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

摘要: 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10～5 000 μg•kg^-1，线性关系良好（r＞0.99）；在10～100 μg•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2 μg•kg^-1。

Abstract: 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%.