超高效液相色谱-串联质谱法同时测定蜂蜜中8种生物胺

建立了同时测定蜂蜜中色胺(TR)、2-苯乙胺(PHE)、腐胺(PUT)、尸胺(CAD)、组胺(HIS)、酪胺(TYR)、亚精胺(SPD)和精胺(SP)8种生物胺的超高效液相色谱串联质谱柱前衍生的分析方法。样品经5%三氯乙酸溶液提取后用丹磺酰氯柱前衍生,采用Agilent Poroshell 120 SB-C₁₈(50 mm×2.1 mm,2.7 μm)柱,以0.1%甲酸水溶液-0.1%甲酸乙腈溶液为流动相进行定性和定量分析。采用本方法对22种市售蜂蜜进行检测,结果显示8种生物胺在不同的蜂蜜中检出,所有蜂蜜样品中均检测到2-苯乙胺和腐胺,其中2-苯乙胺也是蜂蜜样品中平均含量最多的生物胺。本方法中8种生物胺的线性相关系数均大于0.99,检出限为0.01~0.51 μg/L。在添加水平为100、500、1000 μg/kg时,样品的平均回收率在76%~112%之间,日内精密度小于等于9.8%,日间精密度小于等于13.1%。该方法快速简单,灵敏准确,且回收率稳定,适用于蜂蜜中生物胺的检测。

Simultaneous determination of 8 biogenic amines in honey by ultra-high performance liquid chromatography-tandem mass spectrometry

An ultra-high performance liquid chromatographic tandem mass spectrometry analysis with derivatization method was developed for the simultaneous determination of 8 biogenic amines(BAs)in honey which were tryptamine(TR),phenylethylamine(PHE),cadaverine(CAD),histamine(HIS),tyramine(TYR),putrescine(PUT),spermidine(SPD),spermine(SP). The honey samples were extracted by 5% trichloroacetic acid,derived with dansyl chloride. The BAs were separated on Agilent Poroshell 120 SB-C₁₈(50 mm×2.1 mm,2.7 μm)column,and the mobile phase consisting of 0.1%(v/v)aqueous formic acid(A)and ACN with 0.1% formic acid(B)were used for qualitative and quantitative analysis. 22 kinds of commercial honey were detected using the optimized method,the results showed that 8 BAs in different of commercial honey were detected under the method. Phenylethylamine and putrescine were detected in all honey samples,moreover,phenylethylamine was at high average level in honey samples. The correlation coefficients of the calibration curves were more than 0.99,the limits of detections(LODs)were 0.01~0.51 μg/L for the 8 BAs. The recoveries for honey fortified with 8 BAs at levels of 100,500,1000 μg/kg were 76%~112%,the RSD values for the intra-day and inter-day precisions were less than or equal to 9.8% and 13.1% respectively. The present method has advantages such as simplicity,sensitivity and accurately and could be applied to the detection of BAs in honey.