Analysis of 2-Acetyl-1-Pyrroline in Rice by HSSE/GC/MS

Analysis of 2-Acetyl-1-Pyrroline in Rice by HSSE/GC/MS
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DOI:
10.1094/cchem-09-10-0136
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发表时间:
2011-05-01
期刊:
影响因子:
2.4
通讯作者:
McClung, Anna
McClung, Anna
中科院分区:
农林科学4区
文献类型:
--
作者:
Grimm, Casey C.;Champagne, Elaine T.;McClung, Anna

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研究了搅拌棒吸附萃取(Twister)测定大米中2-乙酰基-1-吡咯啉(2AP)的方法。将Twister搅拌棒放置在含有1g米粒、7.5mL0.1M KOH和2.2g NaCl的20-mL小瓶的顶部空间中,沿着第二个涂有特氟隆的搅拌棒用于混合。分析物在40 ° C下吸附到Twister上4小时,然后在270 ° C下解吸到GC柱中,同时在-80 ° C下冷冻聚焦。顶空吸附萃取(HSSE)法的检出率为10%,低于GC/FID法(约6%)。使用HSSE,在通常被认为是芳香族的所有样品中观察到2AP,并且在任何非芳香族样品中未观察到2AP。此外,对2-乙酰基-1-吡咯啉的合成方法进行了改进,并证实了2-乙酰基-1-吡咯啉的互变异构体的存在。
An extremely sensitive method for the analysis of 2-acetyl-1-pyrroline (2AP) in rice, employing stir bar sorptive extraction (Twister) was studied. The Twister stir bar is placed in the headspace of a 20-mL vial containing 1 g of rice kernels, 7.5 mL of 0.1M KOH, and 2.2 g of NaCl, along with a second Teflon-coated stir bar for mixing. Analytes are adsorbed onto the Twister for 4 hr at 40 degrees C and then desorbed at 270 degrees C into a GC column while cryofocusing at -80 degrees C. The headspace sorptive extraction (HSSE) method was able to detect 10%) was not as good as the GC/FID method (approximate to 6%). Using HSSE, 2AP was observed in all samples generally considered to be aromatic and was not observed in any nonaromatic samples. Additionally, a modified method for the synthesis of 2-acetyl-1-pyrroline was studied and the presence of a tautomer of 2-acetyl-1-pyrroline was confirmed.