三嗪基磁性纳米粒子富集和测定粮油中苯并(a)芘

Enrichment and determination benzo[a]pyrene in cereals and oils using triazine-based magnetic nanoparticles

中文关键词:  三嗪基磁性纳米粒子  苯并(a)芘  超高效液相色谱法  磁性固相萃取  谷物  油脂

英文关键词:triazine-based magnetic nanoparticles  benzo[a]pyrene  ultra performance liquid chromatography  magnetic solid-phase extraction  cereals  oils

中文摘要:

      目的 建立超高效液相色谱荧光检测法测定谷物和油脂中苯并(a)芘含量的方法。方法 采用三嗪基共价层状网络修饰的磁性纳米粒子功能材料作为固相萃取吸附剂, 样品经正己烷提取, 提取液经吸附剂净化, Waters BEH C18柱(100 mm×2.1 mm, 1.7 μm)进行色谱分离, 采用超高效液相色谱法测定, 外标法定量, 建立了超高效液相色谱荧光检测谷物和油脂中苯并(a)芘的方法。考察了样品溶液的pH、吸附剂用量、吸附时间、重复使用次数、洗脱剂种类和用量等影响富集萃取效率的因素。结果 在0.5~20.0 ng/mL范围内, 苯并(a)芘线性关系较好, 线性相关系数(R2)为0.9998, 该方法的检出限和定量限分别为0.15 μg/kg和0.5 μg/kg, 回收率为79%~90%, 相对标准偏差小于3.53%。结论 制备的吸附剂对苯并(a)芘具有良好的吸附能力, 可循环使用, 该方法灵敏、简单、节省成本, 并成功应用于粮油中痕量苯并(a)芘检测。

英文摘要:

      Objective To establish a method for the determination of benzo[a]pyrene residues in cereals and oils by ultra performance liquid chromatography fuorescence detection. Methods A rapid and effective magnetic solid-phase extraction ultra performance liquid chromatography fuorescence detection method, using triazine-based covalent layered network modified magnetic nanoparticles as magnetic solid-phase extraction sorbent, was established to enrich and determine benzo[a]pyrene in cereals and oils. The samples were extracted by n-hexane, and purified by the sorbent. The chromatographic separation was performed on Waters BEH C18 (100 mm×2.1 mm, 1.7 μm) chromatographic column, determined by ultra performance liquid chromatography, and quantified by external standard method. Parameters infuencing the extraction effciency, such as pH of the sample solution, amount of sorbent, adsorption time, number of reuses, the eluent type and volume, were examined. Results In the range of 0.5?20.0 ng/mL, had good linear relationships, and the linear correlation coefficient (R2) was 0.9998. The limit of detection and limit of quantitation was 0.15 μg/kg and 0.5 μg/kg, respectively. The recoveries of the method were desirable at 79%?90% and the relative standard deviation was less than 3.53%. Conclusion The prepared adsorbent has good adsorption capacity for benzo[a]pyrene and can be recycled. The proposed method is sensitive, simple, and cost-saving, successfully applied to the detection of trace benzo[a]pyrene in cereal and oil.