79%~112%,相对标准偏差(RSD,n=6)均低于14%。该方法简便、快速、灵敏,可以应用于油脂类食品中23种邻苯二甲酸酯类的同时检测。
An efficient method was established for the simultaneous determination of 23 phthalate esters residues in grease food by gas chromatography coupled with quadrupole time of flight mass spectrometry （ GC - QTOF MS）. The samples were extracted with Acetonitrile - methyl tertiary butyl ether （9 ： 1, v/v） and cleaned -up with PSA adsorbents, then determined by GC -QTOF MS and quantified by external standard method. The confirmatory analysis for target compounds was performed with the retention time and qualitative fragments obtained by data - retrieval and fragmentations. The correlation coefficients of the 23 phthalate esters were more than 0.99 in their linear ranges and the limits of quantifi- cation （LOQs） were 0. 05 - 0. 1 mg/kg. The mean recoveries for the 23 phthalate esters in grease food were between 79% and 112% with the relative standard deviations （ RSDs, n = 6） not more than 14%. The method is rapid, sensitive, and suitable for the simultaneous determination of multi - classes of phthalate esters in grease food.
出处
《贵州师范大学学报（自然科学版）》
CAS
2017年第3期92-97,115,共7页
Journal of Guizhou Normal University：Natural Sciences
基金
国家质检总局科研课题(2015IK085)
关键词
气相色谱-四极杆-飞行时间质谱
邻苯二甲酸酯类
塑化剂
油脂类食品
gas chromatography coupled with quadrupole time of flight Mass spectrometry （GC -QT- OF MS）
phthalate esters
plasticizer
grease food
