基质分散固相萃取—高效液相色谱法检测鸡蛋中氯羟吡啶和二硝托胺药物残留

Determination of Clopidol and Dinitolmide Residues in Eggs based on Matrix Dispersion Solid-phase Extraction and High Performance Liquid Chromatography

建立基于基质分散固相萃取(MSPD)—高效液相色谱法(HPLC)同步检测鸡蛋中氯羟吡啶和二硝托胺残留的快速、高效、经济的方法。鸡蛋样品经甲醇—乙腈混合溶液提取,利用200 mg十八烷基键合硅胶吸附剂(C18)和50 mg N-丙基乙二胺(PSA)混合分散固相萃取粉末净化,C18色谱柱分离,纯水—乙腈作为流动相进行梯度洗脱,外标法进行定性定量分析。结果表明,氯羟吡啶和二硝托胺在0.025~50.0μg/mL范围呈良好的线性关系(R^(2)>0.999),检出限为0.025 mg/kg和0.050 mg/kg,定量限为0.075 mg/kg和0.100 mg/kg。在0.1、2.5 mg/kg和5.0 mg/kg水平的加标回收试验中,氯羟吡啶的回收率为87.70%~101.78%,相对标准偏差(RSD)为0.66%~5.41%;二硝托胺的回收率为84.99%~97.11%,RSD为0.95%~5.34%。该方法简便、净化效果好、回收率高,适用于鸡蛋中氯羟吡啶和二硝托胺药物的同步定量检测。

To establish a rapid,efficient,and cost-effective method for the simultaneous determination of clopidol and dinitolmide residues in eggs based on matrix solid-phase dispersion extraction and high performance liquid chromatography.Egg samples were extracted with a methanol-acetonitrile mixture,purified using a mixture of 200 mg octadecylsilane bonded phase and 50 mg primary secondary amine for dispersion solid-phase extraction,separated using a C18 column,and eluted with a gradient of wateracetonitrile as the mobile phase.Quantitative and qualitative analysis were conducted using an external standard method.Results show that the clopidol and dinitolmide exhibited good linear relationships in the range of 0.025~50.0μg/mL(R^(2)>0.999).The limits of detection were 0.025 mg/kg and 0.050 mg/kg,while the limits of quantitation were 0.075 mg/kg and 0.100 mg/kg for clopidol and dinitolmide In the spiked recovery tests at levels of 0.1,2.5 mg/kg,and 5.0 mg/kg,the recovery rates for clopidol ranged from 87.70%~101.78%,with relative standard deviations ranging from 0.66%~5.41%.For dinitolmide,the recovery rates ranged from 84.99%~97.11%with relative standard deviations ranging from 0.95%~5.34%.This method is simple,with good purification effects and high recovery rates,making it suitable for the simultaneous quantitative detection of clopidol and dinitolmide residues in eggs.