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

SPE-HPLC simultaneous determination of twelve sulfonamide residues in egg powder

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Wa-tersOasisMCX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InertsilODS-3(250mm×4.6mm,5μm)柱分离,以乙腈-水-冰醋酸(23∶77∶0.5)为流动相进行等度洗脱,265nm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22min内出峰,在0.1～10.0μg.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0.002～0.045μg.mL-1,相当于鸡蛋粉中12种磺胺药物的最小检出限在0.002～0.045μg.g-1;当加标水平在0.1～1.0μg.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 coefficients0.9995）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.