液相色谱-串联质谱法检测牛奶中4种阿维菌素类药物残留量的研究

The Research of Avermectins Residues in Milk by LC-MS/MS

关键词:  阿维菌素类药物  残留  牛奶  液相色谱-串联质谱

Key words:  avermectins  residues  milk  LC-MS/MS

摘要:

建立了一种可同时检测牛奶中4种阿维菌素类药物（阿维菌素、伊维菌素、多拉菌素和埃谱利诺菌素）残留的液相色谱-串联质谱方法（LC-MS/MS）。牛奶样品经乙腈提取，高速离心去除蛋白质等杂质，C18柱净化。以0.1%甲酸水溶液和0.1%甲酸乙腈溶液为流动相进行洗脱，流速0.4 mL/min，采用基质匹配标准溶液外标法定量。结果表明：阿维菌素、伊维菌素、多拉菌素和埃谱利诺菌素在0.5~100 ng/mL浓度范围内均呈现良好的线性关系，相关系数（R2）均大于0.996；4种阿维菌素类药物的定量限均为0.5 μg/kg。阿维菌素在0.5～5 μg/kg添加浓度范围内，伊维菌素在0.5～20 μg/kg添加浓度范围内，多拉菌素在0.5～30 μg/kg添加浓度范围内，埃谱利诺菌素在0.5～40 μg/kg添加浓度范围内，回收率为66.4%～120%；批内与批间相对标准偏差均小于20％。该方法具有简便快速、灵敏度高、定性准确，重复性好等特点，可以满足牛奶中4种阿维菌素类药物残留检测的要求。

Abstract:

A LC-MS/MS method was established for the determination of avermectins residues in milk. Avermectin, ivermectin, doramectin and eprinomectin were extracted with acetonitrile and the protein was deposited by high speed centrifugation, then the sample solution was purified with C18 column. The mobile phase were water (0.1% formic acid) and acetonitrile (0.1% formic acid), the flow rate was 0.4 mL/min. The method was quantified by matrix matching standard curves. A good linearity of the calibration curves was obtained with the range of 0.5~50 ng/mL for avermectin, ivermectin, doramectin and eprinomectin,the correlation coefficient R2＞0.996. The limit of quantification of 4 avermectins was 0.5 μg/kg. The average recoveries of avermectins residues from spiked milk were 66.4%～120%, for avermectin at the concentrations of 0.5～5 μg/kg, ivermectin at the concentrations of 0.5～20 μg/kg, doramectin at the concentrations of 0.5～30 μg/kg, and for eprinomectin at the concentrations of 0.5～40 μg/kg. The intra- and inter-batch variation coefficients were both less than 20%. This method can be applied for the determination of avermectins residues in milk.