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目的为测定猪肉中喹乙醇的残留量,建立高效液相色谱的测定方法。方法本文重点研究了喹乙醇残留测定的样品前处理部分,采用不同有机溶液和水进行不同比例混合,优化了样品前处理的条件及测定条件。最终采用均质后的试样在60℃水浴的条件下经甲醇+水(50+50)提取10 min、再经过正已烷的液-液分配净化后,采用旋转蒸发和真空浓缩技术进行浓缩、定容,后经高速离心后取上清液上机。以0.1%乙酸+乙腈(70+30,V/V)为流动相,色谱柱分离后以DAD检测器(二极管阵列检测器)进行测定,外标法定量。结果方法的检出限为40μg/kg,浓度在2.0μg/ml~10.0μg/ml范围内,线性良好(r=0.9998),添加浓度在0.5 mg/kg~2.25 mg/kg时,回收率在83.2%~84.6%之间,相对标准偏差1.2%~2.2%。结论本方法检出限低,回收率高,定性可靠,定量准确,适合于猪肉中喹乙醇残留的检测。
Objective To determine the amount of olaquindox in pork and establish a method for the determination of olaquindox in pork. Methods In this paper, the pretreatment part of olaquindox residue assay was focused on, and different organic solutions and water were mixed in different proportions to optimize the pretreatment conditions and determination conditions. Finally, the homogenized sample was extracted with methanol + water (50 + 50) for 10 min in a water bath at 60 ° C. and purified by liquid-liquid partitioning of n-hexane, then concentrated by rotary evaporation and vacuum concentration , Constant volume, after the high-speed centrifugation to take the supernatant on the machine. The mobile phase was consisted of 0.1% acetic acid and acetonitrile (70 + 30, V / V). After the column was separated by DAD detector (diode array detector), the content was determined by external standard method. Results The detection limit of the method was 40μg / kg and the linearity was good (r = 0.9998) in the range of 2.0μg / ml ~ 10.0μg / ml. The recoveries were in the range of 0.5mg / kg ~ 2.25mg / kg 83.2% ~ 84.6%, the relative standard deviation of 1.2% ~ 2.2%. Conclusion The detection limit of this method is low, the recovery rate is high, qualitative and reliable, quantitative and accurate, suitable for detection of olaquindox residues in pork.