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目的建立了高效液相色谱法测定丹东市售鸡肉中的己烯雌酚和甲睾酮残留量测定方法。方法称取鸡肉匀浆约5 g,放入50 m L具塞离心管中,精密加入甲醇10 m L,涡旋振荡,于5 000 r/min离心5 min,取出上清液,残渣中再精密加入流动相10 m L,重复提取1次,合并上清液,于7 000 r/min离心5 min后上高效液相色谱仪测定。结果该方法己烯雌酚的检出限为10 ng,甲睾酮的检出限为10 ng,己烯雌酚在51.9~1 038 ng/m L的范围内呈良好的线性关系,r=0.999 7。甲睾酮在49.2~984ng/m L的范围内呈良好的线性关系,r=0.999 9。己烯雌酚和甲睾酮的添加平均回收率分别为80.1%和79.7%。相对标准偏差(RSD)分别为3.4%和3.1%。结论该方法灵敏度高,能有效地消除杂质基质带来的干扰,可以作为禽肉样品中上述2种药物残留量的检测方法。
OBJECTIVE To establish a method for the determination of diethylstilbestrol and methyltestosterone in Dandong commercial chicken by high performance liquid chromatography. Methods Weigh about 5 g chicken homogenate, placed in 50 m L with centrifuge tube, add 10 ml of methanol precision, vortexed, centrifuged at 5 000 r / min for 5 min, the supernatant removed, the residue and then Precision adding mobile phase 10 m L, repeated extraction 1, the supernatant was combined, centrifuged at 7 000 r / min 5 min after determination by high performance liquid chromatography. Results The detection limit of diethylstilbestrol was 10 ng, the detection limit of methyltestosterone was 10 ng, and the diethylstilbestrol showed a good linear relationship in the range of 51.9 ~ 1038 ng / m L (r = 0.999 7). Methyltestosterone showed a good linear relationship in the range of 49.2-984 ng / m L, r = 0.999 9. The average recoveries of diethylstilbestrol and methyltestosterone were 80.1% and 79.7%, respectively. The relative standard deviations (RSDs) were 3.4% and 3.1% respectively. Conclusion The method has high sensitivity and can effectively eliminate the interference caused by the impurity matrix, and can be used as a detection method for the residues of the two drugs in the sample of poultry.