超高效液相色谱-串联质谱法测定动物源性食品中10种水杨酰胺类化合物

Determination of 10 Kinds of Salicylamides in Foods of Animal Origin by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

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(r^2)不小于0.995 7,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 new method was developed for the determination of 10 kinds of salicylamides, including 5-chlorosalicylanilid, 4＇-bromosalicylanilid, 3＇, 4＇-dichloro-salicylanilid, 4＇, 5-dichloro-salicylan- ilid, 3＇, 4＇, 5-trichloro-salicylanilid, 5-bromo-4＇-chlorosalicylanilide, 3, 5-dibromo-salicylanilid, 4＇, 5-dibromo-salicylanilid, 3, 4＇, 5-tribromo-salicylanilid and 3, 3＇, 4＇, 5-tetrachloro-salicylan- ilid in foods of animal origin using solid phase extraction （SPE） combined with ultra-performance liq- uid chromatography- tandem mass spectrometry （HPLC -MS/MS）. Samples were extracted using acetonitrile, and purified with an amino（ NH2 ） SPE column. The eluent was concentrated by nitro- gen gas blowing. 10 target compounds were separated on a T3 column（ 100 mm ×2. 1 mm, 1.8 μm） by gradient elution with methanol -0. 1% formic acid as mobile phase, ionized by negative electros- pray ionization（ESI-）, detected under multiple reaction monitoring（MRM） mode, and quantified by the external standard method. Under the optimized condition, the calibration curves of 10 kinds of salicylamides were linear in a certain concentration range with correlation coefficients （r2） no less than 0. 995 7. The limits of detection（LODs, S/N =3） and limits of quantitation（LOQs, S/N = 10） for the target compounds were in the ranges of 0. 5 - 1.0 μg/kg and 1.5 - 3.0 μg/kg, respectively. The average recoveries at three spiked levels ranged from 81.0% to 106% , with relative standard de- viations（ RSD, n = 6） no more than 7. 5%. The method was suitable for the identification and quan- tification of 10 kinds of salicylamides in foods of animal origin.