UPLC-MS/MS法测定食品接触材料中的成核剂

Determination of Nucleating Agents in Food Contact Materials by UPLC-MS/MS

建立了高效液相色谱-串联质谱法(UPLC-MS/MS)测定食品接触材料及制品中(1R,2R,3S,4S)-rel-二环[2.2.1]庚-2,3-二羧酸二钠盐迁移量的方法。样品中的(1R,2R,3S,4S)-rel-二环[2.2.1]庚-2,3-二羧酸二钠盐在一定温度、时间接触的状态下会迁移到食品模拟物中。以T3色谱柱进行分离,甲醇-5 mmol/L甲酸铵为流动相洗脱,采用电喷雾离子源(ESI),多反应监测(MRM)负离子模式进行扫描,测定迁移到食品模拟物中的目标物。结果表明,(1R,2R,3S,4S)-rel-二环[2.2.1]庚-2,3-二羧酸二钠盐的色谱分离良好,在5.00~100μg/L浓度范围内与其峰面积均呈线性关系。该方法对水基、酸性食品、酒精类食品模拟液和油基模拟物的定量限均为5.0μg/L,重复性试验的相对标准偏差为0.73%~1.5%(n=6),加标回收率为80.5%~103%。该方法快速可靠、准确简便,适用于食品接触材料及制品中(1R,2R,3S,4S)-rel-二环[2.2.1]庚-2,3-二羧酸二钠盐的检测。

.A high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was developed to determine the migration amounts of(1 R,2 R,3 S,4 S)-rel-bicyclo[2.2.1]hept-2,3-dicarboxylacid,disodium salt in food contact materials and products.(1 R,2 R,3 S,4 S)-rel-bicyclo[2.2.1]heptane-2,3-dicarboxylicacid disodium salt was transferred into food stimulant in the sample contacted at a certain temperature and time.The separation was performed using a T3 chromatography column with methanol-5 mmol/L ammonium formate as a mobile phase.Under the electrospray ionization source(ESI),(1 R,2 R,3 S,4 S)-rel-bicyclo[2.2.1]heptane-2,3-dicarboxylic acid disodium salt was detected in a multiplereaction monitoring mode(MRM).The results showed that(1 R,2 R,3 S,4 S)-rel-bicyclo[2.2.1]heptane-2,3-dicarboxylic acid disodium salt was well separated,and linear relation between peak area and concentration was excellent,when it ranges from 5.00-100μg/L.LOQ of(1 R,2 R,3 S,4 S)-rel-bicyclo[2.2.1]heptane-2,3-dicarboxylic acid disodium salt was 5.0μg/L for water-based,acidic food,and alcohol-based food simulating liquid,as well as for the oil-based mimic.Relative standard deviation(RSD)was 0.73%-1.5%for repeatability test(n=6),and recovery rate was 80.5%-103%.The method was quick,reliable,accurate and simple,and it was suitable for the determination of(1 R,2 R,3 S,4 S)-rel-bicyclo[2.2.1]heptane-2,3-dicarboxylic acid disodium salt in food contact materials and products.