高效液相色谱-串联质谱法检测多菌灵在啤酒加工过程中的残留量变化

利用高效液相色谱-串联质谱对啤酒加工过程中多菌灵残留变化进行研究,建立了大麦、干麦芽、麦糟、协定麦汁、定型麦汁和啤酒中多菌灵残留的检测方法。运用QuEChERS方法,大麦、麦芽和麦糟样品用6g无水硫酸镁和1.5g醋酸钠提取,150mg无水硫酸镁、50mgC18和50mgPSA净化;协定麦汁、定型麦汁和啤酒样品用去离子水稀释后经C18固相萃取柱净化。经高效液相色谱-串联质谱测定。结果表明:在0.01~0.5mg/kg添加水平下,多菌灵的平均添加回收率在72%~99%之间,相对标准偏差小于9%,定量限为0.01mg/kg。采用所建立的方法测得多菌灵在各样品中的残留量分别为:大麦1.99mg/kg、麦芽2.71mg/kg、麦糟0.41mg/kg、协定麦汁1.37mg/kg、定型麦汁1.34mg/kg和啤酒0.12mg/kg。样品经糖化、煮沸和发酵后,其中的多菌灵残留量总体呈下降趋势,其加工因子分别为0.51、0.98和0.089,其中发酵过程对多菌灵的去除率最高。

Fate of carbendazim residue during beer brewing process by high performance liquid chromatography-tandem mass spectrometry

Fate of carbendazim residue during the beer brewing process was determined by the high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The simultaneous determination of carbendazim in different samples (barley, malt, spent grain, agreement wort, finalize wort and beer) were developed. For barley, malt and spent grain samples, the QuEChERS method was used for the pretreatment. 6 g MgSO₄ and 1.5 g NaAc were used for the extraction, and 150 mg of MgSO₄, 50 mg C₁₈ and 50 mg PSA were used for the purification. Agreement wort, finalize wort and beer samples were directly diluted with deionized water and then purified with C₁₈ solid phase extraction column. The main results are presented as followed: The mean recoveries varied from 72% to 99% and the relative standard deviations (RSD) was less than 9%. The limit of quantitation was 0.01 mg/kg. The residues of carbendazim is 1.99 mg/kg in barley, 2.71 mg/kg in malt, 0.41 mg/kg in spent grain, 1.37 mg/kg in agreement wort, 1.34 mg/kg in finalize wort and 0.12 mg/kg in beer. During saccharification, boiling and fermentation processes, the residue of carbendazim has been reduced with the processing factor 0.51, 0.98 and 0.089, respectively. The removal efficiency of fermentation was the highest.