LC-MS/MS法结合谱库检索测定猪组织中三聚氰胺及其同系物

Determination of Melamine and Its Homologues in Pig Tissues by LC-MS/MS Combining with Spectral Library Search

采用MRM→IDA→EPI→谱库检索模式建立了猪组织中三聚氰胺及其同系物的液相色谱-电喷雾串联质谱多残留检测方法,结合谱库检索功能同时实现了定性定量分析。组织样品经2%三氯乙酸、10%乙酸铅和乙腈混合溶液提取,Sepucol ENVI-CARB柱净化,三聚氰胺及其同系物的线性范围为10~5 000μg.kg-1,线性关系良好（r〉0.99）;在10~100μg.kg-1添加水平范围内,平均回收率为94.2%~99.9%、相对标准偏差为3.8%~7.5%、方法检出限为2μg.kg-1。

MRM→IDA→EPI→spectral library search model was used to establish a HPLC-electrospray ionization tandem mass spectrometry method for the multi-residue detection of melamine and its homologues in pig tissues.The quantitative and qualitative analysis of the target analytes were achieved by with spectral library search function.Tissue samples were treated with 2% trichloroacetic acid,10% lead acetate solution and acetonitrile for extraction,purified with Sepucol ENVI-CARB column.The analytical method in the present study was well validated,and good results were obtained with respect to precision,repeatability and spiked recovery.The limit of detection is 2 μg·kg-1 for melamine and its homologues,and with a linear range from 10 to 5 000 μg·kg-1.The recoveries are between 94.2% and 99.9%,and RSDs are between 3.8% and 7.5%.