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建立了动物源性食品中10种水杨酰胺类化合物(5-氯水杨酰苯胺、4′-溴水杨酰苯胺、3′,4′-二氯水杨酰苯胺、4′,5-二氯水杨酰苯胺、3′,4′,5-三氯水杨酰苯胺、5-溴-4′-氯水杨酰苯胺、3,5-二溴水杨酰苯胺、4′,5-二溴水杨酰苯胺、3,4′,5-三溴水杨酰苯胺、3,3′,4′,5-四氯水杨酰苯胺)的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。样品经乙腈萃取,氨基固相萃取小柱(SPE)净化,T3色谱柱分离后,以甲醇-0.1%甲酸溶液梯度洗脱,串联质谱电喷雾负模式扫描,多反应监测模式检测,外标法定量。结果表明,10种目标物在一定范围内线性关系良好,相关系数(r2)不小于0.9957,检出限为0.5~1.0μg/kg,定量下限为1.5~3.0μg/kg;加标水平为1.5~30.0μg/kg时,回收率为81.0%~106%,相对标准偏差(RSD,n=6)不大于7.5%。该方法净化效果好、定量准确、灵敏快速,适用于动物源性食品中10种水杨酰胺类化合物的检测与确证。
A total of 10 salicylamides (5-salicylanilide, 4’-salicylanilide, 3 ’, 4’-dichlorosalicylanilide, 4’, 5- Dichlorosalicylanilide, 3 ’, 4’, 5-trichlorosalicylanilide, 5-bromo-4’-salicylanilide, 3,5-dibromosalicylanilide, 4 ’, 5 - High Performance Liquid Chromatography Tandem Mass Spectrometry (UPLC) with Dibromosalicylanilide, 3,4 ’, 5-Tribromosalicylanilide and 3,3’, 4 ’, 5-Tetrachlorosalicylanilide -MS / MS) detection method. The sample was purified by acetonitrile and SPE. After separation on T3 column, the sample was eluted with a gradient of methanol-0.1% formic acid, tandem mass spectrometry negative mode electrospray ionization, multi-reaction monitoring mode, external standard method Quantitative. The results showed that there was a good linear relationship between the 10 targets in a certain range, the correlation coefficient (r2) was not less than 0.9957, the detection limit was 0.5-1.0 μg / kg and the lower limit of quantification was 1.5-3.0 μg / kg. The spiked level was 1.5 ~ 30.0μg / kg, the recovery was 81.0% ~ 106%, the relative standard deviation (RSD, n = 6) was not more than 7.5%. The method has the advantages of good purification effect, accurate quantification, quick and sensitive detection and confirmation of 10 salicylamides in animal-derived foods.