摘要
建立了固相萃取法结合气相色谱-三重四级杆串联质谱同时检测香精中22种邻苯二甲酸酯(PAEs)残留量的方法。样品经乙腈和正己烷混合溶液提取,固相萃取小柱净化,然后进行测定,内标法定量。结果表明,22种邻苯二甲酸酯在3～1000μg/L范围内呈线性相关关系,判定系数R^2≥0.9922。方法检出限为0.3～1.0μg/kg,方法定量限为1.0～3.0μg/kg。添加20、40和200μg/kg三个不同浓度水平,香精中22种邻苯二甲酸酯加标回收率为82.4%～107.1%,相对标准偏差为≤9.1%(n=6)。用此建立的方法测定了实际香精样品中的22种邻苯二甲酸酯,检出率为45.0%。此方法操作简单,灵敏度高和准确度高,适用范围广,适合香精中22种邻苯二甲酸酯残留量的检测。
A method was developed for 22 phthalate esters residues in essence using gas chromatography-triple quadrupole mass spectrometry.The samples were extracted with acetonitrile and N-hexane,cleaned up with solid phase extraction,and quantified using internal standard.The results showed that the calibration curves of the 22 phthalate esters showed good linearity in the range of 3～1000 μg/L,with the coefficient of determination（ R^2） not less than 0.9922.The limits of detection（ LODs）were 0.3～1.0 μg/kg and the limits of quantification（ LOQs） were 1.0～3.0 μg/kg.The mean recoveries in essence at the three spiked levels of 20,40 and 200 μg/kg were 82.4% ～107.1%,the relative standard deviation（ RSD） were not more than 9.1%（ n = 6）.The 22 phthalate esters in the actual samples were determined by this method with the detection rate of 45.0%.The method is suitable for the determination of the 22 phthalate esters in essence with easy operation,high sensitivity and accuracy,and wide ranges of applications.
作者
阮小娇
黄海智
盛华栋
吴丹
程焕
李红艳
邢峰
张水锋
RUAN Xiao-jiao;HUANG Hai-zhi;SHENG Hua-dong;WU Dan;CHENG Huan;LI Hong-yan;XING Feng;ZHANG Shui-feng(Zhejiang Fangyuan Test Group Co.,Ltd.,Hangzhou 310018,China;Zhejiang Institute of Quality Inspection Science,Hangzhou 310018,China;College of Biosystems Engineering and Food Science,National-Local Joint Engineering Laboratory of Intelligent Food Technology and Equipment,Zhejiang University,Hangzhou 310058,China)
出处
《食品工业科技》
CAS
CSCD
北大核心
2018年第22期235-240,246,共7页
Science and Technology of Food Industry
基金
浙江省技术质量监督局科研计划项目(20160211)
浙江省自然科学基金项目(LY17C200013)
关键词
气相色谱
三重四级杆串联质谱
邻苯二甲酸酯
香精
同位素稀释
gas chromatography
triple quadrupole mass spectrometry
phthalate esters
essence
isotope dilution
