超高效液相色谱-串联质谱法同时测定小黄花鱼中9种生物胺

为快速检测水产品中精胺、亚精胺、腐胺、尸胺、组胺、色胺、章鱼胺、酪胺、2-苯乙胺9种生物胺含量，本研究以小黄花鱼为基质，优化了流动相组成和样品提取溶剂，建立了超高效液相色谱-串联三重四极杆质谱同时检测方法。样品经0.1%三氯乙酸水溶液重复提取两遍，合并上清液过0.22 μm聚四氟乙烯滤膜。以HSS T3为色谱柱，流动相A为0.1%甲酸乙腈，流动相B为10 mmol/L甲酸铵水溶液含0.2%甲酸，在电喷雾正离子电离、多反应监测模式下，9种生物胺在4 min内得到分离。根据响应强度不同，9种生物胺分成酪胺、2-苯乙胺，腐胺、尸胺、组胺、色胺、章鱼胺，精胺、亚精胺三组，以1:5:25浓度比配制多浓度混合标准中间液。该方法对三组生物胺的线性范围分别为1~40 ng/mL、5~200 ng/mL和25~1000 ng/mL；方法定量限依次为0.01、0.05和0.25 mg/kg。低、中、高三个浓度水平加标回收率分别为81.7%~111.2%、80.0%~110.3%、80.0%~99.0%；精密度（n=6）依次为1.7%~7.3%、1.3%~9.1%、0.7%~4.6%。总体而言，该方法简便、快速，具有良好的灵敏度、回收率和精密度，适用于小黄花鱼中生物胺的测定。

Simultaneous Determination of 9 Biogenic Amines in Larimichthys polyactis by UHPLC-MS/MS

To rapidly determine 9 biogenic amines including spermine, spermidine, putrescine, cadaverine, histamine, tryptamine, octopamine, tyramine and β-phenethylamine in aquatic products, the ultra high-performance liquid chromatography-tandem mass spectrometry method was established with Larimichthys polyactis using as matrix sample, and mobile phase and extract solvents were optimized. Matrix sample was extracted by 0.1% trichloroacetic acid (TCA) in duplicate, the supernatant was combined and filtered by 0.22 μm PTFE filters, and separated by HSS T3 column in 4 min. The mobile phase A was acetonitrile containing 0.1% formic acid, while mobile phase B was 10 mmol/L ammonium formate containing 0.2% formic acid. Nine biogenic amines were divided into three groups based on their different response intensity, with a concentration range of 1 to 40 ng/mL (tyramine and β-phenethylamine), 5 to 200 ng/mL (putrescine, cadaverine, histamine, tryptamine and octopamine), and 25 to 1000 ng/mL (spermine and spermidine). Their method quantification limits (LOQs) were 0.01, 0.05 and 0.25 mg/kg, respectively. The recovery rate of low, medium and high concentrations was 81.7%~111.2%, 80.0%~110.3% and 80.0%~99.0%, respectively, with the corresponding degree of precision (n=6) of 1.7%~7.3%, 1.3%~9.1% and 0.7%~4.6%. This method is simple, fast and with good sensitivity, recovery and precision, which is suitable for the determination of biogenic amines in Larimichthys polyactis.