兔排泄物中阿维菌类药物的高效液相色谱检测

Determination of Avermectins Residues in Rabbit Excreta by High Performance Liquid Chromatography

建立了一种同时检测兔排泄物中阿维菌素、伊维菌素、多拉菌素、爱普菌素的高效液相色谱方法,样品用乙腈提取,Bond Elut C18柱净化,用三氟乙酸酐和1-甲基咪唑的乙腈溶液作衍生化试剂,然后加入冰乙酸和三乙胺进行衍生化反应30min,用液相色谱荧光检测器检测,该方法检测兔排泄物在2～10ng/g的添加范围内兔粪的平均回收率73.17%～101.30%,日内变异系数小于11.61%,日间变异系数小于11.31%,兔尿的的平均回收率在75.69%～101.84%,日内变异系数小于12.20%,日间变异系数小于10.880%,爱普菌素、阿维菌素、多拉菌素和伊维菌素在兔粪中的检出限为0.09～0.25ng.g-1,在兔尿中的检测限为0.04～0.28ng·ml-1。4种药在兔t兔粪便和尿液中的定量限分别是2ng·g-1和2ng·ml-1。该方法可靠、灵敏,可用于常规的残留检测。

A simple muhiresidue analysis method was developed for the simultaneous determination of abamectin, ivermectin, doramectin and eprinomectin ：n rabbit excreta. The samples were extracted with acetonitrile and cleaned up by solid-phase extraction using Bond Elut C18 cartridge, and followed by derivatization with Trifluoroacetic anhydride and 1-methylimidazole in acetonitrile, and acetic acid and Triethylamine were added sequentially. Analysed by high performance liquid chromatography （HPLC）with fluorescence detection after derivatization. Recoveries of avermectins in faeces and urine fortified at 2-10 ng/g were in the range 73.17%-101.30% and 75.69-101.84%, respectively.The intra-day and inter-day variations in faeces were less than 8.52 % and 7.13 % respectively. The intra-day and inter-day variations in urine were less than 12.20 % and 11.88 % respectively. The limits of detection in faeces and urine were n the range 0.09-0.25 ng·g^-1ng/g and0.04-0.28 ng·ml^-1, respectively. The limits of quantification in rabbit faeces and urine were 2 ng·g^-1 and 2 ng·ml^-1 for the four drugs. The procedure provides a reliable and sensitive method for routine residual analysis.