采用注射式分散固相萃取-气相色谱-串联质谱法测定禽蛋中三聚氰胺的含量。禽蛋样品用乙腈提取后，加入无水硫酸镁和氯化钠，离心后，上清液用正己烷除脂。以丙基乙二胺和石墨化炭黑为分散固相吸附剂，进行注射式分散固相萃取，过滤后，滤液用氮气吹干后再进行衍生化。在气相色谱分离中采用DB-5MS石英毛细管色谱柱，在质谱分析中采用定时选择性反应监测模式。三聚氰胺的质量浓度在5.0~200.0 μg·L^-1内与其对应的峰面积呈线性关系，测定下限（10S/N）为2.4~3.5 μg·L^-1。以空白样品为基体进行加标回收试验，所得回收率为80.3%~103%，测定值的相对标准偏差（n=6）为0.60%~8.9%。

GC-MS/MS was applied to the determination of melamine in poultry eggs with dispersive solid phase extraction with syringe. The poultry egg sample was extracted with acetonitrile, and then anhydrous magnesium sulfate and sodium chloride were added. After centrifugation, fat in the supernatant was removed with n-hexane. Dispersive solid phase extraction with syringe was adopted with PSA and GCB as dispersive solid phase adsorbent. After filtration, the filtrate was dried by nitrogen blowing and then derivatized. The DB-5MS quartz capillary chromatographic column was used for GC separation and the timed-selected reaction monitoring mode was adopted in MS determination. Linear relationship between values of peak area and mass concentration of melamine was kept in the range of 5.0-200.0 μg·L^-1, with lower limits of determination (10S/N) in the range of 2.4-3.5 μg·L^-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 80.3%-103%, with RSDs (n=6) in the range of 0.60%-8.9%.