氨基功能化磁性纳米材料净化-高效液相色谱-串联质谱法测定肉类中氟虫腈及其代谢物的含量

Determination of fipronil and its metabolites in meat by amino functionalized magnetic nanomaterials purification-high performance liquid chromatography-mass spectrometry

中文关键词:  氟虫腈及其代谢物  氨基功能化磁性纳米材料  液相色谱-串联质谱法  肉类

英文关键词:fipronil and its metabolites  amino functionalized magnetic nanomaterials  high performance liquid chromatography-mass spectrometry  meat

中文摘要:

      目的 建立氨基功能化磁性纳米材料净化-高效液相色谱-串联质谱法测定肉类中氟虫腈及其代谢物的含量。方法 样品经乙腈-水超声提取, 提取液经氨基功能化磁性纳米材料净化, 氮吹后, 用乙腈水溶液7:3 (V:V)定容并溶解残渣。待测液以甲醇和水为流动相, 采用C18色谱柱作为分析柱, 在电喷雾负离子模式下, 用多反应监测模式进行数据采集, 外标法定量。结果 在所建立的条件下, 目标物质得到很好分离, 在质量浓度1.0~20.0 ng/mL范围内呈现良好的线性关系, 相关系数(r2)大于0.99, 检出限为0.2 μg/kg, 定量限为0.5 μg/kg。通过加标验证, 3个加标水平下的回收率范围为79.94%~94.52%, 相对标准偏差为2.95%~8.22%。结论 与传统前处理方法相比, 该方法利用磁吸架吸磁, 省去离心的操作步骤、节约时间、重现性好、检测成本低, 可以用于肉类中氟虫腈及其代谢物的测定, 为市场中肉类中氟虫腈及代谢产物的残留监测提供技术支撑。

英文摘要:

      Objective To establish a method for determination of fipronil and its metabolites in meat by amino functionalized magnetic nanomaterials purification-high performance liquid chromatography-mass spectrometry. Methods The samples were ultrasonically extracted with acetonitrile-water. The extract was purified by amino-functionalized magnetic nanoparticles, and then concentrated under nitrogen. The residue was dissolved in acetonitrile-water (7:3, V:V) to a final volume. The analyte solution was analyzed using a C18 column with methanol and water as the mobile phase under negative electrospray ionization mode. The data was collected using the multi reaction monitoring mode. The samples were analyzed based on the external standard method. Results Under the established conditions, the target substances were well separated and showed a good linear relationship within the range of 1.0–20.0 ng/mL, with a correlation coefficient (r2) greater than 0.99. The limit of detection was 0.2 μg/kg and the limit of quantitation was 0.5 μg/kg. Through spiked recovery experiments, the recovery rates at 3 spiked levels ranged from 79.94% to 94.52%, with relative standard deviations of 2.95% to 8.22%. Conclusion Compared with traditional pretreatment methods, the proposed method utilizes a magnetic suction frame to absorb magnetism, which can eliminate the centrifugation steps, save time, ensure good reproducibility and reduce detection costs. The proposed method can be used to determine fipronil and its metabolites in meat. The establishment method can provide technical support for monitoring the residues of fipronil and its metabolites in meat on the market supervision.