固相萃取-高效液相色谱法同时测定鸡蛋粉中12种磺胺类药物残留量

目的: 建立鸡蛋粉中12种磺胺类药物残留量的测定方法。方法: 样品用乙腈提取,正己烷脱脂,抽干,盐酸酸化,过Waters Oasis MCX小柱净化,用甲醇淋洗杂质,6%的氨化甲醇溶液洗脱磺胺类药物,洗脱液氮气吹干,流动相溶解后上HPLC仪分析。采用Inertsil ODS-3(250 mm×4.6 mm,5 μm)柱分离,以乙腈-水-冰醋酸 (23∶[KG-*2]77∶[KG-*2]0.5)为流动相进行等度洗脱,265 nm波长检测,外标法定量测定磺胺类药物。结果: 12种磺胺类药物在22 min 内出峰,在0.1~10.0 μg·mL^-1范围内呈良好的线性关系,r值均在0.9995以上;最低检出浓度为0.002~0.045 μg·mL^-1,相当于鸡蛋粉中12种磺胺药物的最小检出限在0.002~0.045 μg·g^-1;当加标水平在0.1~1.0 μg·g^-1时,12种磺胺类药物平均回收率在(71.13±5.02)%~(99.53±5.13)%之间, RSD为0.3%~4.8%。结论: 该法测定鸡蛋粉中的磺胺类药物具有快速、准确、灵敏的特点,符合出口食品残留分析质量控制规范方法要求。

Objective: To establish a method to determine the twelve sulfonamides (SAs) residues in egg powder. Methods: The method includes the extracting SAs from the egg powder with acetonitrile,degreasing with n-hexane,acidation with hydrochloric acid after the evaporation and cleaning up on a Waters Oasis MCX cartridge solid-phase column.The MCX cartridge column was washed with methanol,and the SAs were eluted with 6% ammonia methanol solution.After the evaporation,the residue was dissolved in mobile phase.Analytical separation was performed on an Inertsil ODS-3(25 cm×4.6 mm,5 μm)column with UV detection at 265 nm under the isocratic elution condition with acetonitrile-water-acetic acid glacial (23∶77∶0.5)as a mobile phase. Results: The suggested method exhibits good linearity (correlation coefficients>0.9995) between the peak areas and the concentration of SAs in a broad concentration range (0.1-10.0 μg·mL^-1),and lower limits of detection of 0.002-0.045 μg·mL^-1 parallel to 0.002-0.045 μg ·g^-1 egg powder.When the spiked levels ranged between 0.1 μg ·g^-1and 1.0 μg·g^-1,the average recoveries of (71.13±5.02)%-(99.53±5.13)% and the relative standard deviations (RSD) between 0.3% and 4.8% to all sulfonamides in the sample were obtained. Conclusion: This method is simple,rapid,sensitive and reliable to determine sulfonamides residues in egg powder.