刘红云 吴昊 张莉 许世富 吴蕾 明文庆 蔡一杰 许晓靖


摘要 [目的]采用二极管阵列高效液相色谱法,建立饲料中莫昔克丁的检测方法。[方法]样品经乙腈溶液提取后,通过HLB 6cc SPE固相萃取小柱净化,C18色谱柱分离;以醋酸-醋酸铵缓冲液(pH 4.8)(取醋酸铵7.7 g,加水400 mL溶解后,用冰醋酸调节pH至4.8)-乙腈(400∶600)为流动相;检测波长为242 nm;柱温50 ℃;流速为2.5 mL/min。[结果]莫昔克丁在5~100 μg/mL具有良好的线性关系(R.2=0.999 0)。检出限为0.5 mg/kg,定量限为1.0 mg/kg。样品在定量限1倍、2倍、10倍3个加标水平下的平均回收率为95.0%~105.2%,批内、批间的相对标准偏差小于10%,日间和日内变异系数均低于15%。[结论]该试验建立的HPLC法简便、灵敏、准确,可用于饲料中莫昔克丁的含量测定。
关键词 饲料;莫昔克丁;含量测定;HPLC法
中图分类号 S816.17文献标识码 A文章编号 0517-6611(2021)07-0197-02
Abstract [Objective]A method for the determination of moxidectin feed by diode array high performance liquid chromatography (DADHPLC)was established.[Method]The sample was extracted by acetonitrile solution and purified by HLB 6cc SPE SPE solid phase extraction column. The mobile phase was acetic acidammonium acetate buffer (pH 4.8) (7.7 g ammonium acetate was dissolved in 400 mL water, and pH was adjusted to 4.8 with glacial acetic acid)acetonitrile (400∶600) as the mobile phase;the detection wavelength was 242 nm;the column temperature was 50 ℃;the flow rate was 2.5 mL/min. [Result]There was a good linear relationship in the range of 5-100 μg/mL (R.2=0.999 0). The detection limit was 0.5 mg/kg and the limit of quantitation was 1.0 mg/kg. The average recoveries of the samples were 950% - 105.2% at 1, 2 and 10 times of the limit of quantification (LOQ). The intra and inter assay relative deviations were less than 10%, and the interday and intraday coefficients of variation were less than 15%. [Conclusion]The HPLC method established in this experiment is simple, sensitive and accurate, and can be used to determine the content of moxidectin in feed.
Key words Feed;Moxidectin;Content determination;HPLC method
作者簡介 刘红云(1975—),女,安徽合肥人,高级兽医师,硕士,从事兽药、饲料、畜牧产品检测和研究工作。
莫昔克丁是一种新型抗寄生虫药,是由链霉菌发酵产生、成分单一、半合成的大环内酯类药物。莫昔克丁比阿维菌素类药物具有更好的驱虫活性,同时具有长效、安全等特性,且极低剂量下就有很强的抗线虫和节肢动物等体内外寄生虫活性,对猪体内的消化道线虫、肺线虫和体外寄生虫都有良好的驱杀效果[1-5]。20世纪80年代中期,莫昔克丁开始作为兽用驱虫药使用。作为新一代驱虫药物,莫昔克丁能够高效地杀灭线虫和体表寄生虫,同时对动物有很好的安全性。现有的杀虫剂伊维菌素、阿维菌素等异味较大,施用后无论是对于动物还是使用者而言都有较为严重的感官刺激。……