水产品及水产制品中三聚氰胺检测方法的研究

Research on the detection methods of melamine content in fishery products and aquatic products

采用气相色谱-质谱/质谱法(GC-MS/MS)对鲜、冷或冻水产品(养殖鱼、虾、蟹、贝等)及水产制品(干、熏、盐制水产)中三聚氰胺进行了检测。样品采用乙睛和甲醇提取,提取液离心净化,氮气吹干,利用衍生化试剂BSTFA-TMCS(体积比为99∶1)进行衍生化反应、优化仪器条件、考察基体干扰,利用三重四级杆气相色谱联用的多反应监测(MRM)技术,对三聚氰胺衍生物进行定性定量分析。以三聚氰胺衍生物离子对m/z 342>171、m/z 342>327离子对进行定性,以m/z 342>327进行定量。方法的线性范围为0.005μg/L^0.1μg/L;回归方程为y=1 434 164.378 8x-704.012 5,相关系数R2=0.999 4;方法定量限0.03 mg/kg。回收率达90%以上,相对标准偏差RSD<5.0%。该方法简便、快速、灵敏、准确,适合于水产品和水产制品中三聚氰胺含量的确证和定量测定。

The melamine contents in fresh,cool or frozen fishery products（farming-fish,shrimp,crab,cowry and so on）and aquatic products（dried,smoke-dried,saline）were detected by gas chromatography-mass/mass spectrometry（GC-MS/MS）.Samples were extracted with acetonitrile and methanol,extracting solution was purged after decentralization,blowed dry through nitrogen and derivatized with a mixed system composed of BSTFA and TMCS（99：1,V/V）prior to GC-QqQ-MS/MS analysis in multiple reaction monitoring（MRM）mode.The optimal values of crucial instrument parameters and matrix interference were investigated.Melamine was qualified using the ion pairs of m/z 345〉 171 and m/z 342〉 327 and quantified using the ion pair of m/z 342 〉327.The developed method exhibited good linearity within the range of 0.0050 to 0.100 ug / L.The regression equation was y=1 434 164.378 8x-704.012 5,and correlation was 0.999 4.The detection Limit was 0.03 mg / kg for melamine（RSN =10）and the recoveries for determining melamine were greater than 90%.The relative standard deviations were less than 5.0%.This method is simple and convenient,rapid,sensitive and accurate,and can meet analysis requirements of melamine in fishery Products and aquatic products.