在线柱前衍生-高效液相色谱-荧光检测法测定牛奶中乙酰氨基阿维菌素残留量

Determination of eprinomectin residue in bovine milk by online pre-column derivatization-high performance liquid chromatography-fluorescence detection method

中文关键词:  在线柱前衍生  高效液相色谱法  乙酰氨基阿维菌素  牛奶  残留

英文关键词:online pre-column derivatization  high performance liquid chromatography  eprinomectin  bovine milk  residue

中文摘要:

      目的 建立一种在线柱前衍生-高效液相色谱-荧光检测法测定牛奶中乙酰氨基阿维菌素残留量。 方法 试样经饱和氯化钠水溶液盐析后, 利用乙腈-二氯甲烷溶液提取, 氮气吹干、10%(体积分数)N-甲基咪唑-乙腈溶液复溶、乙腈饱和正己烷多次净化。利用进样程序对净化后的溶液进行在线柱前衍生, 高效液相色谱仪分离, 荧光检测器检测, 以保留时间定性, 峰面积定量。结果 结果表明, 在25~400 ng/mL浓度范围内, 标准曲线线性关系良好, 相关系数r2大于0.999; 该方法的回收率在94.8%~103.8%之间, 相对标准偏差(relative standard deviation, RSD)均小于1.5。结论 该方法非常简便, 且具有较高的准确度、灵敏度和稳定性, 适用于牛奶中乙酰氨基阿维菌素残留的检测。

英文摘要:

      Objective To establish a method for the determination of residual eprinomectin in bovine milk by online pre-column derivatization-high performance liquid chromatography-fluorescence detection (HPLC-FLD). Method The eprinomectin B1a in samples was extracted with acetonitrile-dichloromethane after adding saturated sodium chloride solution for salting out. The acquired extract was dried with nitrogen, reconstituted in acetonitrile containing 10% (volume fraction) N-methylimidazole, and purified by acetonitrile saturated n-hexane for several times. The purified solution was pretreated by injection procedure for online pre-column derivatization, then separated by HPLC and detected by FLD detector. The retention time was used for qualitative analysis and the peak area was used for quantitative analysis. Result The results showed that the standard curves of eprinomectin B1a were linearly correlated in the concentration range of 25?400 ng/mL, and the correlation coefficients were above 0.999. The recoveries of eprinomectin B1a in spiked negative milk sample varied from 94.8% to 103.8%, with the relative standard deviations were less than 1.5%. Conclusion This method is very simple, and has high sensitivity, accuracy and stability, which is suitable for detection of eprinomectin residue in bovine milk.