提出了液相色谱-串联质谱法测定发酵肉制品中组胺、酪胺、腐胺、尸胺和色胺等5种生物胺含量的方法。1.00 g样品经5%(体积分数)高氯酸溶液20 mL提取2次,合并上清液,用400 g·L^-1氢氧化钠溶液调节上述上清液pH至2~3,用0.5%(体积分数,下同)高氯酸溶液定容至50 mL。取2 mL上述溶液,与2 mL 0.5%高氯酸溶液混匀,经正己烷5 mL净化2次。取上述溶液0.25 mL,用乙腈定容至1.00 mL,过滤。以Waters Atlantic^® HILIC Silica色谱柱为固定相,以含10 mmol·L^-1甲酸铵的0.5%(体积分数,下同)甲酸溶液-含10 mmol·L^-1甲酸铵、0.5%甲酸的乙腈溶液为流动相进行梯度洗脱,采用液相色谱-串联质谱法测定滤液中5种生物胺的含量。结果表明:5种生物胺的质量浓度在一定范围内与对应的峰面积呈线性关系,检出限(3S/N)为0.010~0.80 mg·kg^-1。按标准加入法进行回收试验,回收率为82.0%~120%,测定值的相对标准偏差(n=6)为0.80%~12%。

A method for the determination of 5 biogenic amines, including histamine, tyramine, putrescine, cadaverine and tryptamine, in fermented meat products by liquid chromatography tandem mass spectrometry was proposed. 1.00 g of sample was extracted twice with 20 mL of 5% (volume fraction) perchloric acid solution, and then the supernatant was combined and adjusted to pH 2-3 with 400 g·L^-1 sodium hydroxide solution. The volume was made up to 50 mL with 0.5% (volume fraction, the same below) perchloric acid solution. 2 mL of the above solution was taken, mixed with 2 mL of 0.5% perchloric acid solution, and purified twice with 5 mL of n-hexane. 0.25 mL of the above solution was taken, diluted to 1.00 mL with acetonitrile and filtered. 5 biogenic amines in the filtrate were determined by liquid chromatography tandem mass spectrometry, using Waters Atlantic^® HILIC Silica chromatographic column as the stationary phase, and 0.5% (volume fraction, the same below) formic acid solution containing 10 mmol·L^-1 ammonium formate-acetonitrile solution containing 10 mmol·L^-1 ammonium formate and 0.5% formic acid as the mobile phase for gradient elution. As shown by the results, linear relationships between values of the corresponding peak area and mass concentration of 5 biogenic amines were found in definite ranges, with detection limits (3S/N) in the range of 0.010-0.80 mg·kg^-1. Recovery test was carried out according to the standard addition method, giving results in the range of 82.2%-120%, with RSDs (n=6) of the determined values in the range of 0.80%-12%.