高效液相色谱-串联质谱法测定动物性食品中硝基咪唑类药物残留量

Determination of nitroimidazole drugs residues in animal-based foods by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  硝基咪唑类药物  鸡蛋  鸡肉  猪肉  液相色谱-串联质谱  

英文关键词:nitroimidazole drugs  eggs  chicken  pork  high performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立高效液相色谱-串联质谱法测定鸡蛋、鸡肉和猪肉基质中硝基咪唑类药物的残留量的方法。方法 样品经乙腈和乙腈水溶液超声提取, 乙腈饱和的正己烷溶液去油, 离心, 下层提取液经Prime HLB固相萃取柱净化后, 上机分析。采用C18色谱柱(2.1 mm×100 mm, 1.8 μm)分离, 以0.1%甲酸水溶液和乙腈为流动相进行梯度洗脱, 外标法定量测定。结果 10种硝基咪唑药物在1~100 ng/mL的范围内线性关系良好, 相关系数均高于0.995, 定量限均为1.0 μg/kg。10种硝基咪唑药物于1、2、10倍定量限3个水平下的平均加标回收率范围为80.1%~107.7%, 相对标准偏差范围为0.8%~7.5%。采用该方法对收集的150批次样品进行分析, 共检出3批次阳性样品, 其中2批次鸡蛋样品检出甲硝唑, 含量分别为896.0 μg/kg、1341.3 μg/kg; 1批次鸡肉样品中检出地美硝唑, 含量为480.2 μg/kg。结论 该方法高效准确, 满足猪肉、鸡肉、鸡蛋食品中硝基咪唑类药物的定性定量分析, 有效弥补现有国家标准食品基质不全、操作烦琐等问题, 同时为保障动物源性食品的卫生安全提供技术支撑。

英文摘要:

      Objective To establish a method for the determination of nitroimidazole drugs residues in egg, chicken and pork matrices by high performance liquid chromatography-tandem mass spectrometry. Methods Samples were ultrasonically extracted with acetonitrile and acetonitrile-water solution, followed by degreasing with N-hexane saturated with acetonitrile. After centrifugation, the lower extract was purified using a Prime HLB solid-phase extraction column to instrumental analysis. Separation was achieved on a C18 column (2.1 mm×100 mm, 1.8 μm) with a gradient elution using 0.1% formic acid in water and acetonitrile as mobile phases. Quantification was performed by the external standard method. Results The 10 kinds of nitroimidazole drugs exhibited good linearity within the range of 1–100 ng/mL, with correlation coefficients (r2) exceeding 0.995. The limit of quantitation for all compounds was 1.0 μg/kg. Average spike recoveries at 3 levels (1, 2 and 10 time limit of quantitation) ranged from 80.1% to 107.7%, with relative standard deviations between 0.8% and 7.5%. Analysis of 150 batches of samples using this method detected 3 positive batches: Metronidazole was identified in 2 egg samples (896.0 μg/kg and 1341.3 μg/kg), and dimetridazole was found in 1 chicken sample (480.2 μg/kg). Conclusion This method is highly efficient and accurate, capable of conducting qualitative and quantitative analysis of nitroimidazole drugs in pork, chicken and egg products. It effectively addresses the issues of incomplete food matrix and cumbersome operation in the current national standards, and provides technical support for ensuring the hygiene and safety of animal-derived foods.