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液相色谱串联质谱法测定辐照含脂食品中2-十二烷基环丁酮的研究
引用本文:蒋俊树,朱峰,聂磊.液相色谱串联质谱法测定辐照含脂食品中2-十二烷基环丁酮的研究[J].安徽化工,2012,38(3):67-69,71.
作者姓名:蒋俊树  朱峰  聂磊
作者单位:安徽国家农业标准化与监测中心,安徽合肥230051;安徽大学化学化工学院,安徽合肥230039;安徽大学化学化工学院,安徽合肥,230039;安徽国家农业标准化与监测中心,安徽合肥,230051
基金项目:安徽省质检科技计划项目(ziy-011)
摘    要:以辐照含脂食品为实验材料,首次建立了液相色谱串联质谱法(HPLC-ESI-MS/MS)测定辐照含脂食品中2-十二烷基环丁酮(2-DCB)的含量。样品经正己烷提取浓缩得到脂肪,再经中性氧化铝柱净化后,采用液相色谱串联质谱法(HPLC-ESI-MS/MS)分析,多反应监测模式下(MRM)外标法定量。结果表明:方法在5~100μg/L范围内线性良好,线性相关系数为r=0.9996,定量下限为0.08 mg/kg(以脂肪计),回收率在75%~95%之间,相对标准偏差(RSD)小于10%。该方法前处理过程简便快捷,回收率高,可满足实验室大量、快速分析的需求。

关 键 词:2-十二烷基环丁酮  辐照  含脂食品  液相色谱串联质谱

Determination of 2-Dodecylcyclobutanone in Irradiated Foods Containing Fat by HPLC/MS/MS
JIANG Jun-shu , ZHU Feng , NIE Lei.Determination of 2-Dodecylcyclobutanone in Irradiated Foods Containing Fat by HPLC/MS/MS[J].Anhui Chemical Industry,2012,38(3):67-69,71.
Authors:JIANG Jun-shu  ZHU Feng  NIE Lei
Affiliation:1 (1. The Center of Anhui National Agricultural Standardization and Monitoring, Hefei 230051, China; 2. College of Chemistry and Chemical Engineering, Anhui University, Hefei 230039, China)
Abstract:A new method using of ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-ESI-MS/MS) for the analysis of 2-Dodecylcyclobutanone (2-DCB) in irradiated foods containing fat has been firstly developed. The samples were extracted by using ultrasound extraction technology. The extracts were dehydrated by anhydrous sodium sulfatecleaned and concentrated by rotary evaporation technology to get fat. The fat was cleaned up with neutral alumina column. And then determined by LC-ESI-MS/MS. Separated analytes were determined using multiple reaction monitoring (MRM). The result indicated that the calibration curves were linear in the range of 5- 100 μg/L for 2-DCB. The quantitation limit was 0.08 mg/kg (fat). The recoveries of 2-Dodecylcyclobutanone were in the range of 75%~95%, with RSDs (n=6)〈10%. This method shortened the time of pre-treatment process, and the result was credible. It could satisfy the requirement of mass and fast analysis in the laboratory.
Keywords:2-Dodecylcyclobutanone  irradiate  foods containing fat  LC-MS/MS
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