HPLC法测定蜂王浆冻干粉中的甲砜霉素、氟甲砜霉素及代谢物氟甲砜霉素胺

目的建立高效液相色谱方法测定蜂王浆冻干粉中的甲砜霉素、氟甲砜霉素及代谢物氟甲砜霉素胺的方法。方法采用乙酸乙酯-乙腈-氨水提取蜂王浆冻干粉中残留的化合物,凝胶渗透色谱净化,荧光检测器检测。结果平均回收率84.6%～99.1%,相对标准偏差(RSD)6.02%～9.81%;甲砜霉素、氟甲砜霉素在0.20～5.0mg/L氟甲砜霉素胺在0.1～4.0mg/L范围内有良好的线性关系,甲砜霉素与氟甲砜霉素的检测限达0.025mg/kg、氟甲砜霉素胺的检测限达0.015mg/kg。结论该方法快速、灵敏、准确,适用于分析蜂王浆冻干粉中的甲砜霉素、氟甲砜霉素及代谢物氟甲砜霉素胺含量。

Determination of Thiamphenicol, Florfenicol and Florfenicol Amine in Lyophilized Royal Jelly Powder by HPLC

Objective To establish the high performance liquid chromatography （HPLC） method for the determination of thiamphenicol（ TAP）, florfenicol（FF） and florfenicol amine（FFA） in Lyophilized royal jelly powder. Method The analytes were extracted by ethyl acetate - acetonitrile - ammonia, purified by gel permeation chromatography（GPC） and detected by fluorescence detector. Results The average recoveries and relative standard deviations（RSDs） for the analyts were in the range of 84.6% - 99. 1% and 6.02% - 9. 81% （n = 6） , respectively. Good linearities were obtained in the concentration ranging from 0. 20 - 5.0 mg/L for TAP and FF, and 0. 10 - 4.0 mg/L for FFA. The limits of detection were 0. 025mg/kg for TAP and FF, and 0. 015 mg/kg for FFA. Conclusion The method is rapid, sensitive and can meet the needs for detection of thiamphenieol, florfenieol and florfenicol amine in lyophilized royal jelly powder.