摘要
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%.
作者
华永有
陈碧榕
周丽芳
林坚
HUA Yongyou;CHEN Birong;ZHOU Lifang;LIN Jian(Fujian Provincial Key Laboratory of Zoonosis,Fujian Center for Disease Control and Prevention,Fuzhou 350001,China;Zhangpu Center for Disease Control and Prevention,Zhangzhou 363200,China;Zhongshan Hospital Affiliated to Xiamen University,Xiamen 361000,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2023年第3期310-314,共5页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
福建省卫生健康科技计划项目(2020GGA022)
福建省科技创新平台建设项目(2019Y2001)。
关键词
液相色谱-串联质谱法
发酵肉制品
生物胺
liquid chromatography tandem mass spectrometry
fermented meat product
biogenic amine
