柱前衍生-高效液相色谱法同时测定水产品和水发食品中4种脂肪胺  

Simultaneous determination of 4 aliphatic amines in aquatic products and water-soaked foodstuffs by high performance liquid chromatography after pre-column ultraviolet derivatization

作　　者：谢娟[1,2] 李晓辉[3] 王瑶[3] 李明川[3] 史莹[1,2] 曾力[1,2] 卢丹[1,2] 孙成均[1,2] 

机构地区：[1]四川大学华西公共卫生学院,成都610041 [2]食品安全监测与风险评估四川省重点实验室,成都610041 [3]成都市疾病预防控制中心,成都610041

出　　处：《分析试验室》2013年第3期93-97,共5页Chinese Journal of Analysis Laboratory

基　　金：成都市疾病预防控制中心重点项目(100104)资助

摘　　要：建立水产品和水发食品中甲胺、乙胺、二甲胺和二乙胺的柱前衍生-高效液相色谱同时测定方法。样品经10%三氯乙酸匀浆、离心后,取上清液与9-芴甲氧羰酰氯(FMOC-Cl)在0.10 mol/L四硼酸钠溶液中反应生成具有紫外吸收的衍生产物,然后以C18柱为分离柱、甲醇-水为流动相,流速梯度洗脱分离,以DAD检测器在265nm波长处检测,标准曲线法定量。4种脂肪胺衍生产物在16 min内可完全分离。在0.5～25μg/mL浓度范围内,各物质的质量浓度与色谱峰面积均具有良好线性关系(r>0.999),方法检出限分别为:甲胺0.05 mg/kg、乙胺0.21 mg/kg、二甲胺0.29 mg/kg、二乙胺0.80 mg/kg。方法的加标回收率为88.1%～100.7%,相对标准差均小于5%。方法可用于水产品和水发食品中4种脂肪胺的同时快速测定。To establish a high performance liquid chromatographic method for the determination of aliphatic amines including methylamine （ MA ）, ethylamine （ EA）, dimethylamine （DMA） and diethylamine （DEA） in aquatic products and water-soaked foodstuffs after pre-column ultraviolet derivatization with 9-fluorenyl methylchloroformate （FMOC-C1）. The samples were extracted with 10% trichloroacetic acid and centrifuged then a suitable amount of supernatant reacted with FMOC-C1 in 0. 10 mol/L sodium borate buffer solution an d produced ultraviolet absorbing derivatives. The derivatives were separated on a C18 column using flow rate gradient elution with a mobile phase of methanol-water, and detected using a diode array detector （DAD） at 265 nm. The experimental results showed that the four aliphatic amines derivative products could be completely separated in 16 min. The coefficients of correlation of the method in the range from 0. 5 - 25 μg/mL were greater than 0. 999. The detection limits of MA, EA, DMA and DEA were 0. 05, 0. 21,0. 29 and 0. 80 mg/kg, respectively. The recoveries were in the range from 88. 1% to 100. 7% with the relative standard deviations （RSDs） of less than 5%. This method is sensitive and accurate, simple and rapid; and it can be used for the determination of the four aliphatic amines in aquatic products and water-soaked foodstuffs.

关 键 词：高效液相色谱法 柱前紫外衍生 水产品 水发食品 脂肪胺 

分 类 号：O657.7[理学—分析化学]