超高效液相色谱-串联质谱法测定冷冻水产品中生物胺

Determination of Biogenic Amines in Frozen Aquatic Products by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry

建立了一种超高效液相色谱-串联质谱法检测水产品中生物胺类化合物的方法。采用氨水调节pH值使待测生物胺化合物以分子态存在,乙腈提取样品中的尸胺、腐胺、组胺、酪胺和色胺,用150 mg无水硫酸镁、75 mg丙磺酸(PSA)试剂包作为吸附剂进行QuEChERS分散固相萃取净化,然后通过超高效液相色谱-串联质谱法进行检测。结果表明,尸胺、腐胺在20.0~800 ng/mL,组胺、酪胺和色胺在5.00~160 ng/mL浓度范围内具有良好的线性关系,相关系数R^(2)分别为0.9992、0.9937、0.9970、0.9991、0.9974,尸胺、腐胺定量限为0.15 mg/kg,组胺、酪胺和色胺定量限为0.04 mg/kg,回收率为78.0%~102%,精密度均小于15%。该方法操作简单、灵敏度高、重现性好、回收率高,可满足冷冻水产品实际样品中生物胺类物质的测定。

A simple,efficient and accurate method was develeped for the determination of biogenic amines in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry,which used ammonia to adjust the pH value so that the biogenic amines to be measured exist in the molecular state.The cadaveric amines,putrescine,histamine,tyramine and tryptamine were extracted from the samples by acetonitrile and cleaned up by a dispersive solid-phase extraction(Quick,Easy,Cheap,Effective,Rugged,Safe)QuEChERS kit with 150 mg magnesium sulfate(MgSO 4)and 75 mg propanesulfonic acid(PSA)sorbent,and then detected by ultra performance liquid chromatography-tandem mass spectrometry.The results indicated good linearity in the concentration range of 20.0-800 ng/mL for cadaverine and putrescine,and 5.00-160 ng/mL for histamine,tyramine and tryptamine,with R^(2)values of 0.9992,0.9937,0.9970,0.9991 and 0.9974,respectively.The limits of quantification were 0.15 mg/kg for cadaverine and putrescine,and the limits of quantification were 0.04 mg/kg for histamine,tyramine and tryptamine.The recovery is 78.0%-102%,and the precision is less than 15%.The method was simple,sensitive,reproducible and had high recovery,which could meet the determination of biogenic amines in actual samples of frozen aquatic products.