SPE-UPLC-MS/MS法测定茶叶中的5-羟甲基糠醛

Determination of 5-Hydroxymethylfurfural in Tea by SPE-UPLC-MS/MS

建立固相萃取-超高效液相色谱-串联质谱法测定茶叶中5-羟甲基糠醛(5-HMF)含量的方法。样品经水超声提取, HLB固相萃取柱净化,氮吹浓缩至近干,流动相溶解,以SB-C18色谱柱分离,在电喷雾离子源正离子(ESI+)模式下电离,多反应监测(MRM)模式下检测,外标法定量。在优化条件下, 5-HMF检出限为0.012 mg/kg,在2~500μg/L质量浓度范围内线性关系良好,相关系数大于0.998,回收率(n=6)为81.1%~93.9%,日内精密度为1.65%~5.82%;日间精密度(n=3)为5.01%~6.24%。试验方法净化效果好,灵敏度高,准确可靠,重复性好,适用于茶叶中5-HMF含量测定。

A method for 5-hydroxymethylfurfural(5-HMF) in tea by solid phase extraction/ultra performance liquid chromatography-tandem mass spectrometry analysis was to developed. After extracted by ultrasonic, the sample was purified by passing through HLB solid phase extraction column and the eluate evaporated to dryness under nitrogen stream. The residue was redissolved with mobile phase and separated by an agilent zorbax SB-C18(RRHD) column. The quantification of the analyte was achieved by the external standard method, and was carried out with positive electrospray ionization(ESI+) source under multiple reaction monitoring(MRM) mode. Under the optimized condition, this method demonstrated low limit of detection at 0.012 mg/kg and coefficient of determination(r2)>0.998 for 5-HMF with a calibration range established from 2 to 500 μg/L. This method demonstrated excellent quantification accuracy, precision(the intra-day and inter-day precisions were in the range of 1.65%-5.82% and 5.01%-6.24%, respectively) and recovery(81.1%-93.9%). The developed method was characterized by the excellent purification effect, sensitivity and accuracy, and it was competent for the detection of 5-HMF in tea.