高效液相色谱串联质谱法测定牛奶中左旋咪唑的残留量

Determination of levamisole residues in milk by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  牛奶  左旋咪唑  高效液相色谱串联质谱法

英文关键词:milk  levamisole  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牛奶中左旋咪唑的残留量。方法 牛奶样品用碱性乙酸乙酯提取, 经振荡、离心、旋转蒸发后, 再经盐酸提取, 上清液经MCX固相萃取柱净化, 氨化甲醇洗脱, 氮气吹干, 乙腈水定容, 过0.22 μm有机滤膜, 高效液相色谱-串联质谱测定, 多反应监测(multiple reaction monitoring, MRM), 外标法定量。结果 左旋咪唑在0~20 ng/mL的浓度范围内线性关系良好, 相关系数为0.995, 牛奶中左旋咪唑检出限为0.4 μg/kg, 加标回收率为82.33%~104.49%, 相对标准偏差均小于7%。 结论 该方法前处理简便快速, 灵敏度高, 适用于牛奶中左旋咪唑残留量的检测。

英文摘要:

      Objective To establish a method for the determination of levamisole residues in milk by high performance liquid chromatography tandem mass spectrometry. Methods Milk samples were extracted with alkaline ethyl acetate and shaken, centrifuged and rotary evaporated. After extraction with hydrochloric acid, the supernatant was purified by MCX solid phase extraction column, eluted with ammoniated methanol, and dried by nitrogen, then made up to volume with acetonitrile water, and passed through an organic filter of 0.22 μm. It was determined by high performance liquid chromatography-tandem mass spectrometry with multiple reaction monitoring (MRM), and quantified by external standard method. Results The linear relationship of levamisole in the concentration range of 0?20 ng/mL was good, the correlation coefficient was 0.995, the detection limit of levamisole in milk was 0.4 μg/kg, and the recoveries of standard addition were 82.33%?104.49%. The relative standard deviations were less than 7%. Conclusion The pretreatment of this method is simple, rapid, sensitive and suitable for the determination of levamisole residue in milk.