摘要
建立测定乌洛托品的高效液相色谱-串联质谱法,用于快速监测食品中违法添加的乌洛托品。食品中乌洛托品经无水硫酸钠干燥脱水,乙腈提取后,采用梯度洗脱,SCX色谱柱分离,在电喷雾正离子模式下,多反应监测模式进行检测,外标法定量。乌洛托品在1～1 000μg/L浓度范围线性良好,相关系数为0.998 8,方法的检出限为0.2μg/kg,定量限为1.0μg/kg,加标回收率在52.6%～118%,相对标准偏差小于10.2%。本方法快速、准确,特异性强,灵敏度高,样品前处理简便易行,分析周期短,适合大量样品的测定。
A method of liquid chromatography-tandem mass spectrom- etry（LC--MS/MS） was developed to monitor methenamine which il- legally added in foods. Anhydrous sodium sulfate was used for drying and dehydration, and the solution of acetonitrile was used for extrac- ting methenamine. Then, a strong cation exchange（SCX） was ap- plied to separate target compound with gradient elute. The target compound was detected by Multiple Reaction Monitoring（MRM） at electro spray positive ionization（ESIq-） mode. The external standard method was adopted to quantify. The calibration curves showed good linearity for target compound with the detection range of 1 ~ 1000 pg/L. Correlative coefficient was 0. 998 8, the method of limits of deteetion（LOD） and the method of limits of quantitation（LOQ） were respectively 0.2 μg/kg and 1.0μg/kg, respectively. The spiked re- coveries in foods ranged 52. 6% from 118% with RSDs less than10.2%. This proposed method was rapid, accuracy, strong specifici- ty, high sensitivity. Pretreatment was easy to operate and satisfied with fast speed. The conclusion in this study showed it is suitable for the quantitative determination methenamine in foods.
出处
《食品与机械》
CSCD
北大核心
2013年第3期72-78,共7页
Food and Machinery
基金
"十二五"国家科技支撑计划项目(编号:2012BAK17B17)
湖南省科研条件创新专项计划项目(编号:2012TT1008)
关键词
液相色谱-串联质谱法
快速测定
食品
乌洛托品残留量
liquid chromatography-tandem mass spectrometry, rapiddetermination, food, methenamine residues
