同位素稀释高效液相色谱-串联质谱法测定面粉及面制品中的联二脲  

Determination of Biurea in Flour and Flour Products by Isotope Dilution High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：阮莎莎[1] 刘桂华[2] 刘素纯[1] 朱舟[2] 刘建军[2] 

机构地区：[1]湖南农业大学食品科学技术学院,湖南长沙410128 [2]深圳市疾病预防控制中心,广东深圳518055

出　　处：《分析测试学报》2016年第4期420-425,共6页Journal of Instrumental Analysis

基　　金：2014年深圳市科技研发资金基础研究项目(JCYJ20140410164217367)

摘　　要：建立了面粉及其制品中联二脲的同位素稀释高效液相色谱-串联质谱检测方法。采用纯水超声提取,含油脂的样品加正己烷脱脂,所得样液进行高效液相色谱-串联质谱测定。以乙腈与纯水为流动相,梯度洗脱,经Waters XBridge BEH Amide（3.5μm,4.6 mm×150 mm）色谱柱分离,MS/MS采用电喷雾电离正离子（ESI^＋）,多反应监测（MRM）模式检测,同位素内标法定量。方法的线性范围为0.2-100μg/L,相关系数为0.999 9;在面粉、馒头、面包、油条和面条5种基质中的平均加标回收率为82.0%-113.6%,相对标准偏差（RSD）为2.1%-9.3%;方法定量下限（LOQ）为20μg/kg。应用该方法对136份市售的面粉及面制品进行检测,在42份样品中检出联二脲,检出率为30.88%。其中面粉检出4份,含量为43.7-564μg/kg;馒头未检出;面条检出2份,分别为70.8μg/kg与9 840μg/kg;油条检出1份,含量为2 480μg/kg;面包表层检出15份,含量为27.4-8 730μg/kg;面包内芯检出20份,含量为64.3-18 100μg/kg。该方法操作简单、灵敏快速、准确可靠,适用于面粉及其制品中联二脲的测定。An isotope dilution high performance liquid chromatography-tandem mass spectrometric（HPLC-MS /MS） method was established for the determination of biurea in flour and flour products.The biurea in certain matrices was extracted with ultrapure water,defatted with n-hexane when necessary,and then analyzed by HPLC-MS / MS.LC separation was performed on a Waters XBridge BEH Amide column（3.5 μm,4.6 mm × 150 mm） using ultrapure water and acetonitrile as mobile phase by gradient elution.Identification was achieved by electrospray ionization（ESI^＋） in positive mode using multiple reaction monitoring.Quantification was performed by isotope labeled13C2,15N2-biurea internal standard calibration.The calibration curve of biurea showed a good linearity in the range of 0.2-100 μg / L with a correlation coefficient of 0.999 9.The average recoveries of biurea in flour,steamed bun,bread,deep-fried dough stick and noodle matrices（six aliquots for each level）at three spiked levels ranged from 82.0% to 113.6%,with RSDs of 2.1%-9.3%.The LOQ of the methed was 20 μg / kg.The optimized method was successfully applied in the analysis of 136 real samples collected from local markets in Southern China,while biurea residues were found in 42（30.88%） samples,of which 43.7-564 μg /kg of biurea existed in 4 flours,70.8-9 840 μg /kg in 2 noodles,2 480 μg / kg in 1 deep-fried dough stick,27.4-8 730 μg / kg in 15 breads-crust and 64.3-18 100 μg / kg in 20 breads-interior.This method is applicable for the determination of biurea in flour and different flour products due to its operation convenience,high sensitivity and goodaccuracy.

关 键 词：高效液相色谱-串联质谱法 同位素内标 面粉 面制品 联二脲 

分 类 号：O657.63[理学—分析化学] TQ225.261[理学—化学]