固相萃取气相色谱-质谱联用法测定动物组织中的莱克多巴胺、沙丁胺醇

Determination of Ractopamine,Salbutamol in Animal Tissues by Solid Phase Extraction with Gas Chromatography-Mass Spectrometry

通过液液分配和固相萃取提取、净化动物组织中添加的莱克多巴胺、沙丁胺醇,TMS衍生化试剂BSTFA衍生化,气相色谱-质谱联用对衍生物检测分析,确定了动物组织中莱克多巴胺、沙丁胺醇的定性、定量分析方法,该法检出限为0.5μg/L,衍生物的峰面积与样品浓度在1μg/L￣1000μg/L范围内都呈良好的线性关系,线性回归系数均为0.9998。不同组织中莱克多巴胺加标回收率分别为:肝脏74.8%-85.8%,脂肪71.2%-80.6%,肌肉75.0%-82.7%,肾脏72.0%-82.9%;相对标准偏差为2.3%-5.2%。沙丁胺醇加标回收率分别为肝脏70.5%-76.7%,脂肪72.7%-79.5%,肌肉72.6%-78.5%,肾脏72.5%-75.8%;相对标准偏差为1.8%-5.2%。

The residual veterinary drugs of ractopamine and salbutamol in the animal tissues were extracted and purified by the method of liquid-liquid partition and solid phase extraction. The ractopamine and salbutamol were separated and validated by gas chromatography spectrometry after derivatization of the purified samples with the TMS derivative reagent of BSTFA, and the qualitative and quantitative analysis method was developed. Their limit of detection are 0.5 μg/L, and there are good linear correlations between the ratio of peak areas and the concentration of ractopamine and salbutamol in the add range of 1 μg/L- 1000μg/L, the correlative coefficient is 0.9998 respectively, the recoveries of different concentration of ractopamine and salbutamol in different tissue are： liver 74.8%-85.8% （RAC）, 70.5%-76.7%（SAL）, fat 71.2%-80.6%（RAC）, 72.7%-79.5%（SAL）, meat 75.0%-82.7%（RAC）, 72.6%-78.5%（SAL）, kidney 72.0%-82.9%（RAC）, 72.5%-75.8%（SAL） respectively. The RSDs of the method were： 2.3%-5.2%（RAC）, 1.8%-5.2%（SAL）.