摘要
[目的]评定液相色谱-串联质谱法测定三文鱼中生物胺的不确定度。[方法]样品经过5%三氯乙酸提取、正己烷除脂、丹磺酰氯丙酮溶液衍生化后,液相色谱-串联质谱分析三文鱼中9种生物胺的含量,对方法相对标准不确定度、标准不确定度、扩展不确定度进行评估。[结果]色胺、β-苯乙胺、腐胺、尸胺、酪胺、组胺、精胺、亚精胺、去甲基肾上腺素的平均值分别为4.30、5.59、5.72、6.21、4.85、5.48、7.18、6.79、4.77 mg/kg,扩展不确定度分别为0.46、0.56、0.48、0.54、0.42、0.50、0.64、0.55、0.41 mg/kg(k=2)。[结论]标准储备液的配制、稀释以及标准曲线的线性拟合对不确定度的贡献值最大,建议选用精度好的量器,规范试验操作与前处理步骤。
[Objective]To evaluate the uncertainty of determination of biogenic amines in salmon by liquid chromatography tandem mass spectrometry.[Method]The samples were extracted with 5%trichloroacetic acid,defatted with n-hexane and derivatized with dansyl chloroacetone solution.The contents of 9 biogenic amines in salmon were analyzed by LC-MS/MS.The relative standard uncertainty,standard uncertainty and expanded uncertainty of the method were evaluated.[Result]The average values of tryptamine,β-phenylethylamine,putrescine,cadaverine,tyramine,histamine,spermine,spermidine and norepinephrine were 4.30,5.59,5.72,6.21,4.85,5.48,7.18,6.79 and 4.77 mg/kg respectively,and the expanded uncertainty was 0.46,0.56,0.48,0.54,0.42,0.50,0.64,0.55and 0.41 mg/kg respectively(k=2).[Conclusion]The preparation and dilution of standard stock solution and the linear fitting of standard curve have the greatest contribution to the uncertainty.It is suggested to select a measuring instrument with good accuracy and standardize the experimental operation and pretreatment steps.
作者
郑越男
曹进
孙珊珊
郭亚辉
罗娇依
钱和
ZHENG Yue-nan;CAO Jin;SUN Shan-shan(State Key Laboratory of Food Science and Technology,Jiangnan University,Wuxi,Jiangsu 214122;National Institutes for Food and Drug Control,Beijing 100050)
出处
《安徽农业科学》
CAS
2021年第17期189-194,共6页
Journal of Anhui Agricultural Sciences
关键词
三文鱼
生物胺
液相色谱-串联质谱
不确定度
Salmon
Biogenic amine
Liquid chromatography tandem mass spectrometry
Uncertainty
