以三聚氰胺为模板分子制备了三聚氰胺分子印迹聚合物(MIP),并将此聚合物装入自制的漏斗型固相萃取柱(SPE),制成对三聚氰胺有特异分子识别能力的SPE小柱。称取样品溶液10 mL,以0.5 mL·min-1速率流经SPE小柱,依次用水和甲醇-水(1+1)混合液各5 mL淋洗小柱后,用甲醇-氨水(95+5)混合液8 mL自然洗脱,将洗脱液吹氮蒸干,用甲醇1 mL溶解残渣,所得溶液用于高效液相色谱分析。选用Inertsil ODS-SP C18色谱柱及(A) pH 3.0的10 mmol·L-1辛烷磺酸钠-10 mmol·L-1柠檬酸混合溶液和(B)乙腈以90比10比例相混的混合液作为流动相进行色谱分离。检测波长为240 nm。在3个浓度水平进行回收试验,测得回收率在89.0%~97.0%之间。

Melamine was used as pattern plate in the preparation of melamine moleculary imprinted polymer (MIP), which was packed into the self-made funnel-like solid phase extraction (SPE) micro-column, to form a MIP-SPE microcolumn having selective adsorptive property toward melamine. 10 mL of the sample solution was passed through the micro column at a flow-rate of 0.5 mL·min-1. After rinsing the column with 5 mL each of H2O and mixture of CH3OH and H2O(1+1) in succession, the column was eluted with 8 mL of mixture of CH3OH and aq. NH3(95+5), and the eluate was evaporated to dryness by N2-blowing. The residue was dissolved with 1.00 mL of CH3OH, which was used for HPLC analysis. LC separation was performed by using Inertsil ODS-SP C18 column as stationary phase, and using a mixture of (A) mixed solution of 10 mmol·L-1 sodium octane sulfonate and 10 mmol·L-1 citric acid (pH 3.0) and (B) acetonitrile (mixed in the volumic ratio of 90+10) as mobile phase. UV-detection at 240 nm was adopted in the determination. Recovery was tested by standard addition method at 3 concentration levels, values of recovery found were ranged from 89.0% to 97.0%.