论文部分内容阅读
目的建立了双水相萃取结合气相色谱质谱法(gas chromatography-mass spectrometry,GC/MS)测定不同香型白酒中氨基甲酸乙酯的测定方法。方法对比研究了3种不同的样品液液萃取方法,在此基础上,优化获得了最优双水相萃取(LLE-GC/MS)方案:准确移取5 m L试样于10 m L比色管中,再加入内标PC使用液,逐渐增加管中K2HPO4固体,直到饱和为止,静置至分层完全。取上清液1.5 m L于离心管中,加无水Mg SO4 150mg摇匀离心。取上清直接进样,用GC/MS检测样品中氨基甲酸乙酯的含量。通过分别检测白酒三大香型:清香、浓香、酱香型,对LLE-GC/MS方法进行了评价。结果在最优条件下检测的相对标准偏差为2.84%~3.95%,回收率为:86.45%~111.58%,检测限为1.34μg/L。结论此方法准确性好、简便、低成本,适用于上述3种香型白酒中氨基甲酸乙酯的检测。
OBJECTIVE To establish a method for the determination of urethane in different scent liquors by two-phase extraction combined with gas chromatography-mass spectrometry (GC / MS). Methods Three different liquid-liquid extraction methods were compared and studied. Based on this, the optimal dual-phase aqueous extraction (LLE-GC / MS) protocol was optimized: 5 m L Color tube, then add the internal standard PC use solution, and gradually increase the tube K2HPO4 solids, until saturated, allowed to stratified completely. Take the supernatant 1.5 m L in a centrifuge tube, add anhydrous MgSO4 150mg shake centrifuge. The supernatant was injected directly and the content of urethane in the sample was determined by GC / MS. The three major flavors of spirits were detected by the method of LLE-GC / MS. Results The relative standard deviations (RSDs) were 2.84% ~ 3.95%. The recoveries were 86.45% ~ 111.58%. The detection limit was 1.34μg / L. Conclusion This method is accurate, simple and low cost and suitable for the detection of urethane in the above three kinds of scent liquor.