柱前衍生超高效液相色谱-串联质谱法测定三文鱼中9种生物胺

Determination of 9 kinds of biogenic amines in salmon by precolumn derivatization-ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  三文鱼  生物胺  柱前衍生  超高效液相色谱-串联质谱法

英文关键词:salmon  biogenic amine  precolumn derivatization  ultra performance liquid chromatography- tandem mass spectrometry

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)检测三文鱼中9种生物胺(β-苯乙胺、组胺、腐胺、尸胺、酪胺、色胺、精胺、亚精胺、去甲基肾上腺素)的分析方法。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, 经BEH Shield RP18柱(2.1 mm×150 mm, 1.7 μm)分离, 以0.1%甲酸的50%乙腈水溶液和乙腈作为流动相, 采用电喷雾正离子(electrosprary ionization, ESI+)扫描、多反应监测模式分析。结果 9种生物胺分别在0~0.3 mg/L范围内线性良好, 相关系数r＞0.996; β-苯乙胺、色胺、腐胺、尸胺、组胺、酪胺、亚精胺、精胺、去甲基肾上腺素的平均回收率范围为82.43%~95.30%, 检出限依次为0.0605、0.0822、0.0915、0.0244、0.0871、0.1510、0.0744、0.0348、0.0750 μg/g。结论 本方法结合了衍生化反应和超高效液相色谱-串联质谱法的优势。在实际样品检测中, 前处理程序简化, 方法灵敏度提高。此方法的目标物分离性、稳定性和峰型良好, 可对三文鱼复杂基质中生物胺进行快速、准确、稳定的定量、定性分析。

英文摘要:

      Objective To establish an analytical method for the determination of 9 kinds of biogenic amines (β-phenylethylamine, histamine, putrescine, cadaverine, tyramine, tryptamine, spermine, spermidine and norad renaline) in salmon by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were extracted with 5% trichloroacetic acid, degreased with n-hexane, derivatized with dansyl chloride in acetone solution, separated by BEH Shield RP18 column (2.1 mm×150 mm, 1.7 μm) using 50% acetonitrile aqueous solution containing 0.1% formic acid and acetonitrile as the mobile phase, and electrosprary ionization (ESI+) scanning and multi-reaction monitoring mode were used for analysis. Results The linearities of the 9 kinds of biogenic amines were good within the range of 0-0.3 mg/L with the correlation coefficients r>0.996; for β-phenylethylamine, tryptamine, putrescine, cadaverine, histamine, tyramine, spermidine, spermine and noradrenaline, the range of average recoveries were 82.43%-95.30%, and the detection limits were 0.0605, 0.0822, 0.0915, 0.0244, 0.0871, 0.1510, 0.0744, 0.0348 and 0.0750 μg/g, respectively. Conclusion This method combines the advantages of derivatization reaction and UPLC-MS/MS. In the detection of actual samples, the pretreatment procedure is simplified, method sensitivity iss improved. For this method, target separability, stability and peak shape are good, and can be used for rapid, accurate and stable quantitative and qualitative analysis of biogenic amines in salmon complex matrix.