为了建立鸡肉中盐酸硫利达嗪的高效液相色谱分析方法,应用高效液相色谱法连接二极管阵列检测器确定盐酸硫利达嗪最佳检测波长,样品前处理以乙酸乙酯为提取溶剂,正己烷去脂肪,氮吹浓缩,乙腈溶解,用60 mg HLB固相萃取柱净化,经0.22 μm有机滤膜过滤.色谱条件:乙腈-体积分数为0.1%甲酸溶液(体积比35∶65)为流动相,流速1 mL/min,二极管阵列检测器检测,外标法定量.结果表明:该方法在0.1~10.0 μg/mL内的线性关系良好,相关系数r2=0.999 9,检出限为1.2 μg/kg,定量限为4.0 μg/kg,回收率为88.96%~98.58%.本研究建立的鸡肉中盐酸硫利达嗪的高效液相色谱分析方法,具有精密度好、操作方便快捷、回收率高等优点,为动物源性食品中镇静剂的检测提供技术支持.
To establish an HPLC method for the determination of thiolidazine hydrochloride in chicken,the best detection wavelength of thiolidazine hydrochloride was determined by high performance liquid chromatograph(HPLC)with a diode array detector.The samples were extracted with ethyl acetate as solvent, and the fat was removed with n-hexane, concentrated by nitrogen blowing, then dissolved with acetonitrile, purified with 60 mg HLB solid phase extraction column, and finally filtered with 0.22 μm organic membrane. The liquid chromatographic conditions were as follows: mobile phase consisted of acetonitrile-0.1% formic acid aqueous solution(V∶V=35∶65), the flow rate was 1 mL/min, and diode array detector was used for detection. Quantitative analysis was carried out by the external standard method. The results show that the linearity of the method is good in the range of 0.1—10.0 μg/mL. The limit of detection was 1.2 μg/kg, the limit of quantitation was 4.0 μg/kg, and the recoveries were 8.96%—98.58%. The HPLC method established in this study for the determination of thiolidazine hydrochloride in chicken has the advantages of good precision, convenient operation and high recovery.It can provide a technical method for the detection of tranquilizers in animal food.
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